WorldWideScience

Sample records for solid sampling methods

  1. Method for fractional solid-waste sampling and chemical analysis

    DEFF Research Database (Denmark)

    Riber, Christian; Rodushkin, I.; Spliid, Henrik

    2007-01-01

    Chemical characterization of solid waste is a demanding task due to the heterogeneity of the waste. This article describes how 45 material fractions hand-sorted from Danish household waste were subsampled and prepared for chemical analysis of 61 substances. All material fractions were subject...... of variance (20-85% of the overall variation). Only by increasing the sample size significantly can this variance be reduced. The accuracy and short-term reproducibility of the chemical characterization were good, as determined by the analysis of several relevant certified reference materials. Typically, six...

  2. Kinetic studies in solid state reactions by sample-controlled methods and advanced analysis procedures

    OpenAIRE

    Pérez-Maqueda, Luis A.; Criado, J. M.; Sánchez-Jiménez, P.E.; Perejón, Antonio

    2013-01-01

    A comparative study of both conventional rising temperature and sample-controlled methods, like constant rate thermal analysis (CRTA), is carried out after analyzing a set of solid state reactions using both methods. It is shown that CRTA avoids the influence of heat and mass transfer phenomena for a wide range of sample sizes leading to reliable kinetic parameters. On the other hand, conventional rising temperature methods yield α–T plots dependent on experimental conditions, even when using...

  3. A long-term validation of the modernised DC-ARC-OES solid-sample method

    Energy Technology Data Exchange (ETDEWEB)

    Florian, K. [Dept. of Chemistry, Technical University of Kosice (Slovakia); Hassler, J.; Foerster, O. [Elektroschmelzwerk GmbH, Kempten (Germany)

    2001-12-01

    The validation procedure based on ISO 17 025 standard has been used to study and illustrate both the long-term stability of the calibration process of the DC-ARC solid sample spectrometric method and the main validation criteria of the method. In the calculation of the validation characteristics depending on the linearity(calibration), also the fulfilment of predetermining criteria such as normality and homoscedasticity was checked. In order to decide whether there are any trends in the time-variation of the analytical signal or not, also the Neumann test of trend was applied and evaluated. Finally, a comparison with similar validation data of the ETV-ICP-OES method was carried out. (orig.)

  4. A Green Analytical Method Using Ultrasound in Sample Preparation for the Flow Injection Determination of Iron, Manganese, and Zinc in Soluble Solid Samples by Flame Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    M. Carmen Yebra

    2012-01-01

    Full Text Available A simple and rapid analytical method was developed for the determination of iron, manganese, and zinc in soluble solid samples. The method is based on continuous ultrasonic water dissolution of the sample (5–30 mg at room temperature followed by flow injection flame atomic absorption spectrometric determination. A good precision of the whole procedure (1.2–4.6% and a sample throughput of ca. 25 samples h–1 were obtained. The proposed green analytical method has been successfully applied for the determination of iron, manganese, and zinc in soluble solid food samples (soluble cocoa and soluble coffee and pharmaceutical preparations (multivitamin tablets. The ranges of concentrations found were 21.4–25.61 μg g-1 for iron, 5.74–18.30 μg g-1 for manganese, and 33.27–57.90 μg g-1 for zinc in soluble solid food samples and 3.75–9.90 μg g-1 for iron, 0.47–5.05 μg g-1 for manganese, and 1.55–15.12 μg g-1 for zinc in multivitamin tablets. The accuracy of the proposed method was established by a comparison with the conventional wet acid digestion method using a paired t-test, indicating the absence of systematic errors.

  5. A Green Analytical Method Using Ultrasound in Sample Preparation for the Flow Injection Determination of Iron, Manganese, and Zinc in Soluble Solid Samples by Flame Atomic Absorption Spectrometry

    Science.gov (United States)

    Yebra, M. Carmen

    2012-01-01

    A simple and rapid analytical method was developed for the determination of iron, manganese, and zinc in soluble solid samples. The method is based on continuous ultrasonic water dissolution of the sample (5–30 mg) at room temperature followed by flow injection flame atomic absorption spectrometric determination. A good precision of the whole procedure (1.2–4.6%) and a sample throughput of ca. 25 samples h–1 were obtained. The proposed green analytical method has been successfully applied for the determination of iron, manganese, and zinc in soluble solid food samples (soluble cocoa and soluble coffee) and pharmaceutical preparations (multivitamin tablets). The ranges of concentrations found were 21.4–25.61 μg g−1 for iron, 5.74–18.30 μg g−1 for manganese, and 33.27–57.90 μg g−1 for zinc in soluble solid food samples and 3.75–9.90 μg g−1 for iron, 0.47–5.05 μg g−1 for manganese, and 1.55–15.12 μg g−1 for zinc in multivitamin tablets. The accuracy of the proposed method was established by a comparison with the conventional wet acid digestion method using a paired t-test, indicating the absence of systematic errors. PMID:22567553

  6. Method and apparatus for measuring the gas permeability of a solid sample

    Science.gov (United States)

    Carstens, D.H.W.

    1984-01-27

    The disclosure is directed to an apparatus and method for measuring the permeability of a gas in a sample. The gas is allowed to reach a steady flow rate through the sample. A measurable amount of the gas is collected during a given time period and then delivered to a sensitive quadrupole. The quadrupole signal, adjusted for background, is proportional to the amount of gas collected during the time period. The quadrupole can be calibrated with a standard helium leak. The gas can be deuterium and the sample can be polyvinyl alcohol.

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

    Science.gov (United States)

    Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

    2016-10-01

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

  8. Simultaneous Determination of TetracyclinesResidues in Bovine Milk Samples by Solid Phase Extraction and HPLC-FL Method

    Directory of Open Access Journals (Sweden)

    Mehra Mesgari Abbasi

    2011-06-01

    Full Text Available Introduction:Tetracyclines (TCs are widely used in animal husbandry and their residues in milk may resultinharmful effects on human. The aim of this study was to investigate the presence of TCs residues in various bovine milk samples from local markets of Ardabil, Iran. Methods:One hundred and fourteen pasteurized, sterilized and raw milk samples were collected from markets of Ardabil. Tetracycline, Oxytetracycline and Chlortetracycline (TCs residues extraction carried out by Solid Phase Extraction method. Determination of TCs residues were performed by high performance liquid chromatography (HPLC method using Fluorescence detector.Results: The mean of total TCs residues in all samples (114 samples was 97.6 ±16.9ng/g and that of pasteurized, sterilized and raw milk samples were 87.1 ± 17.7, 112.0 ± 57.3 and 154.0 ± 66.3ng/g respectively. Twenty five point four percent of the all samples, and24.4%, 30% and 28.6% of the pasteurized, sterilized and raw milk samples, respectively had higher TCs residues than the recommended maximum levels (100ng/g. Conclusion:This study indicates the presence of tetracycline residues more than allowed amount. Regulatory authorities should ensure proper withdrawal period before milking the animals and definite supervisions are necessary on application of these drugs.

  9. A gas-diffusion flow injection method coupled with online solid-liquid extraction for the determination of ammonium in solid samples.

    Science.gov (United States)

    Timofeeva, Irina I; Bulatov, Andrey V; Moskvin, Aleksey L; Kolev, Spas D

    2015-09-01

    A simple, rapid and reliable gas-diffusion flow injection (GD-FI) method for ammonium determination in building materials has been developed. It is based on leaching ammonium from a ground solid sample into an alkaline solution with subsequent ammonia gas generation. Ammonia is then transported in a nitrogen stream to the GD cell of the FI system where it is absorbed into its acceptor solution containing a mixture of the acid-base indicators cresol red and thymol blue. The maximum increase in the absorbance of the acceptor solution at 580 nm is related to the ammonium concentration in the solid sample. The proposed method is characterized by a linear concentration range of 0.1-5.0 mg NH4(+) kg(-1), a limit of detection of 8 μg NH4(+) kg(-1) and a sample throughput of 10h(-1). A successful application of this method for the determination of ammonium in building materials such as concrete, cement and sand is reported. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Simultaneous Determination of Tetracyclines Residues in Bovine Milk Samples by Solid Phase Extraction and HPLC-FL Method.

    Science.gov (United States)

    Mesgari Abbasi, Mehran; Babaei, Hossein; Ansarin, Masoud; Nourdadgar, Ashraf-O-Sadat; Nemati, Mahboob

    2011-01-01

    Tetracyclines (TCs) are widely used in animal husbandry and their residues in milk may resultin harmful effects on human. The aim of this study was to investigate the presence of TCs residues in various bovine milk samples from local markets of Ardabil, Iran. One hundred and fourteen pasteurized, sterilized and raw milk samples were collected from markets of Ardabil. Tetracycline, Oxytetracycline and Chlortetracycline (TCs) residues extraction carried out by Solid Phase Extraction method. Determination of TCs residues were performed by high performance liquid chromatography (HPLC) method using Fluorescence detector. The mean of total TCs residues in all samples (114 samples) was 97.6 ±16.9ng/g and that of pasteurized, sterilized and raw milk samples were 87.1 ± 17.7, 112.0 ± 57.3 and 154.0 ± 66.3ng/g respectively. Twenty five point four percent of the all samples, and 24.4%, 30% and 28.6% of the pasteurized, sterilized and raw milk samples, respectively had higher TCs residues than the recommended maximum levels (100ng/g). This study indicates the presence of tetracycline residues more than allowed amount. Regulatory authorities should ensure proper withdrawal period before milking the animals and definite supervisions are necessary on application of these drugs.

  11. Developing a New Sampling And Analysis Method For Hydrazine And Monomethyl Hydrazine: Using a Derivatizing Agent With Solid Phase Microextraction

    Science.gov (United States)

    Allen, John

    2001-01-01

    Solid phase microextraction (SPME) will be used to develop a method for detecting monomethyl hydrazine (MMH) and hydrazine (Hz). A derivatizing agent, pentafluorobenzoyl chloride (PFBCI), is known to react readily with MMH and Hz. The SPME fiber can either be coated with PFBCl and introduced into a gaseous stream containing MMH, or PFBCl and MMH can react first in a syringe barrel and after a short equilibration period a SPME is used to sample the resulting solution. These methods were optimized and compared. Because Hz and MMH can degrade the SPME, letting the reaction occur first gave better results. Only MMH could be detected using either of these methods. Future research will concentrate on constructing calibration curves and determining the detection limit.

  12. Nuclear Magnetic Resonance and Headspace Solid-Phase Microextraction Gas Chromatography as Complementary Methods for the Analysis of Beer Samples

    Directory of Open Access Journals (Sweden)

    Sarah R. Johnson

    2017-04-01

    Full Text Available Chemical analysis of the organic components in beer has applications to quality control, authenticity and improvements to the flavor characteristics and brewing process. This study aims to show the complementary nature of two instrumental techniques which, in combination, can identify and quantify a number of organic components in a beer sample. Nuclear Magnetic Resonance (NMR was used to provide concentrations of 26 different organic compounds including alcohols, organic acids, carbohydrates, and amino acids. Calorie content was also estimated for the samples. NMR data for ethanol concentrations were validated by comparison to a Fourier Transform Infrared Spectrometry (FTIR method. Headspace Solid-Phase Microextraction (SPME Gas Chromatography Mass Spectrometry (GCMS was used to identify a range of volatile compounds such as alcohols, esters and hop-derived aroma compounds. A simple and inexpensive conversion of a Gas Chromatography Flame Ionization Detector (GC FID instrument to allow the use of Solid-Phase Microextraction was found to be useful for the quantification of volatile esters.

  13. Development of a full automation solid phase microextraction method for investigating the partition coefficient of organic pollutant in complex sample.

    Science.gov (United States)

    Jiang, Ruifen; Lin, Wei; Wen, Sijia; Zhu, Fang; Luan, Tiangang; Ouyang, Gangfeng

    2015-08-07

    A fully automated solid phase microextraction (SPME) depletion method was developed to study the partition coefficient of organic compound between complex matrix and water sample. The SPME depletion process was conducted by pre-loading the fiber with a specific amount of organic compounds from a proposed standard gas generation vial, and then desorbing the fiber into the targeted samples. Based on the proposed method, the partition coefficients (Kmatrix) of 4 polyaromatic hydrocarbons (PAHs) between humic acid (HA)/hydroxypropyl-β-cyclodextrin (β-HPCD) and aqueous sample were determined. The results showed that the logKmatrix of 4 PAHs with HA and β-HPCD ranged from 3.19 to 4.08, and 2.45 to 3.15, respectively. In addition, the logKmatrix values decreased about 0.12-0.27 log units for different PAHs for every 10°C increase in temperature. The effect of temperature on the partition coefficient followed van't Hoff plot, and the partition coefficient at any temperature can be predicted based on the plot. Furthermore, the proposed method was applied for the real biological fluid analysis. The partition coefficients of 6 PAHs between the complex matrices in the fetal bovine serum and water were determined, and compared to ones obtained from SPME extraction method. The result demonstrated that the proposed method can be applied to determine the sorption coefficients of hydrophobic compounds between complex matrix and water in a variety of samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Dynamic Flow-through Methods for Metal Fractionation in Environmental Solid Samples

    DEFF Research Database (Denmark)

    Miró, Manuel; Hansen, Elo Harald; Petersen, Roongrat

    of elements is quite insufficient to estimate their physicochemical mobility, potential bioavailability, and, consequently, toxicity. Within the last two decades, batchwise equilibrium-based single or sequential extraction schemes have been consolidated as analytical tools for fractionation analyses to assess...... occurring processes always take place under dynamic conditions, recent trends have been focused on the development of alternative flow-through dynamic methods aimed at mimicking environmental events more correctly than their classical extraction counterparts. In this lecture particular emphasis is paid...

  15. Method validation for control determination of mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry.

    Science.gov (United States)

    Torres, Daiane Placido; Martins-Teixeira, Maristela Braga; Cadore, Solange; Queiroz, Helena Müller

    2015-01-01

    A method for the determination of total mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry (TDA AAS) has been validated following international foodstuff protocols in order to fulfill the Brazilian National Residue Control Plan. The experimental parameters have been previously studied and optimized according to specific legislation on validation and inorganic contaminants in foodstuff. Linearity, sensitivity, specificity, detection and quantification limits, precision (repeatability and within-laboratory reproducibility), robustness as well as accuracy of the method have been evaluated. Linearity of response was satisfactory for the two range concentrations available on the TDA AAS equipment, between approximately 25.0 and 200.0 μg kg(-1) (square regression) and 250.0 and 2000.0 μg kg(-1) (linear regression) of mercury. The residues for both ranges were homoscedastic and independent, with normal distribution. Correlation coefficients obtained for these ranges were higher than 0.995. Limits of quantification (LOQ) and of detection of the method (LDM), based on signal standard deviation (SD) for a low-in-mercury sample, were 3.0 and 1.0 μg kg(-1), respectively. Repeatability of the method was better than 4%. Within-laboratory reproducibility achieved a relative SD better than 6%. Robustness of the current method was evaluated and pointed sample mass as a significant factor. Accuracy (assessed as the analyte recovery) was calculated on basis of the repeatability, and ranged from 89% to 99%. The obtained results showed the suitability of the present method for direct mercury measurement in fresh fish and shrimp samples and the importance of monitoring the analysis conditions for food control purposes. Additionally, the competence of this method was recognized by accreditation under the standard ISO/IEC 17025.

  16. A sensitive method for the determination of Sulfonamides in seawater samples by Solid Phase Extraction and UV-Visible spectrophotometry

    Science.gov (United States)

    Errayess, Sophia Ait; Lahcen, Abdellatif Ait; Idrissi, Laila; Marcoaldi, Caterina; Chiavarini, Salvatore; Amine, Aziz

    2017-06-01

    The authors have developed a sensitive spectrophotometric method for determination of sulfonamide derivatives such as sulfanilamide (SAA), sulfadiazine (SDZ), sulfacetamide (SCT) sulfamethoxazole (SMX), sulfamerazine (SMR), sulfadimethoxine (SDX), sulfamethiazole (SMT) and Sulfathiazole (STZ). This method is based on the Bratton-Marshall reaction, which involves the diazotization of sulfonamides with sodium nitrite under acidic conditions, followed by coupling with N-(1-naphtyl) ethylenediamine dihydrochloride (NED) to form a pink colored compound. Therefore, the Bratton-Marshall method was modified by optimizing the reaction conditions, which allows us to determine a low concentration range of sulfonamides compared to the reported methods. The limits of detection and quantification obtained were 0.019-0.05 and 0.06-0.16 μg mL- 1, respectively. In comparison with other reported methods using different coupling agents, the proposed method was found to be the most simple and sensitive for sulfonamides determination. In this paper, the modified method was successfully employed for the determination of sulfonamides in drinking water, seawater and pharmaceutical and veterinary formulations. The purpose of this work is to optimize and develop a simple method for extraction and concentration of sulfonamides present as residues in seawater and their quantification with the recommended spectrophotometric method. Solid phase extraction (SPE) of sulfonamides from seawater samples was evaluated using Oasis HLB cartridges (3 mL, 540 mg). The recovery efficiency was investigated in the sulfonamides concentration range comprised between 0.19 and 126 ng mL- 1. The ease of use of this extraction method makes it very useful for routine laboratory work.

  17. A sensitive method for the determination of Sulfonamides in seawater samples by Solid Phase Extraction and UV-Visible spectrophotometry.

    Science.gov (United States)

    Errayess, Sophia Ait; Lahcen, Abdellatif Ait; Idrissi, Laila; Marcoaldi, Caterina; Chiavarini, Salvatore; Amine, Aziz

    2017-06-15

    The authors have developed a sensitive spectrophotometric method for determination of sulfonamide derivatives such as sulfanilamide (SAA), sulfadiazine (SDZ), sulfacetamide (SCT) sulfamethoxazole (SMX), sulfamerazine (SMR), sulfadimethoxine (SDX), sulfamethiazole (SMT) and Sulfathiazole (STZ). This method is based on the Bratton-Marshall reaction, which involves the diazotization of sulfonamides with sodium nitrite under acidic conditions, followed by coupling with N-(1-naphtyl) ethylenediamine dihydrochloride (NED) to form a pink colored compound. Therefore, the Bratton-Marshall method was modified by optimizing the reaction conditions, which allows us to determine a low concentration range of sulfonamides compared to the reported methods. The limits of detection and quantification obtained were 0.019-0.05 and 0.06-0.16μgmL(-1), respectively. In comparison with other reported methods using different coupling agents, the proposed method was found to be the most simple and sensitive for sulfonamides determination. In this paper, the modified method was successfully employed for the determination of sulfonamides in drinking water, seawater and pharmaceutical and veterinary formulations. The purpose of this work is to optimize and develop a simple method for extraction and concentration of sulfonamides present as residues in seawater and their quantification with the recommended spectrophotometric method. Solid phase extraction (SPE) of sulfonamides from seawater samples was evaluated using Oasis HLB cartridges (3mL, 540mg). The recovery efficiency was investigated in the sulfonamides concentration range comprised between 0.19 and 126ngmL(-1). The ease of use of this extraction method makes it very useful for routine laboratory work. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Combination of dispersive liquid-liquid microextraction and solid-phase microextraction: An efficient hyphenated sample preparation method.

    Science.gov (United States)

    Jafari, Mohammad T; Saraji, Mohammad; Mossaddegh, Mehdi

    2016-09-30

    Two well-known microextraction methods, dispersive liquid-liquid microextraction (DLLME) and solid-phase microextraction (SPME), were combined, resulting in as an encouraging method. The method, named DLLME-SPME, was performed based on total vaporization technique. For the DLLME step, 1,1,2,2-tetrachloroethane and acetonitrile were used as extraction and disperser solvents, respectively. Halloysite nanotubes-titanium dioxide was used as the fiber coating in the SPME step. The method was applied for the extraction of diazinon and parathion (as the test compounds) in environmental water samples and fruit juices, and gas chromatography-corona discharge ion mobility spectrometry was used as the determination apparatus. Desorption temperature and time, extraction temperature and time, and the volume of the extracting solvent in the DLLME step were optimized as the effective parameters on the extraction efficiency. The relative standard deviations (RSDs) of intra-day were found to be 4-7% and 6-8% for diazinon and parathion, respectively. Also, the RSDs of inter-day were 7-9% and 8-10% for diazinon and parathion, respectively. The limits of quantification and detection were obtained to be 0.015 and 0.005μgL(-1) for diazinon, and 0.020 and 0.007μgL(-1) for parathion. A good linearity range (r(2)˃0.993) was obtained in the range of 0.015-3.000 and 0.020-3.000μgL(-1) for diazinon and parathion, respectively. The high enrichment factors were obtained as 3150 and 2965 for diazinon and parathion, respectively. This method showed high sensitivity with good recovery values (between 87 and 99%) for the extraction of target analytes in the real samples. Overall, the results revealed that the developed DLLME-SPME method had better extraction efficiency than DLLME and SPME alone. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Solid matrix transformation and tracer addition using molten ammonium bifluoride salt as a sample preparation method for laser ablation inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Grate, Jay W; Gonzalez, Jhanis J; O'Hara, Matthew J; Kellogg, Cynthia M; Morrison, Samuel S; Koppenaal, David W; Chan, George C-Y; Mao, Xianglei; Zorba, Vassilia; Russo, Richard E

    2017-09-08

    Solid sampling and analysis methods, such as laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), are challenged by matrix effects and calibration difficulties. Matrix-matched standards for external calibration are seldom available and it is difficult to distribute spikes evenly into a solid matrix as internal standards. While isotopic ratios of the same element can be measured to high precision, matrix-dependent effects in the sampling and analysis process frustrate accurate quantification and elemental ratio determinations. Here we introduce a potentially general solid matrix transformation approach entailing chemical reactions in molten ammonium bifluoride (ABF) salt that enables the introduction of spikes as tracers or internal standards. Proof of principle experiments show that the decomposition of uranium ore in sealed PFA fluoropolymer vials at 230 °C yields, after cooling, new solids suitable for direct solid sampling by LA. When spikes are included in the molten salt reaction, subsequent LA-ICP-MS sampling at several spots indicate that the spikes are evenly distributed, and that U-235 tracer dramatically improves reproducibility in U-238 analysis. Precisions improved from 17% relative standard deviation for U-238 signals to 0.1% for the ratio of sample U-238 to spiked U-235, a factor of over two orders of magnitude. These results introduce the concept of solid matrix transformation (SMT) using ABF, and provide proof of principle for a new method of incorporating internal standards into a solid for LA-ICP-MS. This new approach, SMT-LA-ICP-MS, provides opportunities to improve calibration and quantification in solids based analysis. Looking forward, tracer addition to transformed solids opens up LA-based methods to analytical methodologies such as standard addition, isotope dilution, preparation of matrix-matched solid standards, external calibration, and monitoring instrument drift against external calibration standards.

  20. Determination of chemical oxygen demand in heterogeneous solid or semisolid samples using a novel method combining solid dilutions as a preparation step followed by optimized closed reflux and colorimetric measurement.

    Science.gov (United States)

    Noguerol-Arias, Joan; Rodríguez-Abalde, Angela; Romero-Merino, Eva; Flotats, Xavier

    2012-07-03

    This paper reports the development of an innovative sample preparation method for the determination of the chemical oxygen demand (COD) in heterogeneous solid or semisolid samples, with high suspended solids and COD concentrations, using an optimized closed reflux colorimetric method. The novel method, named solid dilution (SD), is based on a different technique of sample preparation, diluting the sample with magnesium sulfate (MgSO(4)) previous to COD determination. With this, it is possible to obtain a solid homogeneous mixture much more easily analyzable. Besides, a modification of concentration and ratio of reagents was optimized to make the closed reflux colorimetric method suitable for complex substrates with COD levels ranging from 5 to 2500 g O(2) kg(-1) TS. The optimized method has been tested with potassium hydrogen phthalate (KHP) as primary solid standard and using different solid or semiliquid substrates like pig slaughterhouse waste and sewage sludge, among others. Finally, the optimized method (SD/SM-CRC) was intensively tested in comparison to the standard titrimetric method (SM-ORT) using different certified reference materials (CRM). The developed method was found to give higher accuracy, 1.4% relative standard deviation (RSD) vs 10.4%, and bias of 2.8% vs 8.0%, in comparison to the standard open reflux titrimetric method.

  1. [A solid-state reference sample of iodine radionuclide activity for checking radiometers and a method for its production].

    Science.gov (United States)

    Sichkar', G A

    1993-01-01

    This development relates to nuclear engineering, concerns the sources of ionizing radiation of iodine radionuclides and the ways of their manufacture. The iodine radionuclides are used for calibration of radiometers that measure the specific activity of iodine radionuclide in biological specimens, in particular for their use to identify noncancer diseases. The purpose of the paper is to design a routine activity sample for iodine radionuclide in the solid-state source for transfer of an iodine radionuclide activity unit from the reference iodine radionuclide activity unit to an operating meter with a simultaneous decrease in testing errors and an increase, in terms of iodine radionuclide half-life, in the life of the reference sample by stabilizing the activity unit of iodine radionuclide (in terms of its half-life) by eliminating the process of sublimation of iodine radionuclide from the working surface of the source. The objective is achieved by the fact that the radionuclide is replaced on the lower internal build-up part of the container, fixed with the upper internal build-up part, then kept for at least 10-12 hours at least at 18-20 degrees C, packed into a hollow container and sealed with epoxide resin. According to the proposed technical design, reference activity samples of iodine radionuclide in the solid-state radiometric source with a preset activity value have been prepared. The testing error for iodine radionuclide activity is minimal and equal to 1.0-3.0% at a 0.95 confidence.

  2. Analysis of Wastewater Samples Using Disk Solid-Phase Extraction (SPE) Following US EPA Method 608.3

    National Research Council Canada - National Science Library

    William R Jones; Zoe A Grosser

    2017-01-01

    Since the use of a halogen-specific detector precludes use of a chlorinated solvent for the sample, the method specifies solvent exchange from methylene chloride into hexane before the analysis step...

  3. Comparison of atomic absorption, mass and X-ray spectrometry techniques using dissolution-based and solid sampling methods for the determination of silver in polymeric samples

    Energy Technology Data Exchange (ETDEWEB)

    Schrijver, Isabel de [Ghent University, Department of Analytical Chemistry, Krijgslaan 281-S12, B-9000 Ghent (Belgium); University College West-Flanders, Department of Industrial Engineering and Technology, Research group EnBiChem, Graaf Karel de Goedelaan 5, B-8500 Kortrijk (Belgium); Aramendia, Maite; Vincze, Laszlo [Ghent University, Department of Analytical Chemistry, Krijgslaan 281-S12, B-9000 Ghent (Belgium); Resano, Martin [University of Zaragoza, Department of Analytical Chemistry, Pedro Cerbuna 12, E-50009 Zaragoza (Spain); Dumoulin, Ann [University College West-Flanders, Department of Industrial Engineering and Technology, Research group EnBiChem, Graaf Karel de Goedelaan 5, B-8500 Kortrijk (Belgium); Vanhaecke, Frank [Ghent University, Department of Analytical Chemistry, Krijgslaan 281-S12, B-9000 Ghent (Belgium)], E-mail: Frank.Vanhaecke@UGent.be

    2007-11-15

    In this work, the capabilities and limitations of solid sampling techniques - laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS), wavelength dispersive X-ray fluorescence spectrometry (WD-XRFS) and solid sampling electrothermal atomic absorption spectrometry (SS-ETAAS) - for the determination of silver in polymers have been evaluated and compared to those of acid digestion and subsequent Ag determination using pneumatic nebulization ICPMS (PN-ICPMS) or flame AAS (FAAS). In a first stage, two dissolution procedures were examined: conventional acid digestion in a Kjeldahl flask and the combination of dry ashing and microwave-assisted digestion. Accurate results for Ag could be obtained, although occasionally, problems of analyte losses and/or incomplete dissolution were observed. LA-ICPMS shows potential for direct analysis of solid materials, but calibration was found to be difficult. A polypropylene sample was used as standard. This approach provided satisfactory results for other polypropylene samples and even for other types of plastics, provided that the {sup 13}C{sup +} signal was used as internal reference, correcting for variations in ablation efficiency. However, the results for polyoxymethylene were overestimated. Similar calibration problems appeared with WD-XRFS, due to differences in absorption efficiency of X-rays. In this case, the accuracy could be improved by using a matrix correction procedure, which however required the matrix composition to be known into sufficient detail. SS-ETAAS, proved to be a fast approach that allowed accurate determination of Ag in polymers using aqueous standard solutions for calibration. Due to the high Ag content and the excellent sensitivity, the use of a 3-field mode Zeeman-effect background correction system was essential for the extension of the working range.

  4. Characterization of solid heterogeneous waste fuel - the effect of sampling and preparation method; Karaktaerisering av fasta inhomogena avfallsbraenslen - inverkan av metoder foer provtagning och provberedning

    Energy Technology Data Exchange (ETDEWEB)

    Wikstroem-Blomqvist, Evalena; Franke, Jolanta; Johansson, Ingvar

    2007-12-15

    The aim of the project is to evaluate the possibilities to simplify the methods used during sampling and laboratory preparation of heterogeneous waste materials. Existing methods for solid fuel material is summarized and evaluated in the project. As a result of the project two new simplified methods, one for field sampling and one for laboratory preparation work has been suggested. One large challenge regarding waste sampling is to achieve a representative sample due to the considerable heterogeneity of the material. How do you perform a sampling campaign that will give rise to representative results without too large costs? The single largest important source of error is the sampling procedure, equivalent to about 80% of the total error. Meanwhile the sample reduction and laboratory work only represents 15 % and 5 % respectively. Thus, to minimize the total error it is very important that the sampling is well planned in a testing program. In the end a very small analytical sample (1 gram) should reflected a large heterogeneous sample population of 1000 of tons. In this project two sampling campaigns, the fall of 2006 and early winter 2007, were conducted at the waste power plant Renova in Gothenburg, Sweden. The first campaign consisted of three different sample sizes with different number of sub-samples. One reference sample (50 tons and 48 sub-samples), two samples consisting of 16 tons and 8 sub-samples and finally two 4 tons consisting of 2 sub-samples each. During the second sampling campaign, four additional 4 ton samples were taken to repeat and thus evaluate the simplified sampling method. This project concludes that the simplified sampling methods only consisting of two sub-samples and a total sample volume of 4 tons give rise to results with as good quality and precision is the more complicated methods tested. Moreover the results from the two sampling campaigns generated equivalent results. The preparation methods used in the laboratory can as well be

  5. Evaluation of ultrasound-assisted in situ sorbent formation solid-phase extraction method for determination of arsenic in water, food and biological samples.

    Science.gov (United States)

    Ezoddin, Maryam; Majidi, Behrooz; Abdi, Khosrou

    2015-01-01

    A simple and rapid ultrasound-assisted in situ sorbent formation solid-phase extraction (UAISFSPE) coupled with electrothermal atomic absorption spectrometry detection (ET-AAS) was developed for preconcentration and determination of arsenic (As) in various samples. A small amount of cationic surfactant is dissolved in the aqueous sample containing As ions, which were complexed by ammonium pyrrolidinedithiocarbamate After shaking, a little volume of hexafluorophosphate (NaPF6) as an ion-pairing agent was added into the solution by a microsyringe. Due to the interaction between surfactant and ion-pairing agent, solid particles are formed. The alkyl groups of the surfactant in the solid particles strongly interact with the hydrophobic groups of analytes and become bound. Sonication aids the dispersion of the sorbent into the sample solution and mass transfer of the analyte into the sorbent, thus reducing the extraction time. The solid particles are centrifuged, and the sedimented particles can be dissolved in an appropriate solvent to recover the absorbed analyte. After separation, total arsenic (As(III) and As(V)) was determined by ET-AAS. Several experimental parameters were investigated and optimized. A detection limit of 7 ng L(-1) with preconcentration factor of 100 and relative standard deviation for 10 replicate determinations of 0.1 µg L(-1) As(III) were 4.5% achieved. Consequently, the method was applied to the determination of arsenic in certified reference materials, water, food and biological samples with satisfactory results.

  6. Assessing total and volatile solids in municipal solid waste samples.

    Science.gov (United States)

    Peces, M; Astals, S; Mata-Alvarez, J

    2014-01-01

    Municipal solid waste is broadly generated in everyday activities and its treatment is a global challenge. Total solids (TS) and volatile solids (VS) are typical control parameters measured in biological treatments. In this study, the TS and VS were determined using the standard methods, as well as introducing some variants: (i) the drying temperature for the TS assays was 105°C, 70°C and 50°C and (ii) the VS were determined using different heating ramps from room tempature to 550°C. TS could be determined at either 105°C or 70°C, but oven residence time was tripled at 70°C, increasing from 48 to 144 h. The VS could be determined by smouldering the sample (where the sample is burnt without a flame), which avoids the release of fumes and odours in the laboratory. However, smouldering can generate undesired pyrolysis products as a consequence of carbonization, which leads to VS being underestimated. Carbonization can be avoided using slow heating ramps to prevent the oxygen limitation. Furthermore, crushing the sample cores decreased the time to reach constant weight and decreased the potential to underestimate VS.

  7. Extraction and RT-qPCR detection of enteroviruses from solid environmental matrixes: Method decision tree for different sample types and viral concentrations.

    Science.gov (United States)

    Martín-Díaz, Julia; Lucena, Francisco

    2018-01-01

    Quantitative RT-PCR methods (RT-qPCR) are becoming increasingly desirable for the detection of enteric viruses in solid environmental matrixes such as sediments, soils and sewage sludge. However, effective methodologies that allow the extraction of high quality RNA ready for molecular quantification continue to be evaluated. In the present study, four different methods for enterovirus extraction from solid environmental matrixes were compared in terms of viral recovery and inhibitor removal. Three indirect methods based on glycine elution and concentration by ultracentrifugation were tested. The main differences between indirect methods were the sample to glycine buffer ratio, and the ultracentrifugation protocol applied. One commercial direct method was also tested. The indirect methods produced better results than the direct method. The ultracentrifugation led to viral losses in samples with high titers; however, as the virus concentration reduced, the ultracentrifugation became increasingly important for viral recovery. Two commercial RNA extraction kits were also evaluated and it was selected the most effective in removing RT-qPCR inhibitors. The results obtained allowed the development of a method decision tree with three versions that are suitable for different samples and viral concentrations. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Solid Matrix Transformation and Tracer Addition using Molten Ammonium Bifluoride Salt as a Sample Preparation Method for Laser Ablation Inductively Coupled Plasma Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Grate, Jay W.; Gonzalez, Jhanis J.; O' Hara, Matthew J.; Kellogg, Cynthia M.; Morrison, Samuel S.; Koppenaal, David W.; Chan, George C.; Mao, Xianglei; Zorba, Vassilia; Russo, Richard

    2017-09-08

    Laser ablation (LA) is a means of sample introduction to inductively coupled plasma (ICP) mass spectrometry (MS) that avoids acid dissolution and chemical separation steps conventionally associated with solid sample analysis. At the same time, certain features of LA-ICP-MS are often mentioned in critical reviews including solid matrix variability and its influence on the ablation process, matrix dependent elemental fractionation, lack of matrix matched standards for external calibration, and limitations to internal calibration because it is challenging to add and distribute spikes into solid samples. In this paper we introduce the concept of a synergistic minimal sample preparation method that is used in combination with LA-ICP-MS as a means to overcome these limitations. The aim of this minimal sample preparation procedure is to reactively transform the original matrix to a more consistent matrix for LA-based analysis, thus reducing the effects of matrix variability, while enabling the addition of tracers. In conjunction with ICP-MS, we call this MTR-LA-ICP-MS, where MTR is derived from matrix transformation including the option to add tracers

  9. Comparison of the solid phase and liquid-liquid extraction methods for methadone determination in human serum and whole blood samples using gas chromatography/mass spectrometry.

    Science.gov (United States)

    Bratinčević, Maja Veršić; Visković, Tanja; Sutlović, Davorka

    2017-12-20

    The aim of this study was to determine the optimal biological sample and the optimal extraction technique for monitoring methadone concentrations in biological samples. We analysed methadone in serum and whole blood samples using gas chromatography/mass spectrometry (GC/MS). Before analysis, we compared five solid-phase extraction (SPE) and two liquid-liquid extraction (LLE) methods and determined that SPE with Supelco LC-18 in serum yielded the best extraction efficiency. The limit of detection was 10 ng mL-1 and the limit of quantification 25 ng mL-1. Correlation coefficient was over 0.999 for the methadone calibration curve in linear range from 50 to 2000 ng mL-1. Intra and inter-day accuracy and precision of the method was satisfactory. The method was successfully applied for determining serum methadone in patients on maintenance therapy.

  10. A sensitive method for determining total vanadium in water samples using colorimetric-solid-phase extraction-fiber optic reflectance spectroscopy.

    Science.gov (United States)

    Filik, Hayati; Yanaz, Zeynep

    2009-12-30

    A selective colorimetric-solid-phase extraction (C-SPE) method for the determination of total vanadium in water samples was developed. This method introduced a new variation of C-SPE. The colour reaction is based on the reaction of vanadium(V) ternary complex formed with 1-(2-Pyridylazo)-2-naphtol (PAN) in the presence hydrogen peroxide (H(2)O(2)). In this technique, the target analytes in samples are extracted onto solid matrix loaded with a colorimetric reagent and then quantified directly on the adsorbent surface by using a miniature fiber optic reflectance spectrometer. The measurements were carried out at a wavelength of 589.4 nm since it yielded the largest divergence different in reflectance spectra before and after reaction with the vanadium. The overall time required for the C-SPE procedure was approximately 20 min. The amount of concentrated V is then determined in a few seconds by using miniature reflectance spectrometer. At the optimal conditions, a calibration curve was constructed, revealing a linear range of 0.05-0.52 mg L(-1) and a detection limit as low as 0.01 mg L(-1) while the RSD lower than 2.8%. In order to verify the accuracy of the method, a certified reference water samples (TMDA) were analysed and the results obtained were in good agreement with the certified values. The proposed method was applied to the determination of vanadium in tap water, seawater samples with a recovery for the spiked samples in the range of 98-102%.

  11. Improved sample preparation of glyphosate and methylphosphonic acid by EPA method 6800A and time-of-flight mass spectrometry using novel solid-phase extraction.

    Science.gov (United States)

    Wagner, Rebecca; Wetzel, Stephanie J; Kern, John; Kingston, H M Skip

    2012-02-01

    The employment of chemical weapons by rogue states and/or terrorist organizations is an ongoing concern in the United States. The quantitative analysis of nerve agents must be rapid and reliable for use in the private and public sectors. Current methods describe a tedious and time-consuming derivatization for gas chromatography-mass spectrometry and liquid chromatography in tandem with mass spectrometry. Two solid-phase extraction (SPE) techniques for the analysis of glyphosate and methylphosphonic acid are described with the utilization of isotopically enriched analytes for quantitation via atmospheric pressure chemical ionization-quadrupole time-of-flight mass spectrometry (APCI-Q-TOF-MS) that does not require derivatization. Solid-phase extraction-isotope dilution mass spectrometry (SPE-IDMS) involves pre-equilibration of a naturally occurring sample with an isotopically enriched standard. The second extraction method, i-Spike, involves loading an isotopically enriched standard onto the SPE column before the naturally occurring sample. The sample and the spike are then co-eluted from the column enabling precise and accurate quantitation via IDMS. The SPE methods in conjunction with IDMS eliminate concerns of incomplete elution, matrix and sorbent effects, and MS drift. For accurate quantitation with IDMS, the isotopic contribution of all atoms in the target molecule must be statistically taken into account. This paper describes two newly developed sample preparation techniques for the analysis of nerve agent surrogates in drinking water as well as statistical probability analysis for proper molecular IDMS. The methods described in this paper demonstrate accurate molecular IDMS using APCI-Q-TOF-MS with limits of quantitation as low as 0.400 mg/kg for glyphosate and 0.031 mg/kg for methylphosphonic acid. Copyright © 2012 John Wiley & Sons, Ltd.

  12. Sample Results from MCU Solids Outage

    Energy Technology Data Exchange (ETDEWEB)

    Peters, T.; Washington, A.; Oji, L.; Coleman, C.; Poirier, M.

    2014-09-22

    Savannah River National Laboratory (SRNL) has received several solid and liquid samples from MCU in an effort to understand and recover from the system outage starting on April 6, 2014. SRNL concludes that the presence of solids in the Salt Solution Feed Tank (SSFT) is the likely root cause for the outage, based upon the following discoveries: A solids sample from the extraction contactor #1 proved to be mostly sodium oxalate; A solids sample from the scrub contactor#1 proved to be mostly sodium oxalate; A solids sample from the Salt Solution Feed Tank (SSFT) proved to be mostly sodium oxalate; An archived sample from Tank 49H taken last year was shown to contain a fine precipitate of sodium oxalate; A solids sample from ; A liquid sample from the SSFT was shown to have elevated levels of oxalate anion compared to the expected concentration in the feed. Visual inspection of the SSFT indicated the presence of precipitated or transferred solids, which were likely also in the Salt Solution Receipt Tank (SSRT). The presence of the solids coupled with agitation performed to maintain feed temperature resulted in oxalate solids migration through the MCU system and caused hydraulic issues that resulted in unplanned phase carryover from the extraction into the scrub, and ultimately the strip contactors. Not only did this carryover result in the Strip Effluent (SE) being pushed out of waste acceptance specification, but it resulted in the deposition of solids into several of the contactors. At the same time, extensive deposits of aluminosilicates were found in the drain tube in the extraction contactor #1. However it is not known at this time how the aluminosilicate solids are related to the oxalate solids. The solids were successfully cleaned out of the MCU system. However, future consideration must be given to the exclusion of oxalate solids into the MCU system. There were 53 recommendations for improving operations recently identified. Some additional considerations or

  13. Optimization of a method based on micro-matrix solid-phase dispersion (micro-MSPD for the determination of PCBs in mussel samples

    Directory of Open Access Journals (Sweden)

    Nieves Carro

    2017-03-01

    Full Text Available This paper reports the development and optimization of micro-matrix solid-phase dispersion (micro-MSPD of nine polychlorinated biphenyls (PCBs in mussel samples (Mytilus galloprovincialis by using a two-level factorial design. Four variables (amount of sample, anhydrous sodium sulphate, Florisil and solvent volume were considered as factors in the optimization process. The results suggested that only the interaction between the amount of anhydrous sodium sulphate and the solvent volume was statistically significant for the overall recovery of a trichlorinated compound, CB 28. Generally most of the considered species exhibited a similar behaviour, the sample and Florisil amounts had a positive effect on PCBs extractions and solvent volume and sulphate amount had a negative effect. The analytical determination and confirmation of PCBs were carried out by using GC-ECD and GC-MS/MS, respectively. The method was validated having satisfactory precision and accuracy with RSD values below 6% and recoveries between 81 and 116% for all congeners. The optimized method was applied to the extraction of real mussel samples from two Galician Rías.

  14. Development of a novel monolith frit-based solid-phase microextraction method for determination of hexanal and heptanal in human serum samples.

    Science.gov (United States)

    Xu, Hui; Yan, Zhihua; Song, Dandan

    2012-03-01

    In this paper, a polypropylene frit with porous network structure and high area-to-thickness ratio (4.8 mm diameter, 1.6 mm thickness, 20 mm pore size) was utilized as a mould of monolith. Poly(methacrylic acid-ethlyene glycol dimethacrylate) (MAA-EGDMA) monolith was in situ synthesized in the micro-channel of frit by photopolymerization. A monolith frit-based solid-phase microextraction method (SPME) was developed for the determination of hexanal and heptanal in serum samples by combining with high-performance liquid chromatography. 2,4-Dinitrophenylhydrazine (DNPH) as the derivatizing reagent was absorbed on a monolith frit, then its derivatization reaction with aldehydes and the absorption of formed hydrazones on the monolith disk occurred simultaneously. The condition parameters for polymerization, derivatization and extraction were optimized systematically. Under the optimum conditions, rigid structure, low back-pressure and high column capacity were achieved for the monolith frit. The limits of detection for hexanal and heptanal were 1.86 and 1.38 nmol/L, respectively. The inter- and intra-day relative standard deviations were less than 7.7% (n = 6). This method was applied successfully to aldehydes analysis in human serum samples. The method possesses advantages such as simplicity, efficiency, low cost and good biocompatibility. It provides an alternative approach for quantification of aldehydes in complex biological samples. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. A new supramolecular based liquid solid microextraction method for preconcentration and determination of trace bismuth in human blood serum and hair samples by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Kahe, Hadi; Chamsaz, Mahmoud

    2016-11-01

    A simple and reliable supramolecule-aggregated liquid solid microextraction method is described for preconcentration and determination of trace amounts of bismuth in water as well as human blood serum and hair samples. Catanionic microstructures of cetyltrimethylammonium bromide (CTAB) and sodium dodecyl sulfate (SDS) surfactants, dissolved in deionized water/propanol, are used as a green solvent to extract bismuth (III)-diethyldithiocarbamate complexes by dispersive microextraction methodology. The extracted solid phase is easily removed and dissolved in 50 μL propanol for subsequent measurement by electrothermal atomic absorption spectrometry (ET-AAS). The procedure benefits the merits of supramolecule aggregates' properties and dispersive microextraction technique using water as the main component of disperser solvent, leading to direct interaction with analyte. Phase separation behavior of extraction solvent and different parameters influencing the extraction efficiency of bismuth ion such as salt concentration, pH, centrifugation time, amount of chelating agent, SDS:CTAB mole ratio, and solvent amounts were thoroughly optimized. Under the optimal experimental conditions, the calibration curve was linear in the range of 0.3-6 μg L-1 Bi (III) with a limit of detection (LOD) of 0.16 μg L-1 (S/N = 3). The relative standard deviations (RSD) of determination were obtained to be 5.1 and 6.2 % for 1 and 3 μg L-1 of Bi (III), respectively. The developed method was successfully applied as a sensitive and accurate technique for determination of bismuth ion in human blood serum, hair samples, and a certified reference material.

  16. Method development for the control determination of mercury in seafood by solid-sampling thermal decomposition amalgamation atomic absorption spectrometry (TDA AAS).

    Science.gov (United States)

    Torres, D P; Martins-Teixeira, M B; Silva, E F; Queiroz, H M

    2012-01-01

    A very simple and rapid method for the determination of total mercury in fish samples using the Direct Mercury Analyser DMA-80 was developed. In this system, a previously weighted portion of fresh fish is combusted and the released mercury is selectively trapped in a gold amalgamator. Upon heating, mercury is desorbed from the amalgamator, an atomic absorption measurement is performed and the mercury concentration is calculated. Some experimental parameters have been studied and optimised. In this study the sample mass was about 100.0 mg. The relative standard deviation was lower than 8.0% for all measurements of solid samples. Two calibration curves against aqueous standard solutions were prepared through the low linear range from 2.5 to 20.0 ng of Hg, and the high linear range from 25.0 to 200.0 ng of Hg, for which a correlation coefficient better than 0.997 was achieved, as well as a normal distribution of the residuals. Mercury reference solutions were prepared in 5.0% v/v nitric acid medium. Lyophilised fish tissues were also analysed; however, the additional procedure had no advantage over the direct analysis of the fresh fish, and additionally increased the total analytical process time. A fish tissue reference material, IAEA-407, was analysed and the mercury concentration was in agreement with the certified value, according to the t-test at a 95% confidence level. The limit of quantification (LOQ), based on a mercury-free sample, was 3.0 µg kg(-1). This LOQ is in accordance with performance criteria required by the Commission Regulation No. 333/2007. Simplicity and high efficiency, without the need for any sample preparation procedure, are some of the qualities of the proposed method.

  17. Shift-excitation Raman difference spectroscopy-difference deconvolution method for the luminescence background rejection from Raman spectra of solid samples.

    Science.gov (United States)

    Osticioli, Iacopo; Zoppi, Angela; Castellucci, Emilio Mario

    2007-08-01

    The feasibility of the shift-excitation Raman difference spectroscopy-difference deconvolution (SERDS-DDM) method for fluorescence suppression from Raman spectra of solid samples is discussed. For SERDS measurements a tunable diode laser source with an emission band centered at 684 nm is coupled to a conventional micro-Raman apparatus and a monochromator device is used for checking the excitation frequency stability. The shifted Raman spectra are then mathematically treated and a deconvolution procedure is used to reconstruct the Raman spectrum devoid of fluorescence. Two different cases are presented. In the first one, fluorescence is intrinsic to the sample and the Raman spectrum of cinnabar pigment is finally reconstructed. In the second, the presence of an external luminescence background in the spectrum of a pure sulfur crystal is considered. The SERDS-DDM reconstructed spectra are compared with spectra obtained via multi-point baseline subtraction and a significant improvement in the detection of weak bands is demonstrated. Practical insights for the application of this method are presented as well.

  18. Sampling system and method

    Science.gov (United States)

    Decker, David L.; Lyles, Brad F.; Purcell, Richard G.; Hershey, Ronald Lee

    2013-04-16

    The present disclosure provides an apparatus and method for coupling conduit segments together. A first pump obtains a sample and transmits it through a first conduit to a reservoir accessible by a second pump. The second pump further conducts the sample from the reservoir through a second conduit.

  19. Fluidics platform and method for sample preparation

    Science.gov (United States)

    Benner, Henry W.; Dzenitis, John M.

    2016-06-21

    Provided herein are fluidics platforms and related methods for performing integrated sample collection and solid-phase extraction of a target component of the sample all in one tube. The fluidics platform comprises a pump, particles for solid-phase extraction and a particle-holding means. The method comprises contacting the sample with one or more reagents in a pump, coupling a particle-holding means to the pump and expelling the waste out of the pump while the particle-holding means retains the particles inside the pump. The fluidics platform and methods herein described allow solid-phase extraction without pipetting and centrifugation.

  20. Method development for the determination of bromine in coal using high-resolution continuum source graphite furnace molecular absorption spectrometry and direct solid sample analysis

    Science.gov (United States)

    Pereira, Éderson R.; Castilho, Ivan N. B.; Welz, Bernhard; Gois, Jefferson S.; Borges, Daniel L. G.; Carasek, Eduardo; de Andrade, Jailson B.

    2014-06-01

    This work reports a simple approach for Br determination in coal using direct solid sample analysis in a graphite tube furnace and high-resolution continuum source molecular absorption spectrometry. The molecular absorbance of the calcium mono-bromide (CaBr) molecule has been measured using the rotational line at 625.315 nm. Different chemical modifiers (zirconium, ruthenium, palladium and a mixture of palladium and magnesium nitrates) have been evaluated in order to increase the sensitivity of the CaBr absorption, and Zr showed the best overall performance. The pyrolysis and vaporization temperatures were 800 °C and 2200 °C, respectively. Accuracy and precision of the method have been evaluated using certified coal reference materials (BCR 181, BCR 182, NIST 1630a, and NIST 1632b) with good agreement (between 98 and 103%) with the informed values for Br. The detection limit was around 4 ng Br, which corresponds to about 1.5 μg g- 1 Br in coal, based on a sample mass of 3 mg. In addition, the results were in agreement with those obtained using electrothermal vaporization inductively coupled plasma mass spectrometry, based on a Student t-test at a 95% confidence level. A mechanism for the formation of the CaBr molecule is proposed, which might be considered for other diatomic molecules as well.

  1. Solid-Phase Extraction Spectrophotometric Determination of Total Antioxidant Capacity in Antioxidant-poor Samples by Using the Ferric-Ferrozine Method.

    Science.gov (United States)

    Berker, Kadriye Isil; Ozyurt, Dilek; Demirata, Birsen; Apak, Resat

    2017-01-01

    Ferrozine (FZ) preferentially stabilizes Fe(II) over Fe(III) to raise the ferric reduction potential and oxidize antioxidants. The advantages of the ferric-ferrozine method over other iron-based total antioxidant capacity assays were: (i) higher molar absorptivity and enhanced sensitivity, (ii) lower interference from foreign ions, (iii) wide pH tolerance (iv) additivity of the absorbances for mixtures. Solid-phase extraction (SPE) could be combined with spectrophotometry, because the magenta-colored anionic Fe(II)-FZ complex was quantitatively sorbed on Sephadex QAE A-25 resin. The sensitivity enhancement using the resin enabled us to conduct total antioxidant capacity (TAC) measurements of antioxidant-poor samples. The apparent molar absorptivity, linear concentration range and trolox equivalent antioxidant capacities (TEAC) of certain antioxidants were found. The calibration curves (lines) of trolox, rutin, and rosmarinic acid individually and in herbal infusions-by using the method of standard additions-were parallel, confirming that the added antioxidants did not interact with herbal constituents to cause chemical deviations from Beer's law.

  2. Sampling system and method

    Energy Technology Data Exchange (ETDEWEB)

    Decker, David L.; Lyles, Brad F.; Purcell, Richard G.; Hershey, Ronald Lee

    2017-03-07

    In one embodiment, the present disclosure provides an apparatus and method for supporting a tubing bundle during installation or removal. The apparatus includes a clamp for securing the tubing bundle to an external wireline. In various examples, the clamp is external to the tubing bundle or integral with the tubing bundle. According to one method, a tubing bundle and wireline are deployed together and the tubing bundle periodically secured to the wireline using a clamp. In another embodiment, the present disclosure provides an apparatus and method for coupling conduit segments together. A first pump obtains a sample and transmits it through a first conduit to a reservoir accessible by a second pump. The second pump further conducts the sample from the reservoir through a second conduit. In a specific example, one or more clamps are used to connect the first and/or second conduits to an external wireline.

  3. Analysis of solid uranium samples using a small mass spectrometer

    Science.gov (United States)

    Kahr, Michael S.; Abney, Kent D.; Olivares, José A.

    2001-07-01

    A mass spectrometer for isotopic analysis of solid uranium samples has been constructed and evaluated. This system employs the fluorinating agent chlorine trifluoride (ClF 3) to convert solid uranium samples into their volatile uranium hexafluorides (UF 6). The majority of unwanted gaseous byproducts and remaining ClF 3 are removed from the sample vessel by condensing the UF 6 and then pumping away the unwanted gases. The UF 6 gas is then introduced into a quadrupole mass spectrometer and ionized by electron impact ionization. The doubly charged bare metal uranium ion (U 2+) is used to determine the U 235/U 238 isotopic ratio. Precision and accuracy for several isotopic standards were found to be better than 12%, without further calibration of the system. The analysis can be completed in 25 min from sample loading, to UF 6 reaction, to mass spectral analysis. The method is amenable to uranium solid matrices, and other actinides.

  4. Radioactive air sampling methods

    CERN Document Server

    Maiello, Mark L

    2010-01-01

    Although the field of radioactive air sampling has matured and evolved over decades, it has lacked a single resource that assimilates technical and background information on its many facets. Edited by experts and with contributions from top practitioners and researchers, Radioactive Air Sampling Methods provides authoritative guidance on measuring airborne radioactivity from industrial, research, and nuclear power operations, as well as naturally occuring radioactivity in the environment. Designed for industrial hygienists, air quality experts, and heath physicists, the book delves into the applied research advancing and transforming practice with improvements to measurement equipment, human dose modeling of inhaled radioactivity, and radiation safety regulations. To present a wide picture of the field, it covers the international and national standards that guide the quality of air sampling measurements and equipment. It discusses emergency response issues, including radioactive fallout and the assets used ...

  5. Development of a new sample preparation method based on liquid-liquid-liquid extraction combined with dispersive liquid-liquid microextraction and its application on unfiltered samples containing high content of solids.

    Science.gov (United States)

    Farajzadeh, Mir Ali; Abbaspour, Maryam

    2017-11-01

    A new sample preparation method based on liquid-liquid-liquid extraction combined with dispersive liquid-liquid microextraction followed by gas chromatography-flame ionization detection has been reported for the extraction/preconcentration and determination of trace levels of twelve pesticide residues from different samples with high content of solids without filtration. This method consists of a three-phase system including an aqueous phase (sample solution), acetonitrile, and hexane. The extraction mechanism is based on different affinities of the substances from the sample matrices towards each of the involved phase, which provides a high selectivity to the process. In other words, interfering hydrophobic compounds are transferred into hexane and will not be present in the final extract. Furthermore, ionic and polar compounds are retained in the aqueous phase. Therefore, only semi-polar compounds such as the studied pesticides are extracted into acetonitrile. In this method, a homogeneous solution of the aqueous phase and acetonitrile (a water-soluble extraction solvent) forms two clearly separated phases in the presence of sodium sulfate (as a phase separation agent) and simultaneously the analytes are extracted into the fine droplets of the acetonitrile collected on the surface of the aqueous phase. To achieve high enrichment factors, the acetonitrile phase is mixed with 1,2-dibromoethane (as a preconcentration solvent) at µL-level to perform the following dispersive liquid-liquid microextraction procedure. Several parameters that can affect extraction efficiency including kind and volume of extraction solvent, type and concentration of phase separation agent, hexane volume, kind of preconcentration solvent, and ionic strength were studied and optimized. Under the optimal conditions, extraction recoveries were obtained in the range of 53-93% and the calibration curves were linear in wide ranges with correlation coefficients ≥ 0.9983. Intra- (n = 6) and

  6. Solid phase microextraction fills the gap in tissue sampling protocols.

    Science.gov (United States)

    Bojko, Barbara; Gorynski, Krzysztof; Gomez-Rios, German Augusto; Knaak, Jan Matthias; Machuca, Tiago; Spetzler, Vinzent Nikolaus; Cudjoe, Erasmus; Hsin, Michael; Cypel, Marcelo; Selzner, Markus; Liu, Mingyao; Keshavjee, Shaf; Pawliszyn, Janusz

    2013-11-25

    Metabolomics and biomarkers discovery are an integral part of bioanalysis. However, untargeted tissue analysis remains as the bottleneck of such studies due to the invasiveness of sample collection, as well as the laborious and time-consuming sample preparation protocols. In the current study, technology integrating in vivo sampling, sample preparation and global extraction of metabolites--solid phase microextraction was presented and evaluated during liver and lung transplantation in pig model. Sampling approaches, including selection of the probe, transportation, storage conditions and analyte coverage were discussed. The applicability of the method for metabolomics studies was demonstrated during lung transplantation experiments. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

    Directory of Open Access Journals (Sweden)

    Helena Prosen

    2014-05-01

    Full Text Available Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc. published in the last decade. Several innovative liquid-phase microextraction (LPME techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME, hollow fiber-liquid phase microextraction (HF-LPME, dispersive liquid-liquid microextraction (DLLME. Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

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

    NARCIS (Netherlands)

    Diez, C.; Traag, W.A.; Zommer, P.; Marinero, P.; Atienza, J.

    2006-01-01

    An acetonitrile/partitioning extraction and "dispersive solid-phase extraction (SPE)" method that provides high quality results with a minimum number of steps and a low solvent and glassware consumption was published in 2003. This method, suitable for the analysis of multiple classes of pesticide

  9. A direct immersion solid-phase microextraction gas chromatography/mass spectrometry method for the simultaneous detection of levamisole and minor cocaine congeners in hair samples from chronic abusers.

    Science.gov (United States)

    Fucci, Nadia; Gambelunghe, Cristiana; Aroni, Kyriaki; Rossi, Riccardo

    2014-12-01

    Because levamisole has been increasingly found as a component of illicit drugs, a robust method to detect its presence in hair samples is needed. However, no systematic research on the detection of levamisole in hair samples has been published. The method presented here uses direct immersion solid-phase microextraction coupled with gas chromatography and mass spectrometry (DI-SPME-GC/MS) to detect levamisole and minor cocaine congeners in hair samples using a single-extraction method. Fifty hair samples taken in the last 4 years were obtained from cocaine abusers, along with controls taken from drug-free volunteers. Sampling was performed using direct immersion with a 30-μm polydimethylsiloxane fused silica/stainless steel fiber. Calibration curves were prepared by adding known amounts of analytes and deuterated internal standards to the hair samples taken from drug-free volunteers. This study focused on the adulterant levamisole and some minor cocaine congeners (tropococaine, norcocaine, and cocaethylene). Levamisole was detected in 38% of the hair samples analyzed; its concentration ranged from 0.2 to 0.8 ng/mg. The limit of quantification and limit of detection for levamisole, tropococaine, norcocaine, and cocaine were 0.2 and 0.1 ng/mg, respectively. DI-SPME-GC/MS is a sensitive and specific method to detect the presence of levamisole and cocaine congeners in hair samples.

  10. Development and validation of a high-performance liquid chromatography method for determination of ractopamine residue in pork samples by solid phase extraction and pre-column derivatization.

    Science.gov (United States)

    Ding, Guanglong; Li, Deguang; Qin, Jiao; Zhu, Juanli; Wang, Baitao; Geng, Qianqian; Guo, Mingcheng; Punyapitak, Darunee; Cao, Yongsong

    2015-08-01

    Ractopamine (RAC) has been approved as a feed additive for swine, cattle or turkey, and is likely to have residue in edible animal products and may pose a potential risk for consumer health. Therefore, it is essential to establish a method to detect the residue of RAC in animal products. This work presents a rapid and sensitive HPLC method for the determination of RAC in pork samples with pre-column derivatization. The RAC derivative was separated on a kromasil C18 column and detected at 284nm with a UV detector. The detection capability (CCβ) was 0.078μgg(-1) and the linearity was established over the concentration range of 0.15-100.0μgg(-1). The overall mean recovery in spike range of 0.2μgg(-1) to 100μgg(-1) was 89.9% with the overall mean relative standard deviation of 4.1%. This method can be used for the quantification of RAC in pork samples and help to establish adequate monitoring of the residue of RAC. Copyright © 2015 Elsevier Ltd. All rights reserved.

  11. Direct synthesis of nitrogen-doped graphene on platinum wire as a new fiber coating method for the solid-phase microextraction of BXes in water samples: Comparison of headspace and cold-fiber headspace modes.

    Science.gov (United States)

    Memarian, Elham; Hosseiny Davarani, Saied Saeed; Nojavan, Saeed; Movahed, Siyavash Kazemi

    2016-09-07

    In this work, a new solid-phase microextraction fiber was prepared based on nitrogen-doped graphene (N-doped G). Moreover, a new strategy was proposed to solve problems dealt in direct coating of N-doped G. For this purpose, first, Graphene oxide (GO) was coated on Pt wire by electrophoretic deposition method. Then, chemical reduction of coated GO to N-doped G was accomplished by hydrazine and NH3. The prepared fiber showed good mechanical and thermal stabilities. The obtained fiber was used in two different modes (conventional headspace solid-phase microextraction and cold-fiber headspace solid-phase microextraction (CF-HS-SPME)). Both modes were optimized and applied for the extraction of benzene and xylenes from different aqueous samples. All effective parameters including extraction time, salt content, stirring rate, and desorption time were optimized. The optimized CF-HS-SPME combined with GC-FID showed good limit of detections (LODs) (0.3-2.3 μg/L), limit of quantifications (LOQs) (1.0-7.0 μg/L) and linear ranges (1.0-5000 μg/L). The developed method was applied for the analysis of benzene and xylenes in rainwater and some wastewater samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Chemical analysis of solid residue from liquid and solid fuel combustion: Method development and validation

    Energy Technology Data Exchange (ETDEWEB)

    Trkmic, M. [University of Zagreb, Faculty of Mechanical Engineering and Naval Architecturek Zagreb (Croatia); Curkovic, L. [University of Zagreb, Faculty of Chemical Engineering and Technology, Zagreb (Croatia); Asperger, D. [HEP-Proizvodnja, Thermal Power Plant Department, Zagreb (Croatia)

    2012-06-15

    This paper deals with the development and validation of methods for identifying the composition of solid residue after liquid and solid fuel combustion in thermal power plant furnaces. The methods were developed for energy dispersive X-ray fluorescence (EDXRF) spectrometer analysis. Due to the fuels used, the different composition and the location of creation of solid residue, it was necessary to develop two methods. The first method is used for identifying solid residue composition after fuel oil combustion (Method 1), while the second method is used for identifying solid residue composition after the combustion of solid fuels, i. e. coal (Method 2). Method calibration was performed on sets of 12 (Method 1) and 6 (Method 2) certified reference materials (CRM). CRMs and analysis test samples were prepared in pellet form using hydraulic press. For the purpose of method validation the linearity, accuracy, precision and specificity were determined, and the measurement uncertainty of methods for each analyte separately was assessed. The methods were applied in the analysis of real furnace residue samples. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  13. Neonatal blood gas sampling methods

    African Journals Online (AJOL)

    Blood gas sampling is part of everyday practice in the care of babies admitted to the neonatal intensive care unit, particularly for those receiving respiratory support. There is little published guidance that systematically evaluates the different methods of neonatal blood gas sampling, where each method has its individual ...

  14. Ultrasonic methods in solid state physics

    CERN Document Server

    Truell, John; Elbaum, Charles

    1969-01-01

    Ultrasonic Methods in Solid State Physics is devoted to studies of energy loss and velocity of ultrasonic waves which have a bearing on present-day problems in solid-state physics. The discussion is particularly concerned with the type of investigation that can be carried out in the megacycle range of frequencies from a few megacycles to kilomegacycles; it deals almost entirely with short-duration pulse methods rather than with standing-wave methods. The book opens with a chapter on a classical treatment of wave propagation in solids. This is followed by separate chapters on methods and techni

  15. Quantitative analysis of solid samples using modified specular reflectance accessory.

    Science.gov (United States)

    Czaja, Tomasz; Mazurek, Sylwester; Szostak, Roman

    2016-12-01

    Diffuse reflectance Fourier transform infrared spectroscopy (DRIFTS) is a fast, reliable and cost effective analytical method, requiring minimal or no sample preparation. It is commonly used in the course of qualitative and quantitative analysis of pharmaceutical ingredients and food. We demonstrate that simpler and cheaper specular reflectance (SR) accessory working in a DRIFTS like mode (SR-DL) can be an alternative for DIRFTS attachment. An application of a modified SR accessory for quantitative analysis of solids samples is presented. As a case study the concentration of cinnarizine in commercial tablets has been determined from DRIFTS and SR-DL infrared (IR) and near-infrared (NIR) spectra recorded using DTGS (deuterated triglicine sulphate) detector in the IR and NIR regions and InGaAs (indium-gallium arsenide) detector in the NIR range. Based on these spectra Partial Least Squares (PLS) models were constructed and relative standard errors of prediction (RSEP) were calculated for the calibration, validation and analysed data sets. They amounted to 2.4-2.5%, 2.1-2.7% and 2.0-2.6% for the DRIFTS attachment while 2.1-2.2%, 2.0-2.3% and 1.9-2.6%, respectively, for the modified SR accessory. Obtained error values indicate that modified SR accessory can be effectively used for quantification of solid pharmaceutical samples in the mid- and near-infrared regions. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. SWOT ANALYSIS ON SAMPLING METHOD

    National Research Council Canada - National Science Library

    CHIS ANCA OANA; BELENESI MARIOARA;

    2014-01-01

    .... Our article aims to study audit sampling in audit of financial statements. As an audit technique largely used, in both its statistical and nonstatistical form, the method is very important for auditors...

  17. Development and optimization of a novel sample preparation method cored on functionalized nanofibers mat-solid-phase extraction for the simultaneous efficient extraction of illegal anionic and cationic dyes in foods.

    Science.gov (United States)

    Qi, Feifei; Jian, Ningge; Qian, Liangliang; Cao, Weixin; Xu, Qian; Li, Jian

    2017-09-01

    A simple and efficient three-step sample preparation method was developed and optimized for the simultaneous analysis of illegal anionic and cationic dyes (acid orange 7, metanil yellow, auramine-O, and chrysoidine) in food samples. A novel solid-phase extraction (SPE) procedure based on nanofibers mat (NFsM) was proposed after solvent extraction and freeze-salting out purification. The preferred SPE sorbent was selected from five functionalized NFsMs by orthogonal experimental design, and the optimization of SPE parameters was achieved through response surface methodology (RSM) based on the Box-Behnken design (BBD). Under the optimal conditions, the target analytes could be completely adsorbed by polypyrrole-functionalized polyacrylonitrile NFsM (PPy/PAN NFsM), and the eluent was directly analyzed by high-performance liquid chromatography-diode array detection (HPLC-DAD). The limits of detection (LODs) were between 0.002 and 0.01 mg kg-1, and satisfactory linearity with correlation coefficients (R > 0.99) for each dye in all samples was achieved. Compared with the Chinese standard method and the published methods, the proposed method was simplified greatly with much lower requirement of sorbent (5.0 mg) and organic solvent (2.8 mL) and higher sample preparation speed (10 min/sample), while higher recovery (83.6-116.5%) and precision (RSDs method, we have successfully detected illegal ionic dyes in three common representative foods: yellow croaker, soybean products, and chili seasonings. Graphical abstract Schematic representation of the process of the three-step sample preparation.

  18. Meshless Methods in Solid Mechanics

    CERN Document Server

    Chen, Youping; Eskandarian, Azim

    2006-01-01

    Finite element method has been the dominant technique in computational mechanics in the past decades, and it has made significant contributions to the developments in engineering and science. Nevertheless, finite element method is not well suited to problems having severe mesh distortion owing to extremely large deformations of materials, encountering moving discontinuities such as crack propagation along arbitrary and complex paths, involving considerable meshing and re-meshing in structural optimization problems, or having multidomain of influence in multi-phenomenon physical problems. It is impossible to completely overcome those mesh-related difficulties by a mesh-based method. The highly structured nature of finite element approximations imposes severe penalties in the solutions of those problems. Distinguishing with finite element, finite difference and finite volume methods, meshless method discretizes the continuum body only with a set of nodal points and the approximation is constructed entirely in t...

  19. SWOT ANALYSIS ON SAMPLING METHOD

    Directory of Open Access Journals (Sweden)

    CHIS ANCA OANA

    2014-07-01

    Full Text Available Audit sampling involves the application of audit procedures to less than 100% of items within an account balance or class of transactions. Our article aims to study audit sampling in audit of financial statements. As an audit technique largely used, in both its statistical and nonstatistical form, the method is very important for auditors. It should be applied correctly for a fair view of financial statements, to satisfy the needs of all financial users. In order to be applied correctly the method must be understood by all its users and mainly by auditors. Otherwise the risk of not applying it correctly would cause loose of reputation and discredit, litigations and even prison. Since there is not a unitary practice and methodology for applying the technique, the risk of incorrectly applying it is pretty high. The SWOT analysis is a technique used that shows the advantages, disadvantages, threats and opportunities. We applied SWOT analysis in studying the sampling method, from the perspective of three players: the audit company, the audited entity and users of financial statements. The study shows that by applying the sampling method the audit company and the audited entity both save time, effort and money. The disadvantages of the method are difficulty in applying and understanding its insight. Being largely used as an audit method and being a factor of a correct audit opinion, the sampling method’s advantages, disadvantages, threats and opportunities must be understood by auditors.

  20. Distance sampling methods and applications

    CERN Document Server

    Buckland, S T; Marques, T A; Oedekoven, C S

    2015-01-01

    In this book, the authors cover the basic methods and advances within distance sampling that are most valuable to practitioners and in ecology more broadly. This is the fourth book dedicated to distance sampling. In the decade since the last book published, there have been a number of new developments. The intervening years have also shown which advances are of most use. This self-contained book covers topics from the previous publications, while also including recent developments in method, software and application. Distance sampling refers to a suite of methods, including line and point transect sampling, in which animal density or abundance is estimated from a sample of distances to detected individuals. The book illustrates these methods through case studies; data sets and computer code are supplied to readers through the book’s accompanying website.  Some of the case studies use the software Distance, while others use R code. The book is in three parts.  The first part addresses basic methods, the ...

  1. Solid Phase Characterization of Tank 241-C-105 Grab Samples

    Energy Technology Data Exchange (ETDEWEB)

    Ely, T. M. [Washington River Protection Solutions LLC, Richland, WA (United States); LaMothe, M. E. [Washington River Protection Solutions LLC, Richland, WA (United States); Lachut, J. S. [Washington River Protection Solutions LLC, Richland, WA (United States)

    2016-01-11

    The solid phase characterization (SPC) of three grab samples from single-shell Tank 241-C-105 (C-105) that were received at the laboratory the week of October 26, 2015, has been completed. The three samples were received and broken down in the 11A hot cells.

  2. Solid-phase microextraction for the analysis of biological samples

    NARCIS (Netherlands)

    Theodoridis, G; Koster, EHM; de Jong, GJ

    2000-01-01

    Solid-phase microextraction (SPME) has been introduced for the extraction of organic compounds from environmental samples. This relatively new extraction technique has now also gained a lot of interest in a broad field of analysis including food, biological and pharmaceutical samples. SPME has a

  3. An innovative method for analysis of Pb (II) in rice, milk and water samples based on TiO2 reinforced caprylic acid hollow fiber solid/liquid phase microextraction.

    Science.gov (United States)

    Bahar, Shahriyar; Es'haghi, Zarrin; Nezhadali, Azizollah; Banaei, Alireza; Bohlooli, Shahab

    2017-04-15

    In the present study, nano-sized titanium oxides were applied for preconcentration and determination of Pb(II) in aqueous samples using hollow fiber based solid-liquid phase microextraction (HF-SLPME) combined with flame atomic absorption spectrometry (FAAS). In this work, the nanoparticles dispersed in caprylic acid as an extraction solvent was placed into a polypropylene porous hollow fiber segment supported by capillary forces and sonification. This membrane was in direct contact with solutions containing Pb (II). The effect of experimental conditions on the extraction, such as pH, stirring rate, sample volume, and extraction time were optimized. Under the optimal conditions, the performance of the proposed method was investigated for the determination of Pb (II) in food and water samples. The method was linear in the range of 0.6-3000μgmL(-1). The relative standard deviations and relative recovery of Pb (II) was 4.9% and 99.3%, respectively (n=5). Copyright © 2016 Elsevier Ltd. All rights reserved.

  4. Lowering detection limits for 1,2,3-trichloropropane in water using solid phase extraction coupled to purge and trap sample introduction in an isotope dilution GC-MS method.

    Science.gov (United States)

    Liao, Wenta; Ghabour, Miriam; Draper, William M; Chandrasena, Esala

    2016-09-01

    Purge and trap sample introduction (PTI) has been the premier sampling and preconcentration technique for gas chromatographic determination of volatile organic compounds (VOCs) in drinking water for almost 50 years. PTI affords sub parts-per-billion (ppb) detection limits for purgeable VOCs including fixed gases and higher boiling hydrocarbons and halocarbons. In this study the coupling of solid phase extraction (SPE) to PTI was investigated as a means to substantially increase enrichment and lower detection limits for the emerging contaminant, 1,2,3-trichloropropane (TCP). Water samples (500 mL) were dechlorinated, preserved with a biocide, and spiked with the isotope labeled internal standard, d5-TCP. The entire 500 mL sample was extracted with activated carbon or carbon molecular sieve SPE cartridges, and then eluted with dichloromethane -- excess solvent was removed in a nitrogen evaporator and diethylene glycol "keeper" remaining was dispersed in 5 mL of water for PTI GC-MS analysis. The experimental Method Detection Limit (MDL) for TCP was 0.11 ng/L (ppt) and accuracy was 95-103% in sub-ppt determinations. Groundwater samples including impaired California sources and treated water (n = 21) were analyzed with results ranging from below the method reporting limit (0.30 ng/L) to > 250 ng/L. Coupling of SPE with PTI may provide similar reductions in detection limits for other VOCs with appropriate physical-chemical properties. Copyright © 2016 Elsevier Ltd. All rights reserved.

  5. Development of headspace solid-phase microextraction method for ...

    African Journals Online (AJOL)

    A headspace solid-phase microextraction (HS-SPME) method was developed as a preliminary investigation using univariate approach for the analysis of 14 multiclass pesticide residues in fruits and vegetable samples. The gas chromatography mass spectrometry parameters (desorption temperature and time, column flow ...

  6. Method for silicon nitride precursor solids recovery

    Science.gov (United States)

    Crosbie, Gary M.; Predmesky, Ronald L.; Nicholson, John M.

    1992-12-15

    Method and apparatus are provided for collecting reaction product solids entrained in a gaseous outflow from a reaction situs, wherein the gaseous outflow includes a condensable vapor. A condensate is formed of the condensable vapor on static mixer surfaces within a static mixer heat exchanger. The entrained reaction product solids are captured in the condensate which can be collected for further processing, such as return to the reaction situs. In production of silicon imide, optionally integrated into a production process for making silicon nitride caramic, wherein reactant feed gas comprising silicon halide and substantially inert carrier gas is reacted with liquid ammonia in a reaction vessel, silicon imide reaction product solids entrained in a gaseous outflow comprising residual carrier gas and vaporized ammonia can be captured by forming a condensate of the ammonia vapor on static mixer surfaces of a static mixer heat exchanger.

  7. Validation of an off line solid phase extraction liquid chromatography-tandem mass spectrometry method for the determination of systemic insecticide residues in honey and pollen samples collected in apiaries from NW Spain.

    Science.gov (United States)

    García-Chao, María; Agruña, María Jesús; Flores Calvete, Gonzalo; Sakkas, Vasilis; Llompart, María; Dagnac, Thierry

    2010-07-05

    The use of pesticides to protect crops against plagues and insects is one of the most important ways to assure agricultural quality and productivity. However, bad application practices may cause the contamination of different environmental compartments and animal species, as a consequence of migration or accumulation of those compounds. Fipronil, imidacloprid and thiametoxam are systemic or systemic-like insecticides widely used in maize crops. Their heavy action in the nervous system of target insects also means a high toxicity to non-target pollinator insects such as honey bees which can get in touch with them through pollen and nectar during foraging activities. These insecticides have even been suspected to cause a significant decrease of honeybee colonies that has been observed in many countries since the past decade. Since September 1st 2008, the European Commission set new MRLs in food and feed of plant and animal origin. The pesticides included in this study have MRLs in honey and pollen between 10 and 50 ng g(-1). In the present work, an analytical method was developed with the aim of determining residues of fipronil and some of its metabolites (fipronil sulfone, fipronil sulfide, fipronil desulfinyl and fipronil carboxamide), thiamethoxam and imidacloprid in honey and pollen samples. The extraction optimization was performed using a Doehlert experimental design by studying two factors, the mixture and the ratio of solvents used. Prior to the extraction procedure, raw hive samples containing honey, pollen and wax were centrifuged at 4000 rpm. The upper solid material was removed, and 1 g of the lower phase was mixed with 3 mL of the optimized mixture of methanol/water (10/90). The extract was passed through a florisil cartridge and the target compounds were eluted with methanol and analysed by LC-MS/MS in selective reaction monitoring (SRM) mode. The method was validated according to the guidelines included in the SANCO/10684/2009 document and the ISO

  8. A new way of solid dosage form samples preparation for SEM and FTIR using microtome.

    Science.gov (United States)

    Šimek, Michal; Grünwaldová, Veronika; Kratochvíl, Bohumil

    2014-06-01

    Rapid and correct production of generic solid dosage forms requires a large amount of analytical data and conclusions. Modern analytical techniques have a good resolution and accuracy and allow obtaining a lot of information about the original product. Scanning electron microscopy (SEM) is used for observation and assessing individual layers, core and surface of solid dosage forms. Fourier transform infrared (FTIR) spectroscopy mapping allows determining the distribution and characterization of individual components in a solid dosage form. However, the samples prepared by common way, using scalpel or tablet splitter, are not good enough. It was the reason for development of a new and better method of sample preparation, which uses microtome. Well-prepared samples analyzed by SEM and FTIR mapping allow to determine a solid dosage form formulation, excipient content and distribution of excipient and active pharmaceutical ingredient.

  9. Cr(VI) generation during sample preparation of solid samples – A ...

    African Journals Online (AJOL)

    Cr(VI) generation during sample preparation of solid samples – A chromite ore case study. R.I Glastonbury, W van der Merwe, J.P Beukes, P.G van Zyl, G Lachmann, C.J.H Steenkamp, N.F Dawson, M.H Stewart ...

  10. Towards Cost-efficient Sampling Methods

    CERN Document Server

    Peng, Luo; Chong, Wu

    2014-01-01

    The sampling method has been paid much attention in the field of complex network in general and statistical physics in particular. This paper presents two new sampling methods based on the perspective that a small part of vertices with high node degree can possess the most structure information of a network. The two proposed sampling methods are efficient in sampling the nodes with high degree. The first new sampling method is improved on the basis of the stratified random sampling method and selects the high degree nodes with higher probability by classifying the nodes according to their degree distribution. The second sampling method improves the existing snowball sampling method so that it enables to sample the targeted nodes selectively in every sampling step. Besides, the two proposed sampling methods not only sample the nodes but also pick the edges directly connected to these nodes. In order to demonstrate the two methods' availability and accuracy, we compare them with the existing sampling methods in...

  11. Sample processing device and method

    DEFF Research Database (Denmark)

    2011-01-01

    A sample processing device is disclosed, which sample processing device comprises a first substrate and a second substrate, where the first substrate has a first surface comprising two area types, a first area type with a first contact angle with water and a second area type with a second contact...... a sample liquid comprising the sample and the first preparation system is adapted to receive a receiving liquid. In a particular embodiment, a magnetic sample transport component, such as a permanent magnet or an electromagnet, is arranged to move magnetic beads in between the first and second substrates....

  12. Systems and methods for monitoring a solid-liquid interface

    Science.gov (United States)

    Stoddard, Nathan G; Lewis, Monte A.; Clark, Roger F

    2013-06-11

    Systems and methods are provided for monitoring a solid-liquid interface during a casting process. The systems and methods enable determination of the location of a solid-liquid interface during the casting process.

  13. Polychlorinated biphenyls (PCB) analysis report for solid sample from 219S tank 104

    Energy Technology Data Exchange (ETDEWEB)

    Ross, G.A.

    1998-03-27

    A sample of solids was obtained from tank 104 of 219S via a peristaltic pump equipped with a stainless steel tube and Norprenel tubing (Phthalate free). The sample obtained in a glass jar with Teflon 2 lid, was analyzed for PCBs as Aroclor mixtures. A soxhlet extraction procedure was used to extract the Aroclors from the sample. Analysis was performed using dual column confirmation gas chromatography/electron capture detection (GC/ECD). The extraction method closely follows SW-846 method 3540C and the analysis follows SW-846 method.

  14. Methods and machinery for pulverising solid wastes

    CSIR Research Space (South Africa)

    Simpkins, MJ

    1976-11-01

    Full Text Available This report is published on behalf of the South African Committee for Solid Wastes which in turn advises the National Committee for Environmental Sciences on problems concerned with Solid Wastes in South Africa. It is particularly concerned...

  15. A method of language sampling

    DEFF Research Database (Denmark)

    Rijkhoff, Jan; Bakker, Dik; Hengeveld, Kees

    1993-01-01

    created with this method will reflect optimally the diversity of the languages of the world. On the basis of the internal structure of each genetic language tree a measure is computed that reflects the linguistic diversity in the language families represented by these trees. This measure is used...

  16. Asymptotic methods in mechanics of solids

    CERN Document Server

    Bauer, Svetlana M; Smirnov, Andrei L; Tovstik, Petr E; Vaillancourt, Rémi

    2015-01-01

    The construction of solutions of singularly perturbed systems of equations and boundary value problems that are characteristic for the mechanics of thin-walled structures are the main focus of the book. The theoretical results are supplemented by the analysis of problems and exercises. Some of the topics are rarely discussed in the textbooks, for example, the Newton polyhedron, which is a generalization of the Newton polygon for equations with two or more parameters. After introducing the important concept of the index of variation for functions special attention is devoted to eigenvalue problems containing a small parameter. The main part of the book deals with methods of asymptotic solutions of linear singularly perturbed boundary and boundary value problems without or with turning points, respectively. As examples, one-dimensional equilibrium, dynamics and stability problems for rigid bodies and solids are presented in detail. Numerous exercises and examples as well as vast references to the relevant Russi...

  17. Alpha-spectrometric analysis of uranium and thorium using solid-phase extraction for sample preparation

    Energy Technology Data Exchange (ETDEWEB)

    Weber, R.; Esterlund, R.A.; Patzelt, P

    1999-05-01

    A method is presented here for the preparation of thin uniform samples of naturally occurring uranium and thorium which are highly suitable for {alpha}-spectrometric analysis. The solid-phase extraction procedure simultaneously achieves a complete separation of the analytes from the sample matrix and a high enrichment factor for uranium and thorium, so that the ensuing eluate is ideally suited for either electrodeposition or ICP-MS, without the need for complicated and painstaking sample preparation. In contrast to conventional liquid-liquid phase-extraction methods, no organic waste solutions are produced, and the process can be easily automated.

  18. Can matrix solid phase dispersion (MSPD) be more simplified? Application of solventless MSPD sample preparation method for GC-MS and GC-FID analysis of plant essential oil components.

    Science.gov (United States)

    Wianowska, Dorota; Dawidowicz, Andrzej L

    2016-05-01

    This paper proposes and shows the analytical capabilities of a new variant of matrix solid phase dispersion (MSPD) with the solventless blending step in the chromatographic analysis of plant volatiles. The obtained results prove that the use of a solvent is redundant as the sorption ability of the octadecyl brush is sufficient for quantitative retention of volatiles from 9 plants differing in their essential oil composition. The extraction efficiency of the proposed simplified MSPD method is equivalent to the efficiency of the commonly applied variant of MSPD with the organic dispersing liquid and pressurized liquid extraction, which is a much more complex, technically advanced and highly efficient technique of plant extraction. The equivalency of these methods is confirmed by the variance analysis. The proposed solventless MSPD method is precise, accurate, and reproducible. The recovery of essential oil components estimated by the MSPD method exceeds 98%, which is satisfactory for analytical purposes. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Sampling Polymorphs of Ionic Solids using Random Superlattices.

    Science.gov (United States)

    Stevanović, Vladan

    2016-02-19

    Polymorphism offers rich and virtually unexplored space for discovering novel functional materials. To harness this potential approaches capable of both exploring the space of polymorphs and assessing their realizability are needed. One such approach devised for partially ionic solids is presented. The structure prediction part is carried out by performing local density functional theory relaxations on a large set of random supperlattices (RSLs) with atoms distributed randomly over different planes in a way that favors cation-anion coordination. Applying the RSL sampling on MgO, ZnO, and SnO_{2} reveals that the resulting probability of occurrence of a given structure offers a measure of its realizability explaining fully the experimentally observed, metastable polymorphs in these three systems.

  20. Gastric emptying of solids: When should we sample

    Energy Technology Data Exchange (ETDEWEB)

    Sfakianakis, G.; Spoliansky, G.; Cassady, J.; Barkin, J.; Serafini, A.

    1984-01-01

    Gastric emptying of solids has been studied for 20 normal volunteers using Tc-99m-sulfur-colloid labeled chicken liver or eggs. Residual gastric activity measured in 15 min intervals for 2 1/2 hrs was used to calculate gastric emptying. The procedure was proposed and is used to examine patients for suspected abnormal emptying. This approach however ties up one gamma camera and one technologist for a period of 2 1/2 - 3 hrs. Furthermore to classify any value more the 1SD below the mean as abnormal includes 16% of normals as abnormally low (false positives). In order to find the pattern of abnormalities and the best time to study patients we analyzed the results of 54 studies performed in patients with a variety of clinical problems. Gastric emptying was measured in 30 min intervals for 2 1/2 hrs after a standard meal of 2 scrambled eggs labeled with 1 mCi of Tc-99m-sulfur-colloid, 2 slices of bread and 300 ml of juice. To choose the point important to observe the authors studied the distribution of values at each time-point to determine when there is the greatest variability from the reported normal. When there is delayed emptying the 2 1/2 hr observation is the best discriminator and when there is accelerated emptying the 60 min observation is the best discriminator. In the group of patients the 150 min observation had no correlation with the age of the patients. It is possible that sampling at a later time could be more discriminatory. The authors propose sampling at 0, 60, and 150 min time as the most informative and cost effective approach to study the solid gastric emptying. The 2SD rather than 1SD below and above the mean should be used as the level to separate normal from abnormal results.

  1. Headspace solid-phase microextraction gas chromatography tandem mass spectrometry for the determination of brominated flame retardants in environmental solid samples.

    Science.gov (United States)

    Salgado-Petinal, Carmen; Garcia-Chao, Maria; Llompart, Maria; Garcia-Jares, Carmen; Cela, Rafael

    2006-06-01

    A headspace solid-phase microextraction gas chromatography coupled with tandem mass spectrometry (HSSPME-GC-MS-MS) methodology for determination of brominated flame retardants in sediment and soil samples is presented. To the best of our knowledge, this is the first time that SPME has been applied to analyze polybrominated biphenyls (PBBs) and polybrominated diphenyl ethers (PBDEs) in environmental solid samples. Analyses were performed using 0.5-g solid samples moisturized with 2 mL water, employing a polydimethylsiloxane (PDMS) fiber coating, exposed to the headspace at 100 degrees C for 60 min. Several types of environmental solid samples were included in this study and the extraction efficiency was related to the organic matter content of the sample. Calibration was performed using real samples, and the method showed good linearity over a wide concentration range, precision, and afforded quantitative recoveries. The obtained detection limits were in the sub-ng g(-1) for all the target analytes in both samples. The proposed procedure was applied to several marine and river sediments and soils, some of which were found to contain PBDEs at concentrations in the ng g(-1) level; BDE-47, BDE-100, and BDE-99 were the major congeners detected. The proposed method constitutes a rapid and low-cost alternative for the analysis of the target brominated flame retardants in environmental solid samples, since the clean-up steps, fractionation, and preconcentration of extracts inherent to the classical multi-step solvent extraction procedures are avoided.

  2. Criteria for the safe avoidance of needle sampling in young women with solid breast masses

    Energy Technology Data Exchange (ETDEWEB)

    Maxwell, A.J., E-mail: anthony.maxwell@rbh.nhs.u [Bolton Breast Unit, Royal Bolton Hospital, Bolton BL4 0JR (United Kingdom); Pearson, J.M. [Bolton Breast Unit, Royal Bolton Hospital, Bolton BL4 0JR (United Kingdom)

    2010-03-15

    Aim: To establish clinical and ultrasonic criteria by which needle sampling can be safely avoided in young women with solid breast masses. Materials and methods: The databases of a large hospital were searched for breast cancers, phyllodes tumours, and papillomas diagnosed in women below the age of 30 years. In addition, the clinical and sonographic findings in female patients less than 25 years of age presenting with a solid breast mass over a 1-year period were reviewed. Results: Nine women with breast cancer, seven with phyllodes, and six with papillomas were found. No delayed diagnoses in those who had ultrasound would have been made if the following criteria had been applied to avoid needle sampling: age less than 25 years; no known risk factors for breast malignancy; mass not rapidly enlarging; smooth discrete mobile mass on clinical examination, or lesion impalpable; well-defined homogeneously isoechoic or mildly hypoechoic solid mass; less than 3 cm in greatest dimension; ovoid shape, aligned parallel to the skin surface; smooth or gently lobulated contour (two or three lobulations only; no microlobulation); thin echogenic pseudocapsule; no calcification; no acoustic shadowing. Needle sampling could have been safely avoided in approximately two-thirds of the women reviewed below the age of 25 with a solid breast mass. Conclusion: Application of the proposed criteria would spare a significant number of young women unnecessary needle sampling.

  3. New prior sampling methods for nested sampling - Development and testing

    Science.gov (United States)

    Stokes, Barrie; Tuyl, Frank; Hudson, Irene

    2017-06-01

    Nested Sampling is a powerful algorithm for fitting models to data in the Bayesian setting, introduced by Skilling [1]. The nested sampling algorithm proceeds by carrying out a series of compressive steps, involving successively nested iso-likelihood boundaries, starting with the full prior distribution of the problem parameters. The "central problem" of nested sampling is to draw at each step a sample from the prior distribution whose likelihood is greater than the current likelihood threshold, i.e., a sample falling inside the current likelihood-restricted region. For both flat and informative priors this ultimately requires uniform sampling restricted to the likelihood-restricted region. We present two new methods of carrying out this sampling step, and illustrate their use with the lighthouse problem [2], a bivariate likelihood used by Gregory [3] and a trivariate Gaussian mixture likelihood. All the algorithm development and testing reported here has been done with Mathematica® [4].

  4. Ignitable solids having an arrayed structure and methods thereof

    Energy Technology Data Exchange (ETDEWEB)

    Adams, David P.; Reeves, Robert V.; Grubbs, Robert K.; Henry, Michael David

    2017-08-08

    The present invention relates to the design and manufacture of an ignitable solid, where the solid is composed of an array of ignitable regions. In some examples, the array provides a three-dimensional periodic arrangement of such ignitable regions. The ignitable region can have any useful geometry and geometric arrangement within the solid, and methods of making such regions are also described herein.

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

    Science.gov (United States)

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

    2015-05-11

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

  6. Solid lithium ion conducting electrolytes and methods of preparation

    Science.gov (United States)

    Narula, Chaitanya K; Daniel, Claus

    2013-05-28

    A composition comprised of nanoparticles of lithium ion conducting solid oxide material, wherein the solid oxide material is comprised of lithium ions, and at least one type of metal ion selected from pentavalent metal ions and trivalent lanthanide metal ions. Solution methods useful for synthesizing these solid oxide materials, as well as precursor solutions and components thereof, are also described. The solid oxide materials are incorporated as electrolytes into lithium ion batteries.

  7. Solid oxide cell stack and method for preparing same

    DEFF Research Database (Denmark)

    2012-01-01

    A method for producing and reactivating a solid oxide cell stack structure by providing a catalyst precursor in at least one of the electrode layers by impregnation and subsequent drying after the stack has been assembled and initiated. Due to a significantly improved performance and an unexpecte...... voltage improvement this solid oxide cell stack structure is particularly suitable for use in solid oxide fuel cell (SOFC) and solid oxide electrolysing cell (SOEC) applications....

  8. Solid sampling determination of magnesium in lithium niobate crystals by graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Dravecz, Gabriella; Laczai, Nikoletta; Hajdara, Ivett; Bencs, László

    2016-12-01

    The vaporization/atomization processes of Mg in high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS) were investigated by evaporating solid (powder) samples of lithium niobate (LiNbO3) optical single crystals doped with various amounts of Mg in a transversally heated graphite atomizer (THGA). Optimal analytical conditions were attained by using the Mg I 215.4353 nm secondary spectral line. An optimal pyrolysis temperature of 1500 °C was found for Mg, while the compromise atomization temperature in THGAs (2400 °C) was applied for analyte vaporization. The calibration was performed against solid (powered) lithium niobate crystal standards. The standards were prepared with exactly known Mg content via solid state fusion of the oxide components of the matrix and analyte. The correlation coefficient (R value) of the linear calibration was not worse than 0.9992. The calibration curves were linear in the dopant concentration range of interest (0.74-7.25 mg/g Mg), when dosing 3-10 mg of the powder samples into the graphite sample insertion boats. The Mg content of the studied 19 samples was in the range of 1.69-4.13 mg/g. The precision of the method was better than 6.3%. The accuracy of the results was verified by means of flame atomic absorption spectrometry with solution sample introduction after digestion of several crystal samples.

  9. Procedures for sampling and sample reduction within quality assurance systems for solid biofuels

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2005-07-01

    The objective of this experimental study on sampling was to determine the size and number of samples of biofuels required (taken at two sampling points in each case) and to compare two methods of sampling. The first objective of the sample-reduction exercise was to compare the reliability of various sampling methods, and the second objective was to measure the variations introduced as a result of reducing the sample size to form suitable test portions. The materials studied were sawdust, wood chips, wood pellets and bales of straw, and these were analysed for moisture, ash, particle size and chloride. The sampling procedures are described. The study was conducted in Scandinavia. The results of the study were presented in Leipzig in October 2004. The work was carried out as part of the UK's DTI Technology Programme: New and Renewable Energy.

  10. Liquid-solid sample preparation followed by headspace solid-phase microextraction determination of multiclass pesticides in soil.

    Science.gov (United States)

    Durović, Rada D; Dordević, Tijana M; Santrić, Ljiljana R

    2012-01-01

    This paper describes development and validation of a multiresidue method for the determination of five pesticides (terbufos, prochloraz, chloridazon, pendimethalin, and fluorochloridone) belonging to different pesticide groups in soil samples by GC/MS, followed by its application in the analysis of some agricultural soil samples. The method is based on a headspace solid-phase microextraction method. Microextraction conditions, namely temperature, extraction time, and NaCI content, were tested and optimized using a 100 microm polydimethylsiloxane fiber. Three extraction solvents [methanol, methanol-acetone (1 + 1, v/v), and methanol-acetone-hexane (2 + 2 + 1, v/v/v)] and the optimum number of extraction steps within the sample preparation stage were optimized for the extraction procedure. LOD values for all the studied compounds were less than 12 microg/kg. Recovery values for multiple analyses of soil samples fortified at 30 microg/kg of each pesticide were higher than 64%. The method was proven to be repeatable, with RSD lower than 15%.

  11. Determination of Chemical Warfare Agents in Water Samples by Solid Phase Microextraction and GC-FID

    OpenAIRE

    Hussain, Fatima

    2007-01-01

    The Norwegian Defence Research Establishment (FFI) is presently developing a mobile laboratory for the identification of chemical warfare agents (CWA) and related compounds. The laboratory will be used in the field, and it is therefore advantageous that the analytical methods give a high priority to low solvent consumption and minimal need for sample preparation. Solid phase microextraction (SPME) meets these requirements, since the technique is based on automatic extraction and concentration...

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

    Science.gov (United States)

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

    2017-12-26

    This work presents a new extraction material, namely, Q-100, based on hypercrosslinked magnetic particles, which was tested in dispersive solid-phase extraction for a group of sweeteners from environmental samples. The hypercrosslinked Q-100 magnetic particles had the advantage of suitable pore size distribution and high surface area, and showed good retention behavior towards sweeteners. Different dispersive solid-phase extraction parameters such as amount of magnetic particles or extraction time were optimized. Under optimum conditions, Q-100 showed suitable apparent recovery, ranging in the case of river water sample from 21 to 88% for all the sweeteners, except for alitame (12%). The validated method based on dispersive solid-phase extraction using Q-100 followed by liquid chromatography with tandem mass spectrometry provided good linearity and limits of quantification between 0.01 and 0.1 μg L -1 . The method was applied to analyze samples from river water and effluent wastewater, and four sweeteners (acesulfame, saccharin, cyclamate and sucralose) were found in both types of sample. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  13. Sampling and analysis methods for geothermal fluids and gases

    Energy Technology Data Exchange (ETDEWEB)

    Watson, J.C.

    1978-07-01

    The sampling procedures for geothermal fluids and gases include: sampling hot springs, fumaroles, etc.; sampling condensed brine and entrained gases; sampling steam-lines; low pressure separator systems; high pressure separator systems; two-phase sampling; downhole samplers; and miscellaneous methods. The recommended analytical methods compiled here cover physical properties, dissolved solids, and dissolved and entrained gases. The sequences of methods listed for each parameter are: wet chemical, gravimetric, colorimetric, electrode, atomic absorption, flame emission, x-ray fluorescence, inductively coupled plasma-atomic emission spectroscopy, ion exchange chromatography, spark source mass spectrometry, neutron activation analysis, and emission spectrometry. Material on correction of brine component concentrations for steam loss during flashing is presented. (MHR)

  14. Direct solid sampling by flame atomic absorption spectrometry: determination of manganese in coal samples

    Directory of Open Access Journals (Sweden)

    Flores Érico M. M.

    2004-01-01

    Full Text Available A new device for the direct solid analysis by flame atomic absorption spectrometry was investigated as an alternative technique for the determination of trace elements in coal. The potential application of the proposed procedure for the determination of manganese was investigated. Ground coal test samples were weighed directly into polyethylene vials and carried as a dry aerosol to a slotted quartz vaporization cell placed between the flame burner and optical path. The transient signals obtained were totally integrated in 1 second. The effect of operating conditions on the analytical signal was investigated. Background signals were always low and a Mn characteristic mass of 1.9 ng was found. Results were considered satisfactory regarding to both accuracy (between 97.5 and 103.2% and precision (RSD better than 6%. The proposed system is simple and can be easily adapted to any conventional atomic absorption spectrometers allowing the analysis of more than 80 test samples in an hour.

  15. Solid waste sampling and distribution project: Sampling report {number_sign}5

    Energy Technology Data Exchange (ETDEWEB)

    1993-10-01

    The US DOE has established a key goal of the Waste Management Program (WMP) to be to ensure that waste management issues do not become obstacles to the commercialization of advanced coal utilization technologies. To achieve this goal, the WMP identifies various emerging coal utilization technologies and performs comprehensive characterizations of the waste streams and products. DOE is now extending their characterization program to include a number of new facilities, particularly larger pilot- and commercial-scale units. Several advanced coal utilization technologies have been tentatively selected for comprehensive waste characterization. One of these technologies is the LOW NO{sub x} process being demonstrated by Southern Company Services, Inc. at Site F. On July 29, 1993 samples were collected to characterize solid waste streams. This document provides background information on the site and describes the sampling activities performed at this facility.

  16. Developments of solid materials for UF6 sampling

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Nicholas [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Hebden, Andrew [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Savina, Joseph [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division

    2017-11-15

    This project demonstrated that a device using majority Commercial Off the Shelf (COTS) components could be used to collect uranium hexafluoride samples safely from gaseous or solid sources. The device was based on the successful Cristallini method developed by ABACC over the past 10 years. The system was designed to capture and store the UF6 as an inert fluoride salt to ease transportation regulations. In addition, the method was considerably faster than traditional cryogenic methods, collected enough material to perform analyses without undue waste, and could be used either inside a facility or in the storage yard.

  17. Solid state lighting devices and methods with rotary cooling structures

    Science.gov (United States)

    Koplow, Jeffrey P.

    2017-03-21

    Solid state lighting devices and methods for heat dissipation with rotary cooling structures are described. An example solid state lighting device includes a solid state light source, a rotating heat transfer structure in thermal contact with the solid state light source, and a mounting assembly having a stationary portion. The mounting assembly may be rotatably coupled to the heat transfer structure such that at least a portion of the mounting assembly remains stationary while the heat transfer structure is rotating. Examples of methods for dissipating heat from electrical devices, such as solid state lighting sources are also described. Heat dissipation methods may include providing electrical power to a solid state light source mounted to and in thermal contact with a heat transfer structure, and rotating the heat transfer structure through a surrounding medium.

  18. Simultaneous ultrasound-assisted emulsification-extraction of polar and nonpolar compounds from solid plant samples.

    Science.gov (United States)

    Pérez-Serradilla, J A; Priego-Capote, F; Luque de Castro, M D

    2007-09-01

    A new approach to solid sample preparation for the simultaneous isolation of polar and nonpolar compounds using a microemulsion as leaching medium is proposed. Methanol/water (dispersed-phase)-hexane (continuous-phase) emulsions formed in the presence of ultrasound and a solid sample allow polar and nonpolar compounds to be transferred to the dispersed and continuous phase, respectively. The efficiency of this dual sample preparation approach was assessed in the characterization of natural products of variable hardness including acorns, grape seeds, and alperujo (a residue of olive oil production). The time needed for quantitative extraction of the target fractions (phenol compounds and fatty acids) is 9 min for acorns and alperujo and 20 min for grape seeds; the longer time needed for grape seeds can be attributed to higher matrix hardness. Such good performance can be ascribed to the ultrasound-enhanced formation of methanol/water microdroplets 1-15 microm in size, which act as solid-liquid microextractors spanning a large surface area. The presence of the sample was found to greatly improve emulsion stability, which can be ascribed to the amphiphilic nature of the fatty acids in the samples. Following leaching and separation of the two phases by centrifugation, the polar and nonpolar fractions were analyzed by HPLC-diode array detection and GC/MS, respectively. The proposed approach provides extraction efficiency similar to the Folch method (reference method for fat extraction, 4.5 h) in a shorter time and extraction efficiency equal to or higher than the stirring-based method (reference method for phenol compounds extraction, 24 h).

  19. Assessment of homogeneity and minimum sample mass for cadmium analysis in powdered certified reference materials and real rice samples by solid sampling electrothermal vaporization atomic fluorescence spectrometry.

    Science.gov (United States)

    Mao, Xuefei; Liu, Jixin; Huang, Yatao; Feng, Li; Zhang, Lihua; Tang, Xiaoyan; Zhou, Jian; Qian, Yongzhong; Wang, Min

    2013-01-30

    To optimize analytical quality controls of solid sampling electrothermal vaporization atomic fluorescence spectrometry (SS-ETV-AFS), the homogeneity (H(E)) of rice samples and their minimum sample mass (M) for cadmium analysis were evaluated using three certified reference materials (CRMs) and real rice samples. The effects of different grinding degrees (particle sizes 1 mm) on H(E) and M of real rice samples were also investigated. The calculated M values of three CRMs by the Pauwels equation were 2.19, 19.76, and 3.79 mg. The well-ground real rice samples (particle size method were compared with the results by microwave digestion graphite furnace atomic absorption spectrometry with a 0.5 g sample mass. There was no significant difference between these two methods, which meant that SS-ETV-AFS could be used to accurately detect Cd in rice with several milligrams of samples instead of the certified value (200 mg) or the recommended mass (200-500 mg) of the methods of the Association of Official Analytical Chemists.

  20. Sample normalization methods in quantitative metabolomics.

    Science.gov (United States)

    Wu, Yiman; Li, Liang

    2016-01-22

    To reveal metabolomic changes caused by a biological event in quantitative metabolomics, it is critical to use an analytical tool that can perform accurate and precise quantification to examine the true concentration differences of individual metabolites found in different samples. A number of steps are involved in metabolomic analysis including pre-analytical work (e.g., sample collection and storage), analytical work (e.g., sample analysis) and data analysis (e.g., feature extraction and quantification). Each one of them can influence the quantitative results significantly and thus should be performed with great care. Among them, the total sample amount or concentration of metabolites can be significantly different from one sample to another. Thus, it is critical to reduce or eliminate the effect of total sample amount variation on quantification of individual metabolites. In this review, we describe the importance of sample normalization in the analytical workflow with a focus on mass spectrometry (MS)-based platforms, discuss a number of methods recently reported in the literature and comment on their applicability in real world metabolomics applications. Sample normalization has been sometimes ignored in metabolomics, partially due to the lack of a convenient means of performing sample normalization. We show that several methods are now available and sample normalization should be performed in quantitative metabolomics where the analyzed samples have significant variations in total sample amounts. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Determination of total mercury for marine environmental monitoring studies by solid sampling continuum source high resolution atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mandjukov, Petko; Orani, Anna Maria; Han, Eunmi; Vassileva, Emilia, E-mail: e.vasileva-veleva@iaea.org

    2015-01-01

    The most critical step in almost all commonly used analytical procedures for Hg determination is the sample preparation due to its extreme volatility. One of the possible solutions of this problem is the application of methods for direct analysis of solid samples. The possibilities for solid sampling high resolution continuum source atomic absorption spectrometry (HR CS AAS) determination of total mercury in various marine environmental samples e.g. sediments and biota are object of the present study. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signal. A calibration technique based on the use of solid standard certified reference materials similar to the nature of the analyzed sample was developed and applied to various CRMs and real samples. This technique allows simple and reliable evaluation of the uncertainty of the result and the metrological characteristics of the method. A validation approach in line with the requirements of ISO 17025 standard and Eurachem guidelines was followed. With this in mind, selectivity, working range (0.06 to 25 ng for biota and 0.025 to 4 ng for sediment samples, expressed as total Hg) linearity (confirmed by Student's t-test), bias (1.6–4.3%), repeatability (4–9%), reproducibility (9–11%), and absolute limit of detection (0.025 ng for sediment, 0.096 ng for marine biota) were systematically assessed using solid CRMs. The relative expanded uncertainty was estimated at 15% for sediment sample and 8.5% for marine biota sample (k = 2). Demonstration of traceability of measurement results is also presented. The potential of the proposed analytical procedure, based on solid sampling HR CS AAS technique was demonstrated by direct analysis of sea sediments form the Caribbean region and various CRMs. Overall, the use of solid sampling HR CS AAS permits obtaining significant advantages for the determination of this complex analyte in marine samples, such as

  2. Dynamic Method for Identifying Collected Sample Mass

    Science.gov (United States)

    Carson, John

    2008-01-01

    G-Sample is designed for sample collection missions to identify the presence and quantity of sample material gathered by spacecraft equipped with end effectors. The software method uses a maximum-likelihood estimator to identify the collected sample's mass based on onboard force-sensor measurements, thruster firings, and a dynamics model of the spacecraft. This makes sample mass identification a computation rather than a process requiring additional hardware. Simulation examples of G-Sample are provided for spacecraft model configurations with a sample collection device mounted on the end of an extended boom. In the absence of thrust knowledge errors, the results indicate that G-Sample can identify the amount of collected sample mass to within 10 grams (with 95-percent confidence) by using a force sensor with a noise and quantization floor of 50 micrometers. These results hold even in the presence of realistic parametric uncertainty in actual spacecraft inertia, center-of-mass offset, and first flexibility modes. Thrust profile knowledge is shown to be a dominant sensitivity for G-Sample, entering in a nearly one-to-one relationship with the final mass estimation error. This means thrust profiles should be well characterized with onboard accelerometers prior to sample collection. An overall sample-mass estimation error budget has been developed to approximate the effect of model uncertainty, sensor noise, data rate, and thrust profile error on the expected estimate of collected sample mass.

  3. Sharp Interface Methods for Cardiac Fluid-Solid Interaction

    Science.gov (United States)

    Kolahdouz, Ebrahim M.; Vadala-Roth, Benjamin L.; Bhalla, Amneet P. S.; Griffith, Boyce E.

    2015-11-01

    Fluid-solid systems are common in scientific and engineering applications. The immersed boundary (IB) method is a general approach to simulating fluid-structure interaction (FSI) in such systems, but a difficulty of the IB formulation of these problems is that the pressure and viscous stress are generally discontinuous at fluid-solid interfaces. The immersed interface (II) method is an IB-like approach to FSI that exactly imposes stress jump conditions, but this method has largely been limited to FSI problems involving thin elastic boundaries. We present extensions of the IB method that sharply resolve stress discontinuities at fluid-solid interfaces that can be viewed as extensions of the immersed interface method to non-interfacial (codimension-0) solid bodies, and the application of these methods to cardiovascular FSI, including the dynamics of the cardiac valves. Department of Mathematics.

  4. Solid state nuclear track detection principles, methods and applications

    CERN Document Server

    Durrani, S A; ter Haar, D

    1987-01-01

    Solid State Nuclear Track Detection: Principles, Methods and Applications is the second book written by the authors after Nuclear Tracks in Solids: Principles and Applications. The book is meant as an introduction to the subject solid state of nuclear track detection. The text covers the interactions of charged particles with matter; the nature of the charged-particle track; the methodology and geometry of track etching; thermal fading of latent damage trails on tracks; the use of dielectric track recorders in particle identification; radiation dossimetry; and solid state nuclear track detecti

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

    Science.gov (United States)

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

    2016-05-20

    The utility of matrix solid phase dispersion (MSPD) for the direct analysis of amphetamines in hair samples has been evaluated, using liquid chromatography (LC) with fluorescence detection and precolumn derivatization. The proposed approach is based on the employment of MSPD for matrix disruption and clean-up, followed by the derivatization of the analytes onto the dispersant-sample blend. The fluorogenic reagent 9-fluorenylmethyl chloroformate (FMOC) has been used for derivatization. Different conditions for MSPD, analyte purification and solid phase derivatization have been tested, using amphetamine (AMP), methamphetamine (MET), ephedrine (EPE) and 3,4-methylenedioxymethamphetamine (MDMA) as model compounds. The results have been compared with those achieved by using ultrasound-assisted alkaline digestion and by MSPD combined with conventional solution derivatization. On the basis of the results obtained, a methodology is proposed for the analysis of amphetamines in hair which integrates sample disruption, clean-up and derivatization using a C18 phase. Improved sensitivity is achieved with respect to that obtained by the alkaline digestion or by the MSPD followed by solution derivatization methods. The method can be used for the quantification of the tested amphetamines within the 2.0-20.0ng/mg concentration interval, with limits of detection (LODs) of 0.25-0.75ng/mg. The methodology is very simple and rapid (the preparation of the sample takes less than 15min). Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Method and apparatus for sampling atmospheric mercury

    Science.gov (United States)

    Trujillo, Patricio E.; Campbell, Evan E.; Eutsler, Bernard C.

    1976-01-20

    A method of simultaneously sampling particulate mercury, organic mercurial vapors, and metallic mercury vapor in the working and occupational environment and determining the amount of mercury derived from each such source in the sampled air. A known volume of air is passed through a sampling tube containing a filter for particulate mercury collection, a first adsorber for the selective adsorption of organic mercurial vapors, and a second adsorber for the adsorption of metallic mercury vapor. Carbon black molecular sieves are particularly useful as the selective adsorber for organic mercurial vapors. The amount of mercury adsorbed or collected in each section of the sampling tube is readily quantitatively determined by flameless atomic absorption spectrophotometry.

  7. Improved extraction procedures for polychlorinated biphenyls in solid samples with aqueous sodium hydroxide under autoclave conditions.

    Science.gov (United States)

    Akimoto, Y; Inouye, Y

    2000-03-01

    The efficacy of the extraction of polychlorinated biphenyls (PCBs) from varnish-infiltrated insulating papers as a model of solid materials with an aqueous sodium hydroxide (NaOH) by autoclaving at 121 degrees C for 30 min was compared with those for the conventional procedures, i.e., saponification with 1 N ethanolic NaOH in a boiling water bath for 60 min and extraction with benzene in a Soxhlet apparatus. The newly invented autoclaving method was found to be superior to the conventional ones, yielding approximately 5- to 6-fold cumulative PCB congeners without being accompanied by extended decomposition. Therefore, the autoclave-based sample treatment is recommended for more accurate determination of PCBs in the case of PCB-impregnated solid materials such as hardened oils and resin-coated or -infiltrated papers instead of being treated conventionally.

  8. Sampling of temporal networks: Methods and biases

    Science.gov (United States)

    Rocha, Luis E. C.; Masuda, Naoki; Holme, Petter

    2017-11-01

    Temporal networks have been increasingly used to model a diversity of systems that evolve in time; for example, human contact structures over which dynamic processes such as epidemics take place. A fundamental aspect of real-life networks is that they are sampled within temporal and spatial frames. Furthermore, one might wish to subsample networks to reduce their size for better visualization or to perform computationally intensive simulations. The sampling method may affect the network structure and thus caution is necessary to generalize results based on samples. In this paper, we study four sampling strategies applied to a variety of real-life temporal networks. We quantify the biases generated by each sampling strategy on a number of relevant statistics such as link activity, temporal paths and epidemic spread. We find that some biases are common in a variety of networks and statistics, but one strategy, uniform sampling of nodes, shows improved performance in most scenarios. Given the particularities of temporal network data and the variety of network structures, we recommend that the choice of sampling methods be problem oriented to minimize the potential biases for the specific research questions on hand. Our results help researchers to better design network data collection protocols and to understand the limitations of sampled temporal network data.

  9. solid phase extraction method for selective determination

    African Journals Online (AJOL)

    FATOKI

    samples that receive effluent from industries that use phthalate esters. The rivers and .... Quality Assurance Studies. A twelve- .... 2.8±0.4 4.0±0.4 a Data are means ± standard deviation for triplicate analyses. S1(EL), S2(EL) and S3(EL) are samples taken at Orient Pier, Dockyard and West Quay Sites, respectively. Generally ...

  10. A method of solid-solid phase equilibrium calculation by molecular dynamics.

    Science.gov (United States)

    Karavaev, A V; Dremov, V V

    2016-12-14

    A method for evaluation of solid-solid phase equilibrium curves in molecular dynamics simulation for a given model of interatomic interaction is proposed. The method allows to calculate entropies of crystal phases and provides an accuracy comparable with that of the thermodynamic integration method by Frenkel and Ladd while it is much simpler in realization and less intense computationally. The accuracy of the proposed method was demonstrated in MD calculations of entropies for EAM potential for iron and for MEAM potential for beryllium. The bcc-hcp equilibrium curves for iron calculated for the EAM potential by the thermodynamic integration method and by the proposed one agree quite well.

  11. Method for Predicting Solubilities of Solids in Mixed Solvents

    DEFF Research Database (Denmark)

    Ellegaard, Martin Dela; Abildskov, Jens; O'Connell, J. P.

    2009-01-01

    A method is presented for predicting solubilities of solid solutes in mixed solvents, based on excess Henry's law constants. The basis is statistical mechanical fluctuation solution theory for composition derivatives of solute/solvent infinite dilution activity coefficients. Suitable approximations...

  12. Solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for gold determination in geological samples after preconcentration onto carbon nanotubes

    Science.gov (United States)

    Dobrowolski, Ryszard; Mróz, Agnieszka; Dąbrowska, Marzena; Olszański, Piotr

    2017-06-01

    A novelty method for the determination of gold in geological samples by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry (SS HR CS GF AAS) after solid-phase extraction onto modified carbon nanotubes (CNT) was described. The methodology developed is based on solid phase extraction of Au(III) ions from digested samples to eliminate strong interference caused by iron compounds and problems related to inhomogeneities of the samples. The use of aqueous or solid standard for calibration was studied and the slope of calibration curve was the same for both of these modes. This statement indicates the possibility to perform the calibration of the method using aqueous standard solutions. Under optimum conditions the absolute detection limit for gold was equal to 2.24 · 10- 6 μg g- 1 while the adsorption capacity of modified carbon nanotubes was 264 mg g- 1. The proposed procedure was validated by the application of certified reference materials (CRMs) with different content of gold and different matrix, the results were in good agreement with certified values. The method was successfully applied for separation and determination of gold ions in complex geological samples, with precision generally better than 8%.

  13. Receiver calibration and the nonlinearity parameter measurement of thick solid samples with diffraction and attenuation corrections.

    Science.gov (United States)

    Jeong, Hyunjo; Barnard, Daniel; Cho, Sungjong; Zhang, Shuzeng; Li, Xiongbing

    2017-11-01

    This paper presents analytical and experimental techniques for accurate determination of the nonlinearity parameter (β) in thick solid samples. When piezoelectric transducers are used for β measurements, the receiver calibration is required to determine the transfer function from which the absolute displacement can be calculated. The measured fundamental and second harmonic displacement amplitudes should be modified to account for beam diffraction and material absorption. All these issues are addressed in this study and the proposed technique is validated through the β measurements of thick solid samples. A simplified self-reciprocity calibration procedure for a broadband receiver is described. The diffraction and attenuation corrections for the fundamental and second harmonics are explicitly derived. Aluminum alloy samples in five different thicknesses (4, 6, 8, 10, 12cm) are prepared and β measurements are made using the finite amplitude, through-transmission method. The effects of diffraction and attenuation corrections on β measurements are systematically investigated. When diffraction and attenuation corrections are all properly made, the variation of β between different thickness samples is found to be less than 3.2%. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2013-12-04

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

  15. Stationary semi-solid battery module and method of manufacture

    Energy Technology Data Exchange (ETDEWEB)

    Slocum, Alexander; Doherty, Tristan; Bazzarella, Ricardo; Cross, III, James C.; Limthongkul, Pimpa; Duduta, Mihai; Disko, Jeffry; Yang, Allen; Wilder, Throop; Carter, William Craig; Chiang, Yet-Ming

    2015-12-01

    A method of manufacturing an electrochemical cell includes transferring an anode semi-solid suspension to an anode compartment defined at least in part by an anode current collector and an separator spaced apart from the anode collector. The method also includes transferring a cathode semi-solid suspension to a cathode compartment defined at least in part by a cathode current collector and the separator spaced apart from the cathode collector. The transferring of the anode semi-solid suspension to the anode compartment and the cathode semi-solid to the cathode compartment is such that a difference between a minimum distance and a maximum distance between the anode current collector and the separator is maintained within a predetermined tolerance. The method includes sealing the anode compartment and the cathode compartment.

  16. A corrected solid boundary treatment method for Smoothed Particle Hydrodynamics

    Science.gov (United States)

    Chen, Yun-sai; Zheng, Xing; Jin, Shan-qin; Duan, Wen-yang

    2017-04-01

    Smoothed Particle Hydrodynamics method (SPH) has a good adaptability for simulating of free surface flow problems. However, there are some shortcomings of SPH which are still in open discussion. This paper presents a corrected solid boundary handling method for weakly compressible SPH. This improved method is very helpful for numerical stability and pressure distribution. Compared with other solid boundary handling methods, this corrected method is simpler for virtual ghost particle interpolation and the ghost particle evaluation relationship is clearer. Several numerical tests are given, like dam breaking, solitary wave impact and sloshing tank waves. The results show that the corrected solid boundary processing method can recover the spurious oscillations of pressure distribution when simulating the problems with complex geometry boundary.

  17. Sampling methods for terrestrial amphibians and reptiles.

    Science.gov (United States)

    Paul Stephen Corn; R. Bruce. Bury

    1990-01-01

    Methods described for sampling amphibians and reptiles in Douglas-fir forests in the Pacific Northwest include pitfall trapping, time-constrained collecting, and surveys of coarse woody debris. The herpetofauna of this region differ in breeding and nonbreeding habitats and vagility, so that no single technique is sufficient for a community study. A combination of...

  18. Uranium analysis by neutron induced fissionography method using solid state nuclear track detectors

    CERN Document Server

    Akyuez, T; Guezel, T; Akyuz, S

    1999-01-01

    In this study total twenty samples (eight reference materials and twelve sediment samples) were analysed for their uranium content which is in the range of 1-17 mu g/g, by neutron induced fissionography (NIF) method using solid state nuclear track detectors (SSNTDs) in comparison with the results of neutron activation analysis (NAA), delayed neutron counting (DNC) technique or fluorometric method. It is found that NIF method using SSNTDs is very sensitive for analysis of uranium.

  19. Solid Phase Microextraction and Related Techniques for Drugs in Biological Samples

    Science.gov (United States)

    Moein, Mohammad Mahdi; Said, Rana; Bassyouni, Fatma

    2014-01-01

    In drug discovery and development, the quantification of drugs in biological samples is an important task for the determination of the physiological performance of the investigated drugs. After sampling, the next step in the analytical process is sample preparation. Because of the low concentration levels of drug in plasma and the variety of the metabolites, the selected extraction technique should be virtually exhaustive. Recent developments of sample handling techniques are directed, from one side, toward automatization and online coupling of sample preparation units. The primary objective of this review is to present the recent developments in microextraction sample preparation methods for analysis of drugs in biological fluids. Microextraction techniques allow for less consumption of solvent, reagents, and packing materials, and small sample volumes can be used. In this review the use of solid phase microextraction (SPME), microextraction in packed sorbent (MEPS), and stir-bar sorbtive extraction (SBSE) in drug analysis will be discussed. In addition, the use of new sorbents such as monoliths and molecularly imprinted polymers will be presented. PMID:24688797

  20. Solid Phase Microextraction and Related Techniques for Drugs in Biological Samples

    Directory of Open Access Journals (Sweden)

    Mohammad Mahdi Moein

    2014-01-01

    Full Text Available In drug discovery and development, the quantification of drugs in biological samples is an important task for the determination of the physiological performance of the investigated drugs. After sampling, the next step in the analytical process is sample preparation. Because of the low concentration levels of drug in plasma and the variety of the metabolites, the selected extraction technique should be virtually exhaustive. Recent developments of sample handling techniques are directed, from one side, toward automatization and online coupling of sample preparation units. The primary objective of this review is to present the recent developments in microextraction sample preparation methods for analysis of drugs in biological fluids. Microextraction techniques allow for less consumption of solvent, reagents, and packing materials, and small sample volumes can be used. In this review the use of solid phase microextraction (SPME, microextraction in packed sorbent (MEPS, and stir-bar sorbtive extraction (SBSE in drug analysis will be discussed. In addition, the use of new sorbents such as monoliths and molecularly imprinted polymers will be presented.

  1. Method of fabricating lipid bilayer membranes on solid supports

    Science.gov (United States)

    Cho, Nam-Joon (Inventor); Frank, Curtis W. (Inventor); Glenn, Jeffrey S. (Inventor); Cheong, Kwang Ho (Inventor)

    2012-01-01

    The present invention provides a method of producing a planar lipid bilayer on a solid support. With this method, a solution of lipid vesicles is first deposited on the solid support. Next, the lipid vesicles are destabilized by adding an amphipathic peptide solution to the lipid vesicle solution. This destabilization leads to production of a planar lipid bilayer on the solid support. The present invention also provides a supported planar lipid bilayer, where the planar lipid bilayer is made of naturally occurring lipids and the solid support is made of unmodified gold or titanium oxide. Preferably, the supported planar lipid bilayer is continuous. The planar lipid bilayer may be made of any naturally occurring lipid or mixture of lipids, including, but not limited to phosphatidylcholine, phosphatidylethanolamine, phosphatidylserine, phosphatidylinsitol, cardiolipin, cholesterol, and sphingomyelin.

  2. Solid waste transuranic storage and assay facility indoor air sampling

    Energy Technology Data Exchange (ETDEWEB)

    Pingel, L.A., Westinghouse Hanford

    1996-08-20

    The purpose of the study is to collect and analyze samples of the indoor air at the Transuranic Storage and Assay Facility (TRUSAF), Westinghouse Hanford. A modified US EPA TO-14 methodology, using gas chromatography/mass spectrography, may be used for the collection and analysis of the samples. The information obtained will be used to estimate the total release of volatile organic compounds from TRUSAF to determine the need for air emmission permits.

  3. Are Flow Injection-based Approaches Suitable for Automated Handling of Solid Samples?

    DEFF Research Database (Denmark)

    Miró, Manuel; Hansen, Elo Harald; Cerdà, Victor

    Flow-based approaches were originally conceived for liquid-phase analysis, implying that constituents in solid samples generally had to be transferred into the liquid state, via appropriate batch pretreatment procedures, prior to analysis. Yet, in recent years, much effort has been focused...... on the design and characterisation of sample processings units coupled with flowing systems aiming to enable the direct introduction and treatment of solid samples of environmental and agricultural origin in an automated fashion [1]. In this respect, various sample pre-treatment techniques including......, multisyringe flow injection, and micro-Lab-on-valve are presented as appealing approaches for on-line handling of solid samples. Special emphasis is given to the capability of flow systems to accommodate sequential extraction protocols for partitioning of trace elements and nutrients in environmental solids (e...

  4. Environmental study of two significant solid samples: gravitation dust sediment and soil.

    Science.gov (United States)

    Remeteiová, Dagmar; Rusnák, Radoslav; Kucanová, Eva; Fióová, Beáta; Ružičková, Silvia; Fekete, Ilona; Horváth, Márk; Dirner, Vojtech

    2012-01-01

    In this work are presented results of the complex study of two significant solid environmental samples: gravitation dust sediments (industrial pollutants, potential source of risk elements input to soils) and soils (component of the environment, potential source of risk elements input to food web). The first phase of this study was focused on the study of the significant chemical properties (phase composition, content of organic and inorganic carbon) of the dust and soil samples. In the second phase, the fractionation analysis was used on the evaluation of the mobility of chosen risk elements (Cu, Ni, Pb, Zn) in the studied samples. The single-step extractions were applied in the order of the isolation of the element forms (fractions), with different mobilities during defined ecological conditions by utilization of the following reagents: 1 mol dm(-3) NH(4)NO(3) for isolation of the "mobile" fraction, 0.05 mol dm(-3) ethylenediaminetetraacetic acid and 0.43 mol dm(-3) CH(3)COOH for isolation of the "mobilizable" fraction, and 2 mol dm(-3) HNO(3) for isolation of all releasable forms. On the basis of the results obtained in this study, it is possible to state that different origins and positions of solid environmental samples in the environment reflect in different chemical properties of their matrix. The different properties of the sample matrix result in different mobilities of risk elements in these kinds of samples. The fractionation analysis with single-step extraction for isolation element fractions is the method most suitable for easy checking of environmental pollution and for evaluation of risk elements cycle in the environment.

  5. Sampling, characterisation and processing of solid recovered fuel production from municipal solid waste: An Italian plant case study.

    Science.gov (United States)

    Ranieri, Ezio; Ionescu, Gabriela; Fedele, Arcangela; Palmieri, Eleonora; Ranieri, Ada Cristina; Campanaro, Vincenzo

    2017-08-01

    This article presents the classification of solid recovered fuel from the Massafra municipal solid waste treatment plant in Southern Italy in compliancy with the EN 15359 standard. In order to ensure the reproducibility of this study, the characterisation methods of waste input and output flow, the mechanical biological treatment line scheme and its main parameters for each stage of the processing chain are presented in details, together with the research results in terms of mass balance and derived fuel properties. Under this study, only 31% of refused municipal solid waste input stream from mechanical biological line was recovered as solid recovered fuel with a net heating value (NC=HV) average of 15.77 MJ kg -1 ; chlorine content average of 0.06% on a dry basis; median of mercury fuel produced meets the European Union standard requirements and can be classified with the class code: Net heating value (3); chlorine (1); mercury (1).

  6. Determination of rhodamine B in soft drink, waste water and lipstick samples after solid phase extraction.

    Science.gov (United States)

    Soylak, Mustafa; Unsal, Yunus Emre; Yilmaz, Erkan; Tuzen, Mustafa

    2011-08-01

    A new solid phase extraction method is described for sensitive and selective determination of trace levels of rhodamine B in soft drink, food and industrial waste water samples. The method is based on the adsorption of rhodamine B on the Sepabeads SP 70 resin and its elution with 5 mL of acetonitrile in a mini chromatographic column. Rhodamine B was determined by using UV visible spectrophotometry at 556 nm. The effects of different parameters such as pH, amount of rhodamine B, flow rates of sample and eluent solutions, resin amount, and sample volume were investigated. The influences of some alkali, alkali earth and transition metals on the recoveries of rhodamine B were investigated. The preconcentration factor was found 40. The detection limit based on three times the standard deviation of the reagent blank for rhodamine B was 3.14 μg L⁻¹. The relative standard deviations of the procedure were found as 5% in 1×10⁻⁵ mol L⁻¹ rhodamine B. The presented procedure was successfully applied to real samples including soft drink, food and industrial waste water and lipstick samples. Copyright © 2011 Elsevier Ltd. All rights reserved.

  7. Advanced methods of solid oxide fuel cell modeling

    CERN Document Server

    Milewski, Jaroslaw; Santarelli, Massimo; Leone, Pierluigi

    2011-01-01

    Fuel cells are widely regarded as the future of the power and transportation industries. Intensive research in this area now requires new methods of fuel cell operation modeling and cell design. Typical mathematical models are based on the physical process description of fuel cells and require a detailed knowledge of the microscopic properties that govern both chemical and electrochemical reactions. ""Advanced Methods of Solid Oxide Fuel Cell Modeling"" proposes the alternative methodology of generalized artificial neural networks (ANN) solid oxide fuel cell (SOFC) modeling. ""Advanced Methods

  8. Development and Application of Solid Phase Extraction Method for ...

    African Journals Online (AJOL)

    NICO

    Solid phase extraction, polycyclic aromatic hydrocarbons, water samples, Johannesburg, South Africa. 1. Introduction. Polycyclic aromatic ... sewage and industrial effluents as well as for urban and rural run-off. Their solubility in ... human health and to the environment.2 Acute toxicity is gener- ally associated with the lower ...

  9. Dynamic flow-through approaches for metal fractionation in environmentally relevant solid samples

    DEFF Research Database (Denmark)

    Miró, Manuel; Hansen, Elo Harald; Chomchoei, Roongrat

    2005-01-01

    In the recent decades, batchwise equilibrium-based single or sequential extraction schemes have been consolidated as analytical tools for fractionation analyses to assess the ecotoxicological significance of metal ions in solid environmental samples. However, taking into account that naturally...

  10. Methods and devices for hyperpolarising and melting NMR samples in a cryostat

    DEFF Research Database (Denmark)

    Ardenkjaer-Larsen, Jan Henrik; Axelsson, Oskar H. E.; Golman, Klaes Koppel

    2006-01-01

    The present invention relates to devices and method for melting solid polarised sample while retaining a high level of polarisation. In an embodiment of the present invention a sample is polarised in a sample-retaining cup 9 in a strong magnetic field in a polarising means 3a, 3b, 3c in a cryosta...

  11. Determination of total mercury for marine environmental monitoring studies by solid sampling continuum source high resolution atomic absorption spectrometry

    Science.gov (United States)

    Mandjukov, Petko; Orani, Anna Maria; Han, Eunmi; Vassileva, Emilia

    2015-01-01

    The most critical step in almost all commonly used analytical procedures for Hg determination is the sample preparation due to its extreme volatility. One of the possible solutions of this problem is the application of methods for direct analysis of solid samples. The possibilities for solid sampling high resolution continuum source atomic absorption spectrometry (HR CS AAS) determination of total mercury in various marine environmental samples e.g. sediments and biota are object of the present study. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signal. A calibration technique based on the use of solid standard certified reference materials similar to the nature of the analyzed sample was developed and applied to various CRMs and real samples. This technique allows simple and reliable evaluation of the uncertainty of the result and the metrological characteristics of the method. A validation approach in line with the requirements of ISO 17025 standard and Eurachem guidelines was followed. With this in mind, selectivity, working range (0.06 to 25 ng for biota and 0.025 to 4 ng for sediment samples, expressed as total Hg) linearity (confirmed by Student's t-test), bias (1.6-4.3%), repeatability (4-9%), reproducibility (9-11%), and absolute limit of detection (0.025 ng for sediment, 0.096 ng for marine biota) were systematically assessed using solid CRMs. The relative expanded uncertainty was estimated at 15% for sediment sample and 8.5% for marine biota sample (k = 2). Demonstration of traceability of measurement results is also presented. The potential of the proposed analytical procedure, based on solid sampling HR CS AAS technique was demonstrated by direct analysis of sea sediments form the Caribbean region and various CRMs. Overall, the use of solid sampling HR CS AAS permits obtaining significant advantages for the determination of this complex analyte in marine samples, such as straightforward

  12. Matrix compatible solid phase microextraction coating, a greener approach to sample preparation in vegetable matrices.

    Science.gov (United States)

    Naccarato, Attilio; Pawliszyn, Janusz

    2016-09-01

    This work proposes the novel PDMS/DVB/PDMS fiber as a greener strategy for analysis by direct immersion solid phase microextraction (SPME) in vegetables. SPME is an established sample preparation approach that has not yet been adequately explored for food analysis in direct immersion mode due to the limitations of the available commercial coatings. The robustness and endurance of this new coating were investigated by direct immersion extractions in raw blended vegetables without any further sample preparation steps. The PDMS/DVB/PDMS coating exhibited superior features related to the capability of the external PDMS layer to protect the commercial coating, and showed improvements in terms of extraction capability and in the cleanability of the coating surface. In addition to having contributed to the recognition of the superior features of this new fiber concept before commercialization, the outcomes of this work serve to confirm advancements in the matrix compatibility of the PDMS-modified fiber, and open new prospects for the development of greener high-throughput analytical methods in food analysis using solid phase microextraction in the near future. Copyright © 2016 Elsevier Ltd. All rights reserved.

  13. Endoscopic ultrasound-guided sampling of solid pancreatic masses: 22-gauge aspiration versus 25-gauge biopsy needles

    OpenAIRE

    Yang, Min Jae; Yim, Hyunee; Hwang, Jae Chul; Lee, Dakeun; Kim, Young Bae; Lim, Sun Gyo; Kim, Soon Sun; Kang, Joon Koo; Yoo, Byung Moo; Kim, Jin Hong

    2015-01-01

    Background Biopsy needles have recently been developed to obtain both cytological and histological specimens during endoscopic ultrasound (EUS). We conducted this study to compare 22-gauge (G) fine needle aspiration (FNA) needles, which have been the most frequently used, and new 25G fine needle biopsy (FNB) needles for EUS-guided sampling of solid pancreatic masses. Methods We conducted a retrospective cohort study of all EUS-guided sampling performed between June 2010 and October 2013. Duri...

  14. Development of a depth-integrated sample arm (DISA) to reduce solids stratification bias in stormwater sampling

    Science.gov (United States)

    Selbig, William R.; ,; Roger T. Bannerman,

    2011-01-01

    A new depth-integrated sample arm (DISA) was developed to improve the representation of solids in stormwater, both organic and inorganic, by collecting a water quality sample from multiple points in the water column. Data from this study demonstrate the idea of vertical stratification of solids in storm sewer runoff. Concentrations of suspended sediment in runoff were statistically greater using a fixed rather than multipoint collection system. Median suspended sediment concentrations measured at the fixed location (near the pipe invert) were approximately double those collected using the DISA. In general, concentrations and size distributions of suspended sediment decreased with increasing vertical distance from the storm sewer invert. Coarser particles tended to dominate the distribution of solids near the storm sewer invert as discharge increased. In contrast to concentration and particle size, organic material, to some extent, was distributed homogenously throughout the water column, likely the result of its low specific density, which allows for thorough mixing in less turbulent water.

  15. Studies of human and veterinary drugs' fate in environmental solid samples--analytical problems.

    Science.gov (United States)

    Wilga, Joanna; Kot-Wasik, Agata; Namieśnik, Jacek

    2008-08-01

    The improvement of medical care worldwide is one of the reasons for the increasing production of pharmaceutical products. Human medicines are affordable to a greater proportion of the world's population. But a significant amount of used pharmaceuticals can create problems--accessibility to high volume production pharmaceuticals contributes to an increased contamination in the environment and the possibility of adverse effects on humans and animals. Many of these substances and their metabolites end up in the soil, sediments, and sludge. Knowledge regarding the environmental occurrence of pharmaceutical products is increasing, but information in the peer-reviewed literature regarding the fate and effects of most pharmaceuticals is limited. One of the reasons for this lack of data is that, until now, there have been few analytical methods capable of detecting these compounds at the low levels, which might be expected in the environment. This review article covers recent developments in the analysis of pharmaceuticals in environmental solid matrices (including soil, sediments, and sludge). We will report applications of different solid sample extraction methods, and current advances in liquid chromatography coupled with mass spectrometry for detection and identification of selected drugs in sludge, soils, manure, and sediments.

  16. Method to fabricate high performance tubular solid oxide fuel cells

    Science.gov (United States)

    Chen, Fanglin; Yang, Chenghao; Jin, Chao

    2013-06-18

    In accordance with the present disclosure, a method for fabricating a solid oxide fuel cell is described. The method includes forming an asymmetric porous ceramic tube by using a phase inversion process. The method further includes forming an asymmetric porous ceramic layer on a surface of the asymmetric porous ceramic tube by using a phase inversion process. The tube is co-sintered to form a structure having a first porous layer, a second porous layer, and a dense layer positioned therebetween.

  17. Stabilizing Agents for Calibration in the Determination of Mercury Using Solid Sampling Electrothermal Atomic Absorption Spectrometry

    Science.gov (United States)

    Zelinková, Hana; Červenka, Rostislav; Komárek, Josef

    2012-01-01

    Tetramethylene dithiocarbamate (TMDTC), diethyldithiocarbamate (DEDTC), and thiourea were investigated as stabilizing agents for calibration purposes in the determination of mercury using solid sampling electrothermal atomic absorption spectrometry (SS-ETAAS). These agents were used for complexation of mercury in calibration solutions and its thermal stabilization in a solid sampling platform. The calibration solutions had the form of methyl isobutyl ketone (MIBK) extracts or MIBK-methanol solutions with the TMDTC and DEDTC chelates and aqueous solutions with thiourea complexes. The best results were obtained for MIBK-methanol solutions in the presence of 2.5 g L−1 TMDTC. The surface of graphite platforms for solid sampling was modified with palladium or rhenium by using electrodeposition from a drop of solutions. The Re modifier is preferable due to a higher lifetime of platform coating. A new SS-ETAAS procedure using the direct sampling of solid samples into a platform with an Re modified graphite surface and the calibration against MIBK-methanol solutions in the presence of TMDTC is proposed for the determination of mercury content in solid environmental samples, such as soil and plants. PMID:22654606

  18. Preparation of molecularly imprinted polymeric fibers using a single bifunctional monomer for the solid-phase microextraction of parabens from environmental solid samples.

    Science.gov (United States)

    Díaz-Álvarez, Myriam; Smith, Stephen P; Spivak, David A; Martín-Esteban, Antonio

    2016-02-01

    In this study, molecularly imprinted polymer fibers for solid-phase microextraction have been prepared with a single bifunctional monomer, N,O-bismethacryloyl ethanolamine using the so-called "one monomer molecularly imprinted polymers" method, replacing the conventional combination of functional monomer and cross-linker to form high fidelity binding sites. For comparison, imprinted fibers were prepared following the conventional approach based on ethylene glycol dimethacrylate as cross-linker and methacrylic acid as monomer. The recognition performance of the new fibers was evaluated in the solid-phase microextraction of parabens, and from this study it was concluded that they provided superior performance over conventionally formulated fibers. Ultimately, real-world environmental testing on spiked solid samples was successful by the molecularly imprinted solid-phase microextraction of samples, and the relative recoveries obtained at enrichment levels of 10 ng/g of parabens were within 78-109% for soil and 83-109% for sediments with a relative standard deviation <15% (n = 3). © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Automated, Ultra-Sterile Solid Sample Handling and Analysis on a Chip

    Science.gov (United States)

    Mora, Maria F.; Stockton, Amanda M.; Willis, Peter A.

    2013-01-01

    There are no existing ultra-sterile lab-on-a-chip systems that can accept solid samples and perform complete chemical analyses without human intervention. The proposed solution is to demonstrate completely automated lab-on-a-chip manipulation of powdered solid samples, followed by on-chip liquid extraction and chemical analysis. This technology utilizes a newly invented glass micro-device for solid manipulation, which mates with existing lab-on-a-chip instrumentation. Devices are fabricated in a Class 10 cleanroom at the JPL MicroDevices Lab, and are plasma-cleaned before and after assembly. Solid samples enter the device through a drilled hole in the top. Existing micro-pumping technology is used to transfer milligrams of powdered sample into an extraction chamber where it is mixed with liquids to extract organic material. Subsequent chemical analysis is performed using portable microchip capillary electrophoresis systems (CE). These instruments have been used for ultra-highly sensitive (parts-per-trillion, pptr) analysis of organic compounds including amines, amino acids, aldehydes, ketones, carboxylic acids, and thiols. Fully autonomous amino acid analyses in liquids were demonstrated; however, to date there have been no reports of completely automated analysis of solid samples on chip. This approach utilizes an existing portable instrument that houses optics, high-voltage power supplies, and solenoids for fully autonomous microfluidic sample processing and CE analysis with laser-induced fluorescence (LIF) detection. Furthermore, the entire system can be sterilized and placed in a cleanroom environment for analyzing samples returned from extraterrestrial targets, if desired. This is an entirely new capability never demonstrated before. The ability to manipulate solid samples, coupled with lab-on-a-chip analysis technology, will enable ultraclean and ultrasensitive end-to-end analysis of samples that is orders of magnitude more sensitive than the ppb goal given

  20. System and Method for Isolation of Samples

    Science.gov (United States)

    Zhang, Ye (Inventor); Wu, Honglu (Inventor)

    2014-01-01

    Systems and methods for isolating samples are provided. The system comprises a first membrane and a second membrane disposed within an enclosure. First and second reservoirs can also be disposed within the enclosure and adapted to contain one or more reagents therein. A first valve can be disposed within the enclosure and in fluid communication with the first reservoir, the second reservoir, or both. The first valve can also be in fluid communication with the first or second membranes or both. The first valve can be adapted to selectively regulate the flow of the reagents from the first reservoir, through at least one of the first and second membranes, and into the second reservoir.

  1. Applications of magnetic surface imprinted materials for solid phase extraction of levofloxacin in serum samples.

    Science.gov (United States)

    Xiao, Deli; Wang, Cuixia; Dai, Hao; Peng, Jun; He, Jia; Zhang, Kai; Kong, Sumei; Qiu, Panzi; He, Hua

    2015-05-01

    In this work, molecularly imprinted magnetic carbon nanotubes (MCNTs@MIPs) was prepared with surface imprinting technique for extraction of levofloxacin in serum samples. The preparation of molecularly imprinted polymers (MIPs) used levofloxacin as template, methacrylic acid as functional monomer, and ethylene glycol dimethacrylate as cross-linker, and the magnetic carbon nanotubes (MCNTs) was synthesized by solvothermal method. The prepared polymers not only can be separated and collected easily by an external magnetic, but also exhibited high specific surface area and high selectivity to template molecules. Kinetic adsorption and static adsorption capacity investigations indicated that the synthesized MCNTs@MIPs had excellent recognition towards levofloxacin. Furthermore, magnetic solid phase extraction (MSPE) using the prepared MCNTs@MIPs as sorbent was then investigated, and an efficient sample cleanup was obtained with recoveries ranged from 78.7 ± 4.8 % to 83.4 ± 4.1%. In addition, several parameters, including the pH of samples, the amount of MCNTs@MIPs, the adsorption and desorption times, and the eluent, were investigated to obtain optimal extraction efficiency. Under the optimal extraction conditions, the stability of the polymer was also evaluated, and the average recovery reduced less than 7.6% after 5 cycles. MCNTs@MIPs successfully applied in the preconcentration and determination of levofloxacin in serum sample suggested that the MSPE method based on the novel polymers could be a promising alternative for selective and efficient extraction of trace amounts of pharmaceutical substances in bio-matrix samples. Copyright © 2015 John Wiley & Sons, Ltd.

  2. Determination of melamine in aquaculture feed samples based on molecularly imprinted solid-phase extraction.

    Science.gov (United States)

    Lian, Ziru; Liang, Zhenlin; Wang, Jiangtao

    2015-10-01

    This research highlights the application of highly efficient molecularly imprinted solid-phase extraction for the preconcentration and analysis of melamine in aquaculture feed samples. Melamine-imprinted polymers were synthesized employing methacrylic acid and ethylene glycol dimethacrylate as functional monomer and cross-linker, respectively. The characteristics of obtained polymers were evaluated by scanning electron microscopy, Fourier transform infrared spectroscopy and binding experiments. The imprinted polymers showed an excellent adsorption ability for melamine and were applied as special solid-phase extraction sorbents for the selective cleanup of melamine. An off-line molecularly imprinted solid-phase extraction procedure was developed for the separation and enrichment of melamine from aquaculture feed samples prior to high-performance liquid chromatography analysis. Optimum molecularly imprinted solid-phase extraction conditions led to recoveries of the target in spiked feed samples in the range 84.6-96.6% and the relative standard deviation less than 3.38% (n = 3). The aquaculture feed sample was determined, and there was no melamine found. The results showed that the molecularly imprinted solid-phase extraction protocols permitted the sensitive, uncomplicated and inexpensive separation and pre-treatment of melamine in aquaculture feed samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Glass bottle sampling solid phase microextraction gas chromatography mass spectrometry for breath analysis of drug metabolites.

    Science.gov (United States)

    Lu, Yan; Niu, Wenqi; Zou, Xue; Shen, Chengyin; Xia, Lei; Huang, Chaoqun; Wang, Hongzhi; Jiang, Haihe; Chu, Yannan

    2017-05-05

    Breath analysis is a non-invasive approach which may be applied to disease diagnosis and pharmacokinetic study. In the case of offline analysis, the exhaled gas needs to be collected and the sampling bag is often used as the storage vessel. However, the sampling bag usually releases some extra compounds, which may interfere with the result of the breath test. In this study, a novel breath sampling glass bottle was developed with a syringe needle sampling port for solid phase microextraction (SPME). Such a glass bottle scarcely liberates compounds and can be used to collect exhaled gas for ensuing analysis by gas chromatography-mass spectrometry (GC-MS). The glass bottle sampling SPME-GC-MS analysis was carried out to investigate the breath metabolites of myrtol, a multicompound drug normally used in the treatment of bronchitis and sinusitis. Four compounds, α-pinene, 2,3-dehydro-1,8-cineole, d-limonene and 1,8-cineole were found in the exhaled breath of all eight volunteers who had taken the myrtol. While for other ten subjects who had not used the myrtol, these compounds were undetectable. In the SPME-GC-MS analysis of the headspace of myrtol, three compounds were detected including α-pinene, d-limonene and 1,8-cineole. Comparing the results of breath and headspace analysis, it indicates that 2,3-dehydro-1,8-cineole in the breath is the metabolite of 1,8-cineole. It is the first time that this metabolite was identified in human breath. The study demonstrates that the glass bottle sampling SPME-GC-MS method is applicable to exhaled gas analysis including breath metabolites investigation of drugs like myrtol. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. A hybrid grid method in an auxiliary coordinate system for irregular fluid-solid interface modelling

    Science.gov (United States)

    Qu, Yingming; Huang, Jianping; Li, Zhenchun; Li, Jinli

    2017-03-01

    Seismic wave propagation in a fluid-solid environment cannot be simulated with a single wave equation, but can be described by use of the acoustic and viscoelastic wave equations for their respective fluid and solid parts. Proper boundary conditions at the fluid-solid interface based on the relationship between pressure and stress are crucial when combining the two different wave equations. Traditional finite difference methods have had difficulties in dealing with the irregular fluid-solid interface topography. The Cartesian grids discretization leads to artificial reflections and diffractions during the conversion between acoustic wave and elastic waves. We propose a variable coordinate transformation methodology to simulate seismic waves in a fluid-solid environment. An irregular fluid-solid interface can be transformed into a horizontal interface, so that pressure and stress can be well converted. We also introduce a multiblock coordinate transformation (MCT) method which meshes each layer with curvilinear grids to transform the interface topography into a horizontal one, thereby allocating vertical sampling points adaptively. The grid size is determined adaptively based on the shape and the parameters of the target area, which reduces in size in when the layers are thin or exhibit low velocities. A Lebedev-standard staggered grid scheme is applied to the MCT method to reduce both the computational cost associated with the Lebedev grid scheme and the instability in the auxiliary coordinate system when using a standard staggered grid scheme.

  5. Sampling trace organic compounds in water: a comparison of a continuous active sampler to continuous passive and discrete sampling methods

    Science.gov (United States)

    Coes, Alissa L.; Paretti, Nicholas V.; Foreman, William T.; Iverson, Jana L.; Alvarez, David A.

    2014-01-01

    A continuous active sampling method was compared to continuous passive and discrete sampling methods for the sampling of trace organic compounds (TOCs) in water. Results from each method are compared and contrasted in order to provide information for future investigators to use while selecting appropriate sampling methods for their research. The continuous low-level aquatic monitoring (CLAM) sampler (C.I.Agent® Storm-Water Solutions) is a submersible, low flow-rate sampler, that continuously draws water through solid-phase extraction media. CLAM samplers were deployed at two wastewater-dominated stream field sites in conjunction with the deployment of polar organic chemical integrative samplers (POCIS) and the collection of discrete (grab) water samples. All samples were analyzed for a suite of 69 TOCs. The CLAM and POCIS samples represent time-integrated samples that accumulate the TOCs present in the water over the deployment period (19–23 h for CLAM and 29 days for POCIS); the discrete samples represent only the TOCs present in the water at the time and place of sampling. Non-metric multi-dimensional scaling and cluster analysis were used to examine patterns in both TOC detections and relative concentrations between the three sampling methods. A greater number of TOCs were detected in the CLAM samples than in corresponding discrete and POCIS samples, but TOC concentrations in the CLAM samples were significantly lower than in the discrete and (or) POCIS samples. Thirteen TOCs of varying polarity were detected by all of the three methods. TOC detections and concentrations obtained by the three sampling methods, however, are dependent on multiple factors. This study found that stream discharge, constituent loading, and compound type all affected TOC concentrations detected by each method. In addition, TOC detections and concentrations were affected by the reporting limits, bias, recovery, and performance of each method.

  6. Mydriatics release from solid and semi-solid ophthalmic formulations using different in vitro methods.

    Science.gov (United States)

    Pescina, Silvia; Macaluso, Claudio; Gioia, Gloria Antonia; Padula, Cristina; Santi, Patrizia; Nicoli, Sara

    2017-09-01

    The aim of the present paper was the development of semi-solid (hydrogels) and solid (film) ophthalmic formulations for the controlled release of two mydriatics: phenylephrine and tropicamide. The formulations - based on polyvinylalcohol and hyaluronic acid - were characterized, and release studies were performed with three different in vitro set-ups, i.e. Franz-type diffusion cell, vial method and inclined plane; for comparison, a solution and a commercial insert, both clinically used to induce mydriasis, were evaluated. Both gels and film allowed for a controlled release of drugs, appearing a useful alternative for mydriatics administration. However, the release kinetic was significantly influenced by the method used, highlighting the need for optimization and standardization of in vitro models for the evaluation of drug release from ophthalmic dosage forms.

  7. Passive sampling of ambient ozone by solid phase microextraction with on-fiber derivatization.

    Science.gov (United States)

    Lee, I-Su; Tsai, Shih-Wei

    2008-03-10

    The solid phase microextraction (SPME) device with the polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber was used as a passive sampler for ambient ozone. Both O-2,3,4,5,6-(pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) and 1,2-di-(4-pyridyl)ethylene (DPE) were loaded onto the fiber before sampling. The SPME fiber assembly was then inserted into a PTFE tubing as a passive sampler. Known concentrations of ozone around the ambient ground level were generated by a calibrated ozone generator. Laboratory validations of the SPME passive sampler with the direct-reading ozone monitor were performed side-by-side in an exposure chamber at 25 degrees C. After exposures, pyriden-4-aldehyde was formed due to the reaction between DPE and ozone. Further on-fiber derivatizations between pyriden-4-aldehyde and PFBHA were followed and the derivatives, oximes, were then determined by portable gas chromatography with electron capture detector. The experimental sampling rate of the SPME ozone passive sampler was found to be 1.10 x 10(-4) cm(3) s(-1) with detection limit of 58.8 microg m(-3) h(-1). Field validations with both SPME device and the direct-reading ozone monitor were also performed. The correlations between the results from both methods were found to be consistent with r=0.9837. Compared with other methods, the current designed sampler provides a convenient and sensitive tool for the exposure assessments of ozone.

  8. Multiple pesticide analysis in wine by MEKC combined with solid-phase microextraction and sample stacking.

    Science.gov (United States)

    Ravelo-Pérez, Lidia M; Hernández-Borges, Javier; Borges-Miquel, Teresa M; Rodríguez-Delgado, Miguel A

    2007-11-01

    In this work, a new method for the determination in white wines of 12 pesticides widely used in vine cultivars (namely, carbendazim, pirimicarb, metalaxyl, pyrimethanil, procymidone, nuarimol, azoxystrobin, tebufenozide, fenarimol, benalaxyl, penconazole, and tetradifon) using solid-phase microextraction (SPME) and MEKC with diode-array detection (DAD) was developed. The MEKC buffer consisted of 100 mM sodium tetraborate and 30 mM SDS at pH 8.5 with 6% v/v 1-propanol. Reversed-electrode polarity stacking mode (REPSM) was applied as on-line preconcentration strategy. In order to carry out an effective and sensitive determination of these pesticides in wine samples, an off-line SPME procedure was optimized by means of an experimental design. After studying the extraction performance of different SPME coatings, PDMS/divinylbenzene (PDMS/DVB) fibers were found the most appropriate for the extraction of most of these pesticides. Carbendazim and metalaxyl could not be extracted from wine samples. Calibration curves for extracted standards and fortified white wines were studied in order to determine the presence of a matrix effect. The combination of both preconcentration procedures (SPME and REPSM) allowed the determination of ten of these pesticides in white wines at concentrations between 0.054 and 0.113 mg/L. (i.e., levels well below the maximum residue limits (MRLs) allowed for these compounds in wine grapes). Ten homemade wines were they analyzed with the optimized method demonstrating the usefulness of the proposed procedure.

  9. Sampling of benzene in tar matrices from biomass gasification using two different solid-phase sorbents.

    Science.gov (United States)

    Osipovs, Sergejs

    2008-06-01

    Biomass tar mainly consists of stable aromatic compounds such as benzene and polyaromatic hydrocarbons, benzene being the biggest tar component in real biomass gasification gas. For the analysis of individual tar compounds, the solid-phase adsorption method was chosen. According to this method, tar samples are collected on a column with an amino-phase sorbent. With a high benzene concentration in biomass tar, some of the benzene will not be collected on the amino-phase sorbent. To get over this situation, we have installed another column with activated charcoal which is intended for collection of volatile organic compounds, including benzene, after the column with the amino-phase sorbent. The study of maximal adsorption amounts of various compounds on both adsorbents while testing different sampling volumes led to the conclusion that benzene is a limiting compound. The research proved that the use of two sorbents (500 mg + 100 mg) connected in series allows for assessment of tar in synthesis gas with a tar concentration up to 30-40 g m(-3), which corresponds to the requirements of most gasifiers.

  10. High purity polyimide analysis by solid sampling graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Santos, Rafael F.; Carvalho, Gabriel S.; Duarte, Fabio A.; Bolzan, Rodrigo C.; Flores, Erico M. M.

    2017-03-01

    In this work, Cr, Cu, Mn, Na and Ni were determined in high purity polyimides (99.5%) by solid sampling graphite furnace atomic absorption spectrometry (SS-GFAAS) using Zeeman effect background correction system with variable magnetic field, making possible the simultaneous measurement at high or low sensitivity. The following analytical parameters were evaluated: pyrolysis and atomization temperatures, feasibility of calibration with aqueous solution, linear calibration range, sample mass range and the use of chemical modifier. Calibration with aqueous standard solutions was feasible for all analytes. No under or overestimated results were observed and up to 10 mg sample could be introduced on the platform for the determination of Cr, Cu, Mn, Na and Ni. The relative standard deviation ranged from 3 to 20%. The limits of detection (LODs) achieved using the high sensitivity mode were as low as 7.0, 2.5, 1.7, 17 and 0.12 ng g- 1 for Cr, Cu, Mn, Na and Ni, respectively. No addition of chemical modifier was necessary, except for Mn determination where Pd was required. The accuracy was evaluated by analyte spike and by comparison of the results with those obtained by inductively coupled plasma optical emission spectrometry and inductively coupled plasma mass spectrometry after microwave-assisted digestion in a single reaction chamber system and also by neutron activation analysis. No difference among the results obtained by SS-GFAAS and those obtained by alternative analytical methods using independent techniques. SS-GFAAS method showed some advantages, such as the determination of metallic contaminants in high purity polyimides with practically no sample preparation, very low LODs, calibration with aqueous standards and determination in a wide range of concentration.

  11. Sample results from the interim salt disposition program macrobatch 8 tank 21H qualification MST solids sample

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-02-01

    Savannah River National Laboratory (SRNL) analyzed samples from Tank 21H in support of qualification of Macrobatch (Salt Batch) 8 for Interim Salt Disposition Program (ISDP) processing. As part of this qualification work, SRNL performed an Actinide Removal Process (ARP) and several Extraction, Scrub, Strip (ESS) tests. This document reports characterization of the monosodium titanate (MST) solids from the ARP test. The results of these analyses are reported and are within historical precedent.

  12. An interlaboratory study as useful tool for proficiency testing of chemical oxygen demand measurements using solid substrates and liquid samples with high suspended solid content.

    Science.gov (United States)

    Raposo, F; de la Rubia, M A; Borja, R; Alaiz, M; Beltrán, J; Cavinato, C; Clinckspoor, M; Demirer, G; Diamadopoulos, E; Helmreich, B; Jenicek, P; Martí, N; Méndez, R; Noguerol, J; Pereira, F; Picard, S; Torrijos, M

    2009-11-15

    In 2008, the first Proficiency Testing Scheme of Chemical Oxygen Demand (1(st)COD-PT(ADG)) was conducted to assess the results obtained for different research groups whose field work is mainly anaerobic digestion. This study was performed using four samples, two solid samples as raw materials and two solid samples to prepare high concentration suspended solid solutions. Invitations were sent to a large number of laboratories, mainly to anaerobic digestion research groups. Finally, thirty labs from sixteen countries agreed to participate, but for different reasons four participants could not send any data. In total, twenty-six results were reported to the COD-PT coordinator. This study showed the importance of continuous participation in proficiency testing (PT) schemes in order to compare the results obtained. Taking into account the lack of a general standard method and high quality certified reference materials (CRMs), the traceability of COD determination is not currently easy to check. In addition, the spread of participants' results obtained was high and pointed to the advisability of using consensus values due to their unreliability. Therefore, the theoretical oxygen demand (ThOD) values were considered as assigned values for all the samples analysed. On the other hand, in this PT the established standard deviation (ESD) has been determined by the Horwitz modified function. Participants of this 1(st)COD-PT(ADG) were asked to give a short report on the analytical method used. Although all the participants used potassium dichromate as their oxidant reagent, their experimental procedures were very different. With the purpose of comparing the results obtained, the different experimental conditions used were classified into five methods, corresponding to two main categories, open and closed reflux. The performance of laboratories was expressed by the z-score, whose value is considered satisfactory when z-score

  13. A modified method for COD determination of solid waste, using a commercial COD kit and an adapted disposable weighing support.

    Science.gov (United States)

    André, L; Pauss, A; Ribeiro, T

    2017-03-01

    The chemical oxygen demand (COD) is an essential parameter in waste management, particularly when monitoring wet anaerobic digestion processes. An adapted method to determine COD was developed for solid waste (total solids >15%). This method used commercial COD tubes and did not require sample dilution. A homemade plastic weighing support was used to transfer the solid sample into COD tubes. Potassium hydrogen phthalate and glucose used as standards showed an excellent repeatability. A small underestimation of the theoretical COD value (standard values around 5% lower than theoretical values) was also observed, mainly due to the intrinsic COD of the weighing support and to measurement uncertainties. The adapted COD method was tested using various solid wastes in the range of 1-8 mg COD , determining the COD of dried and ground cellulose, cattle manure, straw and a mixed-substrate sample. This new adapted method could be used to monitor and design dry anaerobic digestion processes.

  14. Apparatus and method for solid fuel chemical looping combustion

    Energy Technology Data Exchange (ETDEWEB)

    Siriwardane, Ranjani V; Weber, Justin M

    2015-04-14

    The disclosure provides an apparatus and method utilizing fuel reactor comprised of a fuel section, an oxygen carrier section, and a porous divider separating the fuel section and the oxygen carrier section. The porous divider allows fluid communication between the fuel section and the oxygen carrier section while preventing the migration of solids of a particular size. Maintaining particle segregation between the oxygen carrier section and the fuel section during solid fuel gasification and combustion processes allows gases generated in either section to participate in necessary reactions while greatly mitigating issues associated with mixture of the oxygen carrier with char or ash products. The apparatus and method may be utilized with an oxygen uncoupling oxygen carrier such as CuO, Mn.sub.3O.sub.4, or Co.sub.3O.sub.4, or utilized with a CO/H.sub.2 reducing oxygen carrier such as Fe.sub.2O.sub.3.

  15. On-line sample processing methods in flow analysis

    DEFF Research Database (Denmark)

    Miró, Manuel; Hansen, Elo Harald

    2008-01-01

    -line dilution, derivatization, separation and preconcentration methods encompassing solid reactors, solvent extraction, sorbent extraction, precipitation/coprecipitation, hydride/vapor generation and digestion/leaching protocols as hyphenated to a plethora of detection devices is discussed in detail...

  16. Broth versus solid agar culture of swab samples of cadaveric allograft musculoskeletal tissue.

    Science.gov (United States)

    Varettas, Kerry

    2013-12-01

    As part of the donor assessment protocol, bioburden assessment must be performed on allograft musculoskeletal tissue samples collected at the time of tissue retrieval. Swab samples of musculoskeletal tissue allografts from cadaveric donors are received at the microbiology department of the South Eastern Area Laboratory Services (Australia) to determine the presence of bacteria and fungi. This study will review the isolation rate of organisms from solid agar and broth culture of swab samples of cadaveric allograft musculoskeletal tissue over a 6-year period, 2006-2011. Swabs were inoculated onto horse blood agar (anaerobic, 35 °C) and chocolate agar (CO2, 35 °C) and then placed into a cooked meat broth (aerobic, 35 °C). A total of 1,912 swabs from 389 donors were received during the study period. 557 (29.1 %) swabs were culture positive with the isolation of 713 organisms, 249 (34.9 %) from solid agar culture and an additional 464 (65.1 %) from broth culture only. This study has shown that the broth culture of cadaveric allograft musculoskeletal swab samples recovered a greater amount of organisms than solid agar culture. Isolates such as Clostridium species and Staphylococcus aureus would not have been isolated from solid agar culture alone. Broth culture is an essential part of the bioburden assessment protocol of swab samples of cadaveric allograft musculoskeletal tissue in this laboratory.

  17. Towards steady-state direct solid sample analysis by inductively coupled plasma atomic emission spectrometry: qualitative evaluation of an intraplasmic powdered sample digester

    Science.gov (United States)

    Hamier, Jan; Salin, Eric D.

    1998-08-01

    A new type of reactor designed for continuous halogen-assisted digestion and analysis of powdered samples was evaluated. Two different halogenating gas introduction methods were tested, as well as the use of an internal baffle to increase the residence time of the solids inside the reactor. Studies were carried out on Al 2O 3 and CuO as model compounds for optimization of the reactor's parameters, such as the carrier gas flow, the fraction of halogenating gas and the feed rate, using Freon-12 as the halogenating gas. A qualitative study of a pseudo fluidized bed reactor (PFBR) was also performed on a soil sample certified reference material (SO-4). The internal gas flow rate had to be kept to an absolute minimum in order to minimize cooling of the PFBR's inner walls. Pre-mixing of the halogenating reagent into the solid aerosol carrier resulted in a much more efficient reaction than separate flow introduction. The use of a baffle drastically improved the digestion efficiency by virtue of an increased solid residence time. The argon plasma did not have a sufficiently high heat transfer capability to ensure proper operation of the PFBR under continuous sample loading. The porosity of the graphite used for the PFBR construction caused some tailing and memory effects due to analyte seepage into the reactor's walls.

  18. Solid electrolyte material manufacturable by polymer processing methods

    Science.gov (United States)

    Singh, Mohit; Gur, Ilan; Eitouni, Hany Basam; Balsara, Nitash Pervez

    2012-09-18

    The present invention relates generally to electrolyte materials. According to an embodiment, the present invention provides for a solid polymer electrolyte material that is ionically conductive, mechanically robust, and can be formed into desirable shapes using conventional polymer processing methods. An exemplary polymer electrolyte material has an elastic modulus in excess of 1.times.10.sup.6 Pa at 90 degrees C. and is characterized by an ionic conductivity of at least 1.times.10.sup.-5 Scm-1 at 90 degrees C. An exemplary material can be characterized by a two domain or three domain material system. An exemplary material can include material components made of diblock polymers or triblock polymers. Many uses are contemplated for the solid polymer electrolyte materials. For example, the present invention can be applied to improve Li-based batteries by means of enabling higher energy density, better thermal and environmental stability, lower rates of self-discharge, enhanced safety, lower manufacturing costs, and novel form factors.

  19. Collection of solid and gaseous samples to diagnose inertial confinement fusion implosions.

    Science.gov (United States)

    Stoyer, M A; Velsko, C A; Spears, B K; Hicks, D G; Hudson, G B; Sangster, T C; Freeman, C G

    2012-02-01

    Collection of representative samples of debris following inertial confinement fusion implosions in order to diagnose implosion conditions and efficacy is a challenging endeavor because of the unique conditions within the target chamber such as unconverted laser light, intense pulse of x-rays, physical chunks of debris, and other ablative effects. We present collection of gas samples following an implosion for the first time. High collection fractions for noble gases were achieved. We also present collection of solid debris samples on flat plate collectors. Geometrical collection efficiencies for Au hohlraum material were achieved and collection of capsule debris (Be and Cu) was also observed. Asymmetric debris distributions were observed for Au and Be samples. Collection of Be capsule debris was higher for solid collectors viewing the capsule through the laser entrance hole in the hohlraum than for solid collectors viewing the capsule around the waist of the hohlraum. Collection of Au hohlraum material showed the opposite pattern: more Au debris was collected around the waist than through the laser entrance hole. The solid debris collectors were not optimized for minimal Cu backgrounds, which limited the conclusions about the symmetry of the Cu debris. The quality of the data limited conclusions on chemical fractionation effects within the burning, expanding, and then cooling plasma.

  20. Analysis of anatoxin-a in biological samples using liquid chromatography with fluorescence detection after solid phase extraction and solid phase microextraction.

    Science.gov (United States)

    Rellán, Sandra; Osswald, Joana; Vasconcelos, Vitor; Gago-Martinez, Ana

    2007-07-13

    Anatoxin-a is a naturally occurring, potent neurotoxin produced by some species of cyanobacteria in freshwaters. This toxin, which is a potential health hazard, especially to animals, has been determined in different biological matrices such as several cyanobacterial cultures and water samples and carps and mussels tissue using a sensitive High Performance Liquid Chromatography with Fluorescence detection method. Sonication was the technique selected for the extraction of intracellular anatoxin-a and solid phase extraction using weak cation exchange was used for the concentration and purification of the samples. 4-Fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) was used to convert anatoxin into a highly fluorescent derivative. Recovery experiments were performed for each type of matrix used in this work, and adequate values were obtained (71-87%). Limits of detection for anatoxin-a were estimated to be in the ng/L and ng/g level for water and cyanobacterial samples, respectively. The results obtained were also compared with those obtained after using solid phase microextraction, as an alternative for the extraction and purification of the samples. Advantages and disadvantages regarding to the efficiency for impurities removal, simplicity and rapidity and the potential for concentration enhancement of using both methodologies have been also discussed.

  1. Dissipation peak as an indicator of sample inhomogeneity in solid $^4$He oscillator experiments

    OpenAIRE

    Huse, David A.; Khandker, Zuhair U.

    2007-01-01

    A simple phenomenological model is developed for the recent torsional oscillator experiments on solid $^4$He. Within this model, for a homogeneous sample there is a specific quantitative relation between the change in the oscillator's frequency and its maximum damping at the apparent supersolid transition. Much of the published data do not satisfy this relation, indicating that the dissipation peaks in those samples are strongly inhomogeneously broadened.

  2. Statistical sampling method, used in the audit

    Directory of Open Access Journals (Sweden)

    Gabriela-Felicia UNGUREANU

    2010-05-01

    Full Text Available The rapid increase in the size of U.S. companies from the early twentieth century created the need for audit procedures based on the selection of a part of the total population audited to obtain reliable audit evidence, to characterize the entire population consists of account balances or classes of transactions. Sampling is not used only in audit – is used in sampling surveys, market analysis and medical research in which someone wants to reach a conclusion about a large number of data by examining only a part of these data. The difference is the “population” from which the sample is selected, ie that set of data which is intended to draw a conclusion. Audit sampling applies only to certain types of audit procedures.

  3. Simultaneous determination of non-steroidal anti-inflammatory drugs and oestrogenic hormones in environmental solid samples.

    Science.gov (United States)

    Kumirska, Jolanta; Migowska, Natalia; Caban, Magda; Łukaszewicz, Paulina; Stepnowski, Piotr

    2015-03-01

    Pharmaceuticals are continually being released into the environment. Because of their physical and chemical properties, many of them or their bioactive metabolites can accumulate in sediments, sludge and soils, and induce adverse effects in terrestrial organisms. However, due to the very limited methods permitting the detection of these low-level concentration compounds in such complex matrices, their concentrations in natural solids remain largely unknown. In this paper, an analytical method for the simultaneous determination of thirteen pharmaceuticals (eight non-steroidal anti-inflammatory drugs and five oestrogenic hormones) in solid matrices was developed. The proposed MAE-SPE-GC-MS(SIM) method has been successfully validated providing a linear response over a concentration range of 1(17)-1000(1200)ng/g, depending on the pharmaceuticals, with correlation coefficients above 0.991. The method detection limits were in the range of 0.3-5.7 ng/g, absolute recoveries above 50%, except estrone. The developed method was applied in the analysis of the target compounds in sediment, sludge and soils collected in Poland giving primary data on their concentrations in such matrices in Poland. The obtained results confirmed that the proposed method can be successfully used in the analysis of real environmental solid samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Fluorescence spectrophotometer analysis of polycyclic aromatic hydrocarbons in environmental samples based on solid phase extraction using molecularly imprinted polymer.

    Science.gov (United States)

    Krupadam, Reddithota J; Bhagat, Bhagyashree; Wate, Satish R; Bodhe, Ghanshyam L; Sellergren, Borje; Anjaneyulu, Yerramilli

    2009-04-15

    A molecularly imprinted polymer (MIP) was synthesized using a polycyclic aromatic hydrocarbon (PAH) standard as a template, methacrylic acid as a functional monomer, ethylene glycol dimethacrylate as a cross-linker, and acetonitrile as a porogen. This polymer was used as a solid phase adsorbent for the quantitative enrichment of PAHs in coastal sediments, atmospheric particulates, and industrial effluents. The MIP selective adsorption capacity for PAHs started reducing when the chemical oxygen demand (COD) and total dissolved solids (TDS) was more than 800 mg L(-1) in the targeted environmental samples. The adsorption stability of the MIP was tested by the consecutive contact of environmental samples, and it was shown that the performance of the MIP did not vary after 10 enrichments and desorption cycles. Recoveries of eight PAH compounds, extracted from 10 g of coastal sediments and 1 L of industrial effluent spiked with 10 microL of standard PAHs, showed recoveries between 85 and 96%. The fluorescence spectrophotometer limit of detection of PAHs varied from 10 to 30 etag L(-1) in industrial effluent and from 0.1 to 2.9 etag kg(-1) in solid samples (coastal sediment and atmospheric particulates), and this indicates that the environmental analytical method is significantly sensitive, when compared with other commonly used methods such as gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry.

  5. Protein quantity on the air-solid interface determines degradation rates of human growth hormone in lyophilized samples.

    Science.gov (United States)

    Xu, Yemin; Grobelny, Pawel; Von Allmen, Alexander; Knudson, Korben; Pikal, Michael; Carpenter, John F; Randolph, Theodore W

    2014-05-01

    Recombinant human growth hormone (rhGH) was lyophilized with various glass-forming stabilizers, employing cycles that incorporated various freezing and annealing procedures to manipulate glass formation kinetics, associated relaxation processes, and glass-specific surface areas (SSAs). The secondary structure in the cake was monitored by infrared and in reconstituted samples by circular dichroism. The rhGH concentrations on the surface of lyophilized powders were determined from electron spectroscopy for chemical analysis. Glass transition temperature (Tg ), SSAs, and water contents were determined immediately after lyophilization. Lyophilized samples were incubated at 323 K for 16 weeks, and the resulting extents of rhGH aggregation, oxidation, and deamidation were determined after rehydration. Water contents and Tg were independent of lyophilization process parameters. Compared with samples lyophilized after rapid freezing, rhGH in samples that had been annealed in frozen solids prior to drying, or annealed in glassy solids after secondary drying retained more native-like protein secondary structure, had a smaller fraction of the protein on the surface of the cake, and exhibited lower levels of degradation during incubation. A simple kinetic model suggested that the differences in the extent of rhGH degradation during storage in the dried state between different formulations and processing methods could largely be ascribed to the associated levels of rhGH at the solid-air interface after lyophilization. © 2014 Wiley Periodicals, Inc. and the American Pharmacists Association.

  6. Protein Quantity on the Air-Solid Interface Determines Degradation Rates of Human Growth Hormone in Lyophilized Samples

    Science.gov (United States)

    Xu, Yemin; Grobelny, Pawel; von Allmen, Alexander; Knudson, Korben; Pikal, Michael; Carpenter, John F.; Randolph, Theodore W.

    2014-01-01

    rhGH was lyophilized with various glass-forming stabilizers, employing cycles that incorporated various freezing and annealing procedures to manipulate glass formation kinetics, associated relaxation processes and glass specific surface areas (SSA’s). The secondary structure in the cake was monitored by IR and in reconstituted samples by CD. The rhGH concentrations on the surface of lyophilized powders were determined from ESCA. Tg, SSA’s and water contents were determined immediately after lyophilization. Lyophilized samples were incubated at 323 K for 16 weeks, and the resulting extents of rhGH aggregation, oxidation and deamidation were determined after rehydration. Water contents and Tg were independent of lyophilization process parameters. Compared to samples lyophilized after rapid freezing, rhGH in samples that had been annealed in frozen solids prior to drying, or annealed in glassy solids after secondary drying retained more native-like protein secondary structure, had a smaller fraction of the protein on the surface of the cake and exhibited lower levels of degradation during incubation. A simple kinetic model suggested that the differences in the extent of rhGH degradation during storage in the dried state between different formulations and processing methods could largely be ascribed to the associated levels of rhGH at the solid-air interface after lyophilization. PMID:24623139

  7. Solid sampling determination of total fluorine in baby food samples by high-resolution continuum source graphite furnace molecular absorption spectrometry.

    Science.gov (United States)

    Ozbek, Nil; Akman, Suleyman

    2016-11-15

    This study describes the applicability of solid sampling technique for the determination of fluorine in various baby foods via molecular absorption of calcium monofluoride generated in a graphite furnace of high-resolution continuum source atomic absorption spectrometry. Fluorine was determined at CaF wavelength, 606.440nm in a graphite tube applying a pyrolysis temperature of 1000°C and a molecule forming temperature of 2200°C. The limit of detection and characteristic mass of the method were 0.20ng and 0.17ng of fluorine, respectively. The fluorine concentrations determined in standard reference sample (bush branches and leaves) were in good agreement with the certified values. By applying the optimized parameters, the concentration of fluorine in various baby foods were determined. The fluorine concentrations were ranged from sample amounts used in solid sampling analysis, micro-scale distribution of fluorine in the samples was also determined. Copyright © 2016 Elsevier Ltd. All rights reserved.

  8. Application of solid phase extraction procedures for rare earth elements determination in environmental samples.

    Science.gov (United States)

    Pyrzynska, Krystyna; Kubiak, Anna; Wysocka, Irena

    2016-07-01

    Determination of rare earth elements in environmental samples requires often pre-concentration and separation step due to a low metal content and high concentration of the interfering matrix components. A solid phase extraction technique with different kind of solid sorbents offers a high enrichment factor, rapid phase separation and the possibility of its combination with various detection techniques used either in on-line or off-line mode. The recent developments in this area published over the last five years are presented and discussed in this paper. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. Transmission vs. Diffuse Transmission in Circular Dichroism: What to Choose for Probing Solid-State Samples?

    Science.gov (United States)

    Górecki, Marcin

    2015-07-01

    Recent advances in equipment enabled the collection of solid-state electronic circular dichroism (ECD) spectra using the commercially available integrating sphere attachment for a regular ECD spectrometer. This accessory was designed to reduce negative factors occurring in solid-state ECD measurements, and is, thereby, very useful for recording diffuse transmittance CD (DTCD) spectra using the pellet technique. In the present article, the operating principle of the integrating sphere and utility of the DTCD method in recording solid-state ECD spectra is demonstrated. Based on illustrative examples, i.e., 10-camphorsulfonic acid ammonium, cholest-4-en-3-one, (3R,4R,5S)-oseltamivir, and (S)-linezolid, ECD solid-state measurements were performed by means of both transmission and diffusion methods and later compared. Selection of these compounds as models for comparative studies was made in view of their different chromophoric systems and the profound importance in the pharmaceutical industry. During the course of this work the benefits and limitations of the use of integrating sphere are presented. The final conclusion is that more relevant solid-state spectra can be obtained by means of the DTCD method. © 2015 Wiley Periodicals, Inc.

  10. Comparison of two methods for determination of tomato paste solids: vacuum oven versus microwave oven.

    Science.gov (United States)

    Jazaeri, Sahar; Kakuda, Yukio; Gismondi, Stephen; Wigle, Doug G

    2011-01-01

    Two analytical procedures used to determine total, soluble, and insoluble solids in tomato paste were evaluated. The microwave oven (MO) method was compared to the vacuum oven (VO) method. The VO method is tedious and measured the three solids fractions in the paste directly, while the MO method measured the total solids directly but used an equation to calculate the water-soluble and -insoluble solids. The MO method was faster and less labor-intensive, and yielded small but statistically significant higher values for total and insoluble solids and lower statistically significant values for soluble solids.

  11. Synthesis of nitrogen-doped graphene via solid microwave method

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Li, E-mail: zhangli379@sohu.com [School of Electrical Engineering, Dalian University of Technology, Dalian, Liaoning 116024 (China); Ji, Bingcheng, E-mail: debbo.jee@outlook.com [School of Electrical Engineering, Dalian University of Technology, Dalian, Liaoning 116024 (China); Wang, Kai [School of Electrical Engineering, Dalian University of Technology, Dalian, Liaoning 116024 (China); Song, Jinyan [School of Information Engineering, Dalian Ocean University, Dalian, Liaoning 116024 (China)

    2014-07-01

    Graphical abstract: - Highlights: • A direct solid microwave method is developed to prepare nitrogen-doped graphene. • The method consists of two steps, namely the functionalization and microwave irradiation. • Melamine can serve as not only functionalizing agent but also nitrogen source. - Abstract: In this paper, we propose a solid microwave-mediated method for scalable production of nitrogen-doped graphene sheets (NGS) using low-cost industrial material melamine as functionalizing agent and nitrogen source. The strong interaction of microwaves with graphene oxide has been fully utilized to generate in situ heating that induces the decompose melamine and nitrogen doping of graphene. The morphology, structure, and components of the as-produced nitrogen-doped graphene are characterized by scanning electron microscopy (SEM), transmission electron microscope (TEM), Brunauer–Emmett–Teller (BET), pore-size distribution (PSD), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectra (XPS), X-ray diffraction (XRD), and Raman spectroscopy. The results show NGS can be successfully synthesized via this strategy.

  12. Apparatus and method for determining solids circulation rate

    Science.gov (United States)

    Ludlow, J Christopher [Morgantown, WV; Spenik, James L [Morgantown, WV

    2012-02-14

    The invention relates to a method of determining bed velocity and solids circulation rate in a standpipe experiencing a moving packed bed flow, such as the in the standpipe section of a circulating bed fluidized reactor The method utilizes in-situ measurement of differential pressure over known axial lengths of the standpipe in conjunction with in-situ gas velocity measurement for a novel application of Ergun equations allowing determination of standpipe void fraction and moving packed bed velocity. The method takes advantage of the moving packed bed property of constant void fraction in order to integrate measured parameters into simultaneous solution of Ergun-based equations and conservation of mass equations across multiple sections of the standpipe.

  13. Intraurban Analysis of Domestic Solid Waste Disposal Methods in a Sub-Sahara African City

    Directory of Open Access Journals (Sweden)

    Oluwole Samuel Ojewale

    2014-01-01

    Full Text Available The study examined the influence of socioeconomic attributes of residents on domestic solid waste disposal methods in Lagos metropolis, Nigeria. Primary data for the study were obtained through questionnaire administered on residents in Eti-Osa, Ikeja, and Mushin Local Government Areas (LGAs representing the low, medium, and high densities, respectively, into which the sixteen LGAs in Lagos metropolis were stratified. One out of every four wards in each LGA was selected for survey. From a total of 15,275 residential buildings in the ten wards, one out of every forty buildings (2.5% was selected using systematic random sampling where a household head was sampled. Information obtained includes the residential characteristics and the disposal methods. Enquiries into the socioeconomic attributes of the residents showed that 59.9% were high income earners and 76.6% had attained tertiary school education. This study concluded that six disposal methods were common in the study area. Furthermore, through multinomial logistic regression, the influence of socioeconomic characteristics of residents (density, income, age of respondents, educational status, and length of stay on domestic solid waste disposal methods varied significantly in Lagos metropolis. The study established that most of the solid waste disposal methods utilized by residents in Lagos metropolis were not environment-friendly.

  14. System and method for extracting a sample from a surface

    Science.gov (United States)

    Van Berkel, Gary; Covey, Thomas

    2015-06-23

    A system and method is disclosed for extracting a sample from a sample surface. A sample is provided and a sample surface receives the sample which is deposited on the sample surface. A hydrophobic material is applied to the sample surface, and one or more devices are configured to dispense a liquid on the sample, the liquid dissolving the sample to form a dissolved sample material, and the one or more devices are configured to extract the dissolved sample material from the sample surface.

  15. Polychromatic solid-state lamps versus tungsten radiator: hue changes of Munsell samples

    Science.gov (United States)

    Stanikunas, R.; Vaitkevicius, H.; Svegzda, A.; Viliunas, V.; Bliznikas, Z.; Breive, K.; Vaicekauskas, R.; Novickovas, A.; Kurilcik, G.; Zukauskas, A.; Gaska, R.; Shur, M. S.

    2005-09-01

    Colour-perception differences under illumination by two quadrichromatic solid-state sources of light have been studied with respect to a tungsten radiator with the same correlated colour temperature (2600 K). A virtual RYgCB source (illuminant), which contains red, yellow-green, cyan and blue components with the line width typical of AlGaInP and AlInGaN light-emitting diodes (LEDs), was fully optimized for the highest value of the general colour-rendering index (CRI) (Ra = 98.3). An implemented RAGB source (lamp) contained commercially available red, amber, green and blue LEDs (Ra = 79.4). Colorimetric calculations in the Commission Internationale de l'Eclairage 1976 (u',v') colour plane for 40 Munsell colour samples (value 6, chroma/6, hue increment 2.5) revealed the differences in hue discrimination and distortion for both sources in the yellow-green and blue-cyan ranges. These differences were not revealed by the standard analysis of the special CRIs and were lower for the RYgCB illuminant, which contained primary LEDs in the sensitive ranges. A psychophysical experiment on seven subjects was performed using the RAGB lamp stabilized against thermal and ageing drifts. Despite different colour-perception abilities of the subjects under investigation, the experiment confirmed the calculation results. Methods of obtaining composite white light with high subjective ratings are discussed, based on the obtained data.

  16. Perpendicular distance sampling: an alternative method for sampling downed coarse woody debris

    Science.gov (United States)

    Michael S. Williams; Jeffrey H. Gove

    2003-01-01

    Coarse woody debris (CWD) plays an important role in many forest ecosystem processes. In recent years, a number of new methods have been proposed to sample CWD. These methods select individual logs into the sample using some form of unequal probability sampling. One concern with most of these methods is the difficulty in estimating the volume of each log. A new method...

  17. Modern methods of sample preparation for GC analysis

    NARCIS (Netherlands)

    de Koning, S.; Janssen, H.-G.; Brinkman, U.A.Th.

    2009-01-01

    Today, a wide variety of techniques is available for the preparation of (semi-) solid, liquid and gaseous samples, prior to their instrumental analysis by means of capillary gas chromatography (GC) or, increasingly, comprehensive two-dimensional GC (GC × GC). In the past two decades, a large number

  18. Measurement of Drinking Water Contaminants by Solid Phase Microextraction (SPME) Initially Quantified in Source Water Samples by the USGS

    Science.gov (United States)

    Stiles, Robert; Yang, Ill; Lippincott, Robert Lee; Murphy, Eileen; Buckley, Brian

    2014-01-01

    Two adsorbent solid phase microextraction (SPME) fibers, 70 μm Carbowax divinylbenzene (CW/DVB) and 65 μm polydimethylsiloxane divinylbenzene (PDMS/DVB), were selected for the analysis of several target analytes (phenols, phosphates, phthalates, polycyclic aromatic hydrocarbons (PAHs) and chlorinated pesticides) identified by the USGS in surface waters. Detection limits for standards ranged from 0.1 to 1 ng/mL for the CW/DVB fiber and 0.1 to 2 ng/mL for the PDMS/DVB fiber for twenty of the analytes. The remaining analytes were not extracted because their polarity precluded their partition to the solid phase of the SPME fiber. Groundwater and treated water samples collected from wells in Northern New Jersey were then sampled for the USGS analytes by the SPME method as well as a modified version of EPA 525.5 using C-18 bonded solid phase extraction (SPE) columns. Nine of the USGS analytes - bisphenol A, bis (2-ethylhexyl) phthalate, butylated hydroxytoluene, butlyated hydroxyanisole, diethyltoulamide, diethyl phthalate, bis (2-ethylhexyl) adipate, 1,4-dichlorobenzene and triphenyl phosphate - were detected in ground water samples using the CW/DVB fiber. PMID:18497153

  19. Measuring Sulfur Isotope Ratios from Solid Samples with the Sample Analysis at Mars Instrument and the Effects of Dead Time Corrections

    Science.gov (United States)

    Franz, H. B.; Mahaffy, P. R.; Kasprzak, W.; Lyness, E.; Raaen, E.

    2011-01-01

    The Sample Analysis at Mars (SAM) instrument suite comprises the largest science payload on the Mars Science Laboratory (MSL) "Curiosity" rover. SAM will perform chemical and isotopic analysis of volatile compounds from atmospheric and solid samples to address questions pertaining to habitability and geochemical processes on Mars. Sulfur is a key element of interest in this regard, as sulfur compounds have been detected on the Martian surface by both in situ and remote sensing techniques. Their chemical and isotopic composition can belp constrain environmental conditions and mechanisms at the time of formation. A previous study examined the capability of the SAM quadrupole mass spectrometer (QMS) to determine sulfur isotope ratios of SO2 gas from a statistical perspective. Here we discuss the development of a method for determining sulfur isotope ratios with the QMS by sampling SO2 generated from heating of solid sulfate samples in SAM's pyrolysis oven. This analysis, which was performed with the SAM breadboard system, also required development of a novel treatment of the QMS dead time to accommodate the characteristics of an aging detector.

  20. Appropriate maximum holding times for analysis of total suspended solids concentration in water samples taken from open-channel waterways.

    Science.gov (United States)

    Oudyn, Frederik W; Lyons, David J; Pringle, M J

    2012-01-01

    Many scientific laboratories follow, as standard practice, a relatively short maximum holding time (within 7 days) for the analysis of total suspended solids (TSS) in environmental water samples. In this study we have subsampled from bulk water samples stored at ∼4 °C in the dark, then analysed for TSS at time intervals up to 105 days after collection. The nonsignificant differences in TSS results observed over time demonstrates that storage at ∼4 °C in the dark is an effective method of preserving samples for TSS analysis, far past the 7-day standard practice. Extending the maximum holding time will ease the pressure on sample collectors and laboratory staff who until now have had to determine TSS within an impractically short period.

  1. Development of immunoaffinity solid phase microextraction rods for analysis of three estrogens in environmental water samples.

    Science.gov (United States)

    Wang, Cuicui; Yang, Linyan; Li, Na; Zhang, Xinda; Guo, Yongze; Li, Cun

    2017-09-01

    In this study, immunoaffinity solid phase microextraction (SPME) rods were developed for the analysis of diethylstilbestrol (DES), hexestrol (HES) and dienestrol (DIS) followed by ultra high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). This immunoaffinity SPME device was built with three stainless steel rods bundled together as one and modified with porous silicate particles. As an extraction sorbent, antibody immobilization approach was employed based on the covalent attachment of the anti-diethylstilbestrol monoclonal antibody (mAb) onto the rods. The immunoaffinity SPME rod was characterized and confirmed by scanning electron microscopy and X-ray photoelectron spectroscopy analysis. The porous network showed a very large active surface area and significantly increased the adsorption capacity which can reach 49.6pmol/cm(2). Moreover, the immunoaffinity sorbent showed good sturdiness at least 10 times with stable extraction performance. Once the main experimental parameters were optimized, the method was used to detect DES, HES and DIS in environmental water samples. The limits of detection for the three estrogens were 0.05-0.15ng/mL, and the limits of quantification was 0.5ng/mL. The average recoveries ranged from 34.2 to 62.7% were achieved with good intra-day and inter-day precision ranging from 7.8 to 12.7% and from 8.2 to 13.5% respectively. The newly developed immunoaffinity SPME showed high adsorption capacity, good sensitivity and reproducibility and was successfully applied to the analysis of DES, HES and DIS in environmental water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Nondestructive characterization methods for monolithic solid oxide fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Ellingson, W.A.

    1993-01-01

    Monolithic solid oxide fuel cells (MSOFCS) represent a potential breakthrough in fuel cell technology, provided that reliable fabrication methods can be developed. Fabrication difficulties arise in several steps of the processing: First is the fabrication of uniform thin (305 {mu}m) single-layer and trilayer green tapes (the trilayer tapes of anode/electrolyte/cathode and anode/interconnect/cathode must have similar coefficients of thermal expansion to sinter uniformly and to have the necessary electrochemical properties); Second is the development of fuel and oxidant channels in which residual stresses are likely to develop in the tapes; Third is the fabrication of a ``complete`` cell for which the bond quality between layers and the quality of the trilayers must be established; and Last, attachment of fuel and oxidant manifolds and verification of seal integrity. Purpose of this report is to assess nondestructive characterization methods that could be developed for application to laboratory, prototype, and full-scale MSOFCs.

  3. ALTERNATIVE METHODS OF SEALING PLANAR SOLID OXIDE FUEL CELLS

    Energy Technology Data Exchange (ETDEWEB)

    Weil, K. Scott; Coyle, Christopher A.; Hardy, John S.; Kim, Jin Yong Y.; Xia, Gordon

    2005-03-01

    One of the key limiting issues in designing and fabricating a high performance planar solid oxide fuel cell (pSOFC) stack is the development of the appropriate materials and techniques for hermetically sealing the metal and ceramic components. There are essentially two standard methods of sealing: (1) by forming a rigid joint or (2) by constructing a compressive “sliding” seal. While short-term success has been achieved with both techniques, it is apparent that to meet the long-term operational needs of stack designers, alternative sealing concepts will need to be conceived. Described below are two alternative pSOFC sealing methods that have been developed at Pacific Northwest National Laboratory.

  4. Municipal solid waste composition: Sampling methodology, statistical analyses, and case study evaluation

    DEFF Research Database (Denmark)

    Edjabou, Vincent Maklawe Essonanawe; Jensen, Morten Bang; Götze, Ramona

    2015-01-01

    stratification parameter. Separating food leftovers from food packaging during manual sorting of the sampled waste did not have significant influence on the proportions of food waste and packaging materials, indicating that this step may not be required. (C) 2014 Elsevier Ltd. All rights reserved.......Sound waste management and optimisation of resource recovery require reliable data on solid waste generation and composition. In the absence of standardised and commonly accepted waste characterisation methodologies, various approaches have been reported in literature. This limits both...... comparability and applicability of the results. In this study, a waste sampling and sorting methodology for efficient and statistically robust characterisation of solid waste was introduced. The methodology was applied to residual waste collected from 1442 households distributed among 10 individual sub...

  5. Comparison of methods for solids retention time determination and control

    Science.gov (United States)

    Balbierz, Piotr; Knap, Marta

    2017-11-01

    Solids retention time (SRT) is the basic and most important process parameter in design, operation and control of activated sludge (AS) systems, especially with nitrification and biological nutrient removal. However, determination of SRT at the full-scale wastewater treatment plant (WWTP) may not be straightforward and the significance of proper SRT control is often underestimated by plant operators, which may lead to severe operational problems, including complete nitrification failure. This paper presents different methods for SRT determination and control, including simple hydraulic method and phosphorous mass balance method. The comparison is based on an extended data set from a large WWTP in south-west Poland, both in stable and transient operational conditions. The results of the comparison show that during stable operational conditions, all the SRT determination methods give similar results, thus the simple hydraulic method can be applied during standard operation, even at small WWTPs, which lack laboratory facilities. Hydraulic method is based on continuous on-line flowrate measurements, therefore it gives opportunity to implement an algorithm to automatically control SRT and sludge wastage from the system.

  6. Molecularly Imprinted Polymers (MIP for Selective Solid Phase Extraction of Celecoxib in Urine Samples Followed by High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Saeedeh Ansari

    2017-09-01

    Full Text Available In this study, for the analysis of human urine samples, a novel method explained for the determination of celecoxib, a nonsteroidal anti-inflammatory drug (NSAID, using molecularly imprinted solid-phase extraction (MISPE coupled with high-performance liquid chromatography (HPLC. The synthesis of the MIP was performed by precipitation polymerization in methacrylic acid (MAA, ethylene glycol dimethacrylate (EGDMA, chloroform, 2,2′-azobisisobutyronitrile (AIBN and celecoxib as the functional monomer, cross-linker monomer, solvent, initiator and target drug, respectively. The celecoxib imprinted polymer was utilized as a specific sorbent for the solid phase extraction (SPE of celecoxib from samples. The molecularly imprinted polymer (MIP performance was compared with the synthesized non-molecularly imprinted polymer (NIP. Scanning electron microscopy (SEM, FT-IR spectroscopy, UV-VIS spectrophotometry and thermogravimetric analysis (TGA/DTG were used for characterizing the synthesized polymers. Moreover, the MISPE procedure parameters such as pH, eluent solvent flow rate, eluent volume and sorbent mass that probably influence the extraction process have been optimized to achieve the highest celecoxib extraction efficiency. The relative standard deviation (RSD %, recovery percent, limit of detection (LOD and limit of quantification (LOQ of this proposed method were 1.12%, 96%, 8 µg L-1 and 26.7 µg L-1, respectively. The proposed MISPE-HPLC-UV method can be used for the separation and enrichment of trace amounts of celecoxib in human urine and biological samples.

  7. Photochemistry of solid interstellar molecular samples exposed to vacuum-ultraviolet synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Lo, Jen-Iu; Chou, Sheng-Lung; Peng, Yu-Chain; Lin, Meng-Yeh; Lu, Hsiao-Chi; Cheng, Bing-Ming, E-mail: bmcheng@nsrrc.org.tw

    2014-10-15

    Highlights: • By means of an end station attached to synchrotron, we investigate the VUV photolysis of gaseous samples condensed at 3 K. • The end station is applicable to explore the VUV photochemistry of interstellar solid molecules. • We upgraded the end station with detection of absorption of IR light and of emission of UV–vis light. • As a demonstration, we recorded simultaneously absorption spectra of photoproduct N{sub 3} and emission from VUV excited N{sub 2}. • The end station is applicable to investigate cometary mixed-ice analogs excited with VUV light from the synchrotron. - Abstract: At the vacuum-ultraviolet (VUV) beamline of the Taiwan synchrotron, an end station for photochemistry coupled to instruments to record infrared absorption spectra and ultraviolet and visible emission spectra is used to investigate the photolysis of samples of gases condensed at 3 K. This end station is applicable to explore the VUV photochemistry of interstellar molecules in solid samples. For demonstration, we discuss the response of solid dinitrogen to VUV irradiation. In the future, the upgraded photochemistry end station is applicable to investigate the cometary mixed-ice analogs excited with VUV light from the synchrotron.

  8. Graphene-Based Materials as Solid Phase Extraction Sorbent for Trace Metal Ions, Organic Compounds, and Biological Sample Preparation.

    Science.gov (United States)

    Ibrahim, Wan Aini Wan; Nodeh, Hamid Rashidi; Sanagi, Mohd Marsin

    2016-07-03

    Graphene is a new carbon-based material that is of interest in separation science. Graphene has extraordinary properties including nano size, high surface area, thermal and chemical stability, and excellent adsorption affinity to pollutants. Its adsorption mechanisms are through non-covalent interactions (π-π stacking, electrostatic interactions, and H-bonding) for organic compounds and covalent interactions for metal ions. These properties have led to graphene-based material becoming a desirable adsorbent in a popular sample preparation technique known as solid phase extraction (SPE). Numerous studies have been published on graphene applications in recent years, but few review papers have focused on its applications in analytical chemistry. This article focuses on recent preconcentration of trace elements, organic compounds, and biological species using SPE-based graphene, graphene oxide, and their modified forms. Solid phase microextraction and micro SPE (µSPE) methods based on graphene are discussed.

  9. SOLID PHASE CHARACTERIZATION OF HEEL SAMPLES FROM TANK 241-C-110

    Energy Technology Data Exchange (ETDEWEB)

    PAGE JS; COOKE GA; PESTOVICH JA; HUBER HJ

    2011-12-01

    During sluicing operations of tank 241-C-110, a significant amount of solids were unable to be retrieved. These solids (often referred to as the tank 'heel') were sampled in 2010 and chemically and mineralogically analyzed in the 222-S Laboratory. Additionally, dissolution tests were performed to identify the amount of undissolvable material after using multiple water contacts. This report covers the solid phase characterization of six samples from these tests using scanning electron microscopy, polarized light microscopy, and X-ray diffraction. The chemical analyses, particle size distribution analysis, and dissolution test results are reported separately. Two of the samples were from composites created from as-received material - Composite A and Composite B. The main phase in these samples was sodium-fluoride-phosphate hydrate (natrophosphate) - in the X-ray diffraction spectra, this phase was the only phase identifiable. Polarized light microscopy showed the presence of minor amounts of gibbsite and other phases. These phases were identified by scanning electron microscopy - energy dispersive X-ray spectroscopy as sodium aluminosilicates, sodium diuranate, and sodium strontium phosphate hydrate (nastrophite) crystals. The natrophosphate crystals in the scanning electron microscopy analysis showed a variety of erosive and dissolution features from perfectly shaped octahedral to well-rounded appearance. Two samples were from water-washed Composites A and B, with no change in mineralogy compared to the as-received samples. This is not surprising, since the water wash had only a short period of water contact with the material as opposed to the water dissolution tests. The last two samples were residual solids from the water dissolution tests. These tests included multiple additions of water at 15 C and 45 C. The samples were sieved to separate a coarser fraction of > 710 {mu}m and a finer fraction of < 710 {mu}m. These two fractions were analyzed

  10. Solid phase extraction of Cd, Pb, Ni, Cu, and Zn in environmental samples on multiwalled carbon nanotubes.

    Science.gov (United States)

    Yilmaz, Erkan; Soylak, Mustafa

    2014-09-01

    A simple and sensitive solid phase extraction (SPE) method on multiwalled carbon nanotubes (MWCNTs) is presented for the determination of cadmium, lead, nickel, copper, and zinc at trace levels combined with flame atomic absorption spectrometry. The effects of parameters like pH, sample volume, sample and eluent flow rates, eluent concentration, and volume and type of eluent on the recovery of trace elements was examined. The metals retained on the nanotube at pH 6.5 as α-benzoin oxime complexes were eluted by 10 mL 2 M HNO3 in acetone. The influence of matrix ions on the developed method was also evaluated. The preconcentration factor of the method was found to be 50. The detection limits for Cd(II), Pb(II), Ni(II), Cu(II), and Zn(II) were found as 1.7, 5.5, 6.0, 2.3, and 2.4 μg L(-1), respectively. To test the accuracy of the method, the method was applied to TMDA-70 fortified lake water and Spinach 1570A standard reference materials. Addition recovery studies were applied to tap water and cracked wheat samples, and determination of the analyte elements was carried out in some food samples with good results.

  11. Solid-Phase Extraction Strategies to Surmount Body Fluid Sample Complexity in High-Throughput Mass Spectrometry-Based Proteomics

    Directory of Open Access Journals (Sweden)

    Marco R. Bladergroen

    2015-01-01

    Full Text Available For large-scale and standardized applications in mass spectrometry- (MS- based proteomics automation of each step is essential. Here we present high-throughput sample preparation solutions for balancing the speed of current MS-acquisitions and the time needed for analytical workup of body fluids. The discussed workflows reduce body fluid sample complexity and apply for both bottom-up proteomics experiments and top-down protein characterization approaches. Various sample preparation methods that involve solid-phase extraction (SPE including affinity enrichment strategies have been automated. Obtained peptide and protein fractions can be mass analyzed by direct infusion into an electrospray ionization (ESI source or by means of matrix-assisted laser desorption ionization (MALDI without further need of time-consuming liquid chromatography (LC separations.

  12. Novel Electrosorption-Enhanced Solid-Phase Microextraction Device for Ultrafast In Vivo Sampling of Ionized Pharmaceuticals in Fish.

    Science.gov (United States)

    Qiu, Junlang; Wang, Fuxin; Zhang, Tianlang; Chen, Le; Liu, Yuan; Zhu, Fang; Ouyang, Gangfeng

    2017-12-13

    Decreasing the tedious sample preparation duration is one of the most important concerns for the environmental analytical chemistry especially for in vivo experiments. However, due to the slow mass diffusion paths for most of the conventional methods, ultrafast in vivo sampling remains challenging. Herein, for the first time, we report an ultrafast in vivo solid-phase microextraction (SPME) device based on electrosorption enhancement and a novel custom-made CNT@PPY@pNE fiber for in vivo sampling of ionized acidic pharmaceuticals in fish. This sampling device exhibited an excellent robustness, reproducibility, matrix effect-resistant capacity, and quantitative ability. Importantly, the extraction kinetics of the targeted ionized pharmaceuticals were significantly accelerated using the device, which significantly improved the sensitivity of the SPME in vivo sampling method (limits of detection ranged from 0.12 ng·g-1 to 0.25 ng·g-1) and shorten the sampling time (only 1 min). The proposed approach was successfully applied to monitor the concentrations of ionized pharmaceuticals in living fish, which demonstrated that the device and fiber were suitable for ultrafast in vivo sampling and continuous monitoring. In addition, the bioconcentration factor (BCF) values of the pharmaceuticals were derived in tilapia (Oreochromis mossambicus) for the first time, based on the data of ultrafast in vivo sampling. Therefore, we developed and validated an effective and ultrafast SPME sampling device for in vivo sampling of ionized analytes in living organisms and this state-of-the-art method provides an alternative technique for future in vivo studies.

  13. Some connections between importance sampling and enhanced sampling methods in molecular dynamics

    Science.gov (United States)

    Lie, H. C.; Quer, J.

    2017-11-01

    In molecular dynamics, enhanced sampling methods enable the collection of better statistics of rare events from a reference or target distribution. We show that a large class of these methods is based on the idea of importance sampling from mathematical statistics. We illustrate this connection by comparing the Hartmann-Schütte method for rare event simulation (J. Stat. Mech. Theor. Exp. 2012, P11004) and the Valsson-Parrinello method of variationally enhanced sampling [Phys. Rev. Lett. 113, 090601 (2014)]. We use this connection in order to discuss how recent results from the Monte Carlo methods literature can guide the development of enhanced sampling methods.

  14. Evaluation of solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for direct determination of chromium in medicinal plants

    Energy Technology Data Exchange (ETDEWEB)

    Virgilio, Alex; Nobrega, Joaquim A. [Department of Chemistry, Federal University of Sao Carlos, Post Office Box 676, 13560-970, Sao Carlos-SP (Brazil); Rego, Jardes F. [Department of Analytical Chemistry, Institute of Chemistry, Sao Paulo State University-UNESP, Post Office Box 355, 14801-970, Araraquara-SP (Brazil); Neto, Jose A. Gomes, E-mail: anchieta@iq.unesp.br [Department of Analytical Chemistry, Institute of Chemistry, Sao Paulo State University-UNESP, Post Office Box 355, 14801-970, Araraquara-SP (Brazil)

    2012-12-01

    A method for Cr determination in medicinal plants using direct solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry was developed. Modifiers were dispensable. Pyrolysis and atomization temperatures were 1500 Degree-Sign C and 2400 Degree-Sign C, respectively. Slopes of calibration curves (50-750 pg Cr, R{sup 2} > 0.999) using aqueous and solid standards coincides in 96%, indicated feasibility of aqueous calibration for solid sampling of medicinal plants. Accuracy was checked by analysis of four plant certified reference materials. Results were in agreement at 95% confidence level with certified and non-certified values. Ten samples of medicinal plants were analyzed and Cr contents were in the 1.3-17.7 {mu}g g{sup -1} Cr range. The highest RSD (n = 5) was 15.4% for the sample Melissa officinalis containing 13.9 {+-} 2.1 {mu}g g{sup -1} Cr. The limit of detection was 3.3 ng g{sup -1} Cr. - Highlights: Black-Right-Pointing-Pointer Direct solid sampling is first time employed for Cr in plant materials. Black-Right-Pointing-Pointer Calibration curves with liquids and solids are coincident. Black-Right-Pointing-Pointer Microanalysis of plants for Cr is validated by reference materials. Black-Right-Pointing-Pointer The proposed HR-CS GF AAS method is environmental friendly.

  15. Rapid determination of trace level copper in tea infusion samples by solid contact ion selective electrode

    Directory of Open Access Journals (Sweden)

    Aysenur Birinci

    2016-07-01

    Full Text Available A new solid contact copper selective electrode with a poly (vinyl chloride (PVC membrane consisting of o-xylylenebis(N,N-diisobutyldithiocarbamate as ionophore has been prepared. The main novelties of constructed ion selective electrode concept are the enhanced robustness, cheapness, and fastness due to the use of solid contacts. The electrode exhibits a rapid (< 10 seconds and near-Nernstian response to Cu2+ activity from 10−1 to 10−6 mol/L at the pH range of 4.0–6.0. No serious interference from common ions was found. The electrode characterizes by high potential stability, reproducibility, and full repeatability. The electrode was used as an indicator electrode in potentiometric titration of Cu(II ions with EDTA and for the direct assay of tea infusion samples by means of the calibration graph technique. The results compared favorably with those obtained by the atomic absorption spectroscopy (AAS.

  16. 19 CFR 151.83 - Method of sampling.

    Science.gov (United States)

    2010-04-01

    ... 19 Customs Duties 2 2010-04-01 2010-04-01 false Method of sampling. 151.83 Section 151.83 Customs Duties U.S. CUSTOMS AND BORDER PROTECTION, DEPARTMENT OF HOMELAND SECURITY; DEPARTMENT OF THE TREASURY (CONTINUED) EXAMINATION, SAMPLING, AND TESTING OF MERCHANDISE Cotton § 151.83 Method of sampling. For...

  17. 7 CFR 29.110 - Method of sampling.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 2 2010-01-01 2010-01-01 false Method of sampling. 29.110 Section 29.110 Agriculture Regulations of the Department of Agriculture AGRICULTURAL MARKETING SERVICE (Standards, Inspections, Marketing... INSPECTION Regulations Inspectors, Samplers, and Weighers § 29.110 Method of sampling. In sampling tobacco...

  18. an assessment of methods for sampling carabid beetles

    African Journals Online (AJOL)

    Mgina

    particular habitat where we sampled (rugged montane rain forest) pitfall trapping has no advantage over searching methods with respect to ease of operation, low cost or efficiency. However, despite its inefficiency, pitfall trapping cannot be left out of sampling protocols because the method sampled some species that were ...

  19. Sampling Methods in Cardiovascular Nursing Research: An Overview.

    Science.gov (United States)

    Kandola, Damanpreet; Banner, Davina; O'Keefe-McCarthy, Sheila; Jassal, Debbie

    2014-01-01

    Cardiovascular nursing research covers a wide array of topics from health services to psychosocial patient experiences. The selection of specific participant samples is an important part of the research design and process. The sampling strategy employed is of utmost importance to ensure that a representative sample of participants is chosen. There are two main categories of sampling methods: probability and non-probability. Probability sampling is the random selection of elements from the population, where each element of the population has an equal and independent chance of being included in the sample. There are five main types of probability sampling including simple random sampling, systematic sampling, stratified sampling, cluster sampling, and multi-stage sampling. Non-probability sampling methods are those in which elements are chosen through non-random methods for inclusion into the research study and include convenience sampling, purposive sampling, and snowball sampling. Each approach offers distinct advantages and disadvantages and must be considered critically. In this research column, we provide an introduction to these key sampling techniques and draw on examples from the cardiovascular research. Understanding the differences in sampling techniques may aid nurses in effective appraisal of research literature and provide a reference pointfor nurses who engage in cardiovascular research.

  20. Investigating the solid-liquid phase transition of water nanofilms using the generalized replica exchange method

    Science.gov (United States)

    Lu, Qing; Kim, Jaegil; Farrell, James D.; Wales, David J.; Straub, John E.

    2014-11-01

    The generalized Replica Exchange Method (gREM) was applied to study a solid-liquid phase transition in a nanoconfined bilayer water system using the monatomic water (mW) model. Exploiting optimally designed non-Boltzmann sampling weights with replica exchanges, gREM enables an effective sampling of configurations that are metastable or unstable in the canonical ensemble via successive unimodal energy distributions across phase transition regions, often characterized by S-loop or backbending in the statistical temperature. Extensive gREM simulations combined with Statistical Temperature Weighted Histogram Analysis Method (ST-WHAM) for nanoconfined mW water at various densities provide a comprehensive characterization of diverse thermodynamic and structural properties intrinsic to phase transitions. Graph representation of minimized structures of bilayer water systems determined by the basin-hopping global optimization revealed heterogeneous ice structures composed of pentagons, hexagons, and heptagons, consistent with an increasingly ordered solid phase with decreasing density. Apparent crossover from a first-order solid-liquid transition to a continuous one in nanoconfined mW water with increasing density of the system was observed in terms of a diminishing S-loop in the statistical temperature, smooth variation of internal energies and heat capacities, and a characteristic variation of lateral radial distribution functions, and transverse density profiles across transition regions.

  1. On Angular Sampling Methods for 3-D Spatial Channel Models

    DEFF Research Database (Denmark)

    Fan, Wei; Jämsä, Tommi; Nielsen, Jesper Ødum

    2015-01-01

    This paper discusses generating three dimensional (3D) spatial channel models with emphasis on the angular sampling methods. Three angular sampling methods, i.e. modified uniform power sampling, modified uniform angular sampling, and random pairing methods are proposed and investigated in detail....... The random pairing method, which uses only twenty sinusoids in the ray-based model for generating the channels, presents good results if the spatial channel cluster is with a small elevation angle spread. For spatial clusters with large elevation angle spreads, however, the random pairing method would fail...

  2. Method for removing hydrocarbon contaminants from solid materials

    Science.gov (United States)

    Bala, G.A.; Thomas, C.P.

    1995-10-03

    A system is described for removing hydrocarbons from solid materials. Contaminated solids are combined with a solvent (preferably terpene based) to produce a mixture. The mixture is washed with water to generate a purified solid product (which is removed from the system) and a drainage product. The drainage product is separated into a first fraction (consisting mostly of contaminated solvent) and a second fraction (containing solids and water). The first fraction is separated into a third fraction (consisting mostly of contaminated solvent) and a fourth fraction (containing residual solids and water). The fourth fraction is combined with the second fraction to produce a sludge which is separated into a fifth fraction (containing water which is ultimately reused) and a sixth fraction (containing solids). The third fraction is then separated into a seventh fraction (consisting of recovered solvent which is ultimately reused) and an eighth fraction (containing hydrocarbon waste). 4 figs.

  3. Headspace solid phase microextraction for screening for the presence of resins in Egyptian archaeological samples.

    Science.gov (United States)

    Hamm, Sandrine; Bleton, Jean; Tchapla, Alain

    2004-02-01

    The aim of this study was to use headspace solid phase microextraction (SPME) to reveal the presence of resin in archaeological samples, such as mummification balms, from ancient Egypt. Experiments were first performed with fresh resins of known origin. The SPME fibre readily extracted mono- and sesquiterpenes and, to a lesser extent, diterpenes. Using mass spectra and retention indices of constitutive compounds, qualitative analysis of the volatile fraction allowed us to differentiate resins or gum-resins such as myrrh, olibanum, galbanum, labdanum, mastic, and conifer resins. SPME was then successfully applied to archaeological samples from ancient Egypt in which the presence of resins was detected. Volatile components were desorbed and trapped according to the same SPME procedure as was applied to fresh resins, after a sample preparation consisting of a fine grinding.

  4. New adaptive sampling method in particle image velocimetry

    Science.gov (United States)

    Yu, Kaikai; Xu, Jinglei; Tang, Lan; Mo, Jianwei

    2015-03-01

    This study proposes a new adaptive method to enable the number of interrogation windows and their positions in a particle image velocimetry (PIV) image interrogation algorithm to become self-adapted according to the seeding density. The proposed method can relax the constraint of uniform sampling rate and uniform window size commonly adopted in the traditional PIV algorithm. In addition, the positions of the sampling points are redistributed on the basis of the spring force generated by the sampling points. The advantages include control of the number of interrogation windows according to the local seeding density and smoother distribution of sampling points. The reliability of the adaptive sampling method is illustrated by processing synthetic and experimental images. The synthetic example attests to the advantages of the sampling method. Compared with that of the uniform interrogation technique in the experimental application, the spatial resolution is locally enhanced when using the proposed sampling method.

  5. Determination of Atrazine, Acetochlor, Clomazone, Pendimethalin and Oxyfluorfen in Soil by a Solid Phase Microextraction Method

    Directory of Open Access Journals (Sweden)

    Rada Đurović

    2008-01-01

    Full Text Available A solid phase microextraction (SPME method for simultaneous determination of atrazine, acetochlor, clomazone, pendimethalin and oxyfluorfen in soil samples was developed. The method is based on a combination of conventional liquid-solid procedure and a following SPME determination of the selected pesticides. Initially, various microextraction conditions, such as the fibre type, desorption temperature and time, extraction time and NaCl content, were investigated and optimized. Then, extraction efficiencies of severalsolvents (water, hexane, acetonitrile, acetone and methanol and the optimum number of extraction steps within the sample preparation step were optimized. According to the results obtained in these two sets of experiments, two successive extractions with methanol as the extraction solvent were the optimal sample preparation procedure, while the following conditions were found to be most efficient for SPME measurements: 100 μm PDMS fibre, desorption for 7 min at 2700C, 30 min extraction time and 5% NaCl content (w/v. Detection and quantification were done by gas chromatography-mass spectrometry(GC/MS. Relative standard deviation (RSD values for multiple analysis of soil samples fortified at 30 μg/kg of each pesticide were below 19%. Limits of detection (LOD for all the compounds studied were less than 2 μg/kg.

  6. Spatio-temporal variability of solid, total dissolved and labile metal: passive vs. discrete sampling evaluation in river metal monitoring.

    Science.gov (United States)

    Priadi, Cindy; Bourgeault, Adeline; Ayrault, Sophie; Gourlay-Francé, Catherine; Tusseau-Vuillemin, Marie-Hélène; Bonté, Philippe; Mouchel, Jean-Marie

    2011-05-01

    In order to obtain representative dissolved and solid samples from the aquatic environment, a spectrum of sampling methods are available, each one with different advantages and drawbacks. This article evaluates the use of discrete sampling and time-integrated sampling in illustrating medium-term spatial and temporal variation. Discrete concentration index (CI) calculated as the ratio between dissolved and solid metal concentrations in grab samples are compared with time-integrated concentration index (CI) calculated from suspended particulate matter (SPM) collected in sediment traps and labile metals measured by the diffusive gel in thin films (DGT) method, collected once a month during one year at the Seine River, upstream and downstream of the Greater Paris Region. Discrete CI at Bougival was found to be significantly higher than at Triel for Co, Cu, Mn, Ni and Zn, while discrete metal partitioning at Marnay was found to be similar to Bougival and Triel. However, when using time-integrated CI, not only was Bougival CI significantly higher than Triel CI, CI at Marnay was also found to be significantly higher than CI at Triel which was not observed for discrete CI values. Since values are time-averaged, dramatic fluctuations were smoothed out and significant medium-term trends were enhanced. As a result, time-integrated concentration index (CI) was able to better illustrate urbanization impact between sites when compared to discrete CI. The impact of significant seasonal phenomenon such as winter flood, low flow and redox cycles was also, to a certain extent, visible in time-integrated CI values at the upstream site. The use of time-integrated concentration index may be useful for medium- to long-term metal studies in the aquatic environment.

  7. Graphene aerogel based monolith for effective solid-phase extraction of trace environmental pollutants from water samples.

    Science.gov (United States)

    Han, Qiang; Liang, Qionglin; Zhang, Xiaoqiong; Yang, Liu; Ding, Mingyu

    2016-05-20

    Graphene aerogel (GA), a typical kind of three-dimensional (3D) macroscopic assembly, not only provides inherently excellent properties of graphene sheets (GS), but also exhibits interesting characteristics of the 3D macroporous architecture including large and tunable pore volumes, high specific surface areas and fast mass transport kinetics. Thus, it is rational to expect GA to be an efficient adsorbent for solid-phase extraction (SPE). In this paper, a novel GA monolith based solid-phase extraction method was investigated in the application of environment analysis. The GA monolith based SPE cartridge was fabricated directly in the empty cartridge through template-free "sol-cryo" method. Due to the efficient mass transfer, more adsorption sites as well as effective retention for the analytes, the adsorption property of GA for bisphenol A revealed better performance than that of GS. What's more, GA also outperformed in loading and eluting for target analysis. On the basis of the above advantages, the obtained cartridge was applied for the separation of environmental pollutants from water samples. Taking endocrine disrupting chemicals and polychlorinated biphenyls as the polar and weak polar model analytes, optimizing several parameters influencing the recoveries, limits of detection in the range of 0.01-0.11ngmL(-1) and 0.19-1.53ngL(-1) for the two series of compounds were provided by the established methods. The satisfied sensitivity was accessed and recoveries ranging from 76.3 to 112.5% were obtained for all the analytes when the proposed methods were applied in real water samples analysis. The results revealed the potential of GA as an effective sorbent in sample preparation processes. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. A technique for the determination of 18O/16O and 17O/16O isotopic ratios in water from small liquid and solid samples.

    Science.gov (United States)

    Baker, L; Franchi, I A; Maynard, J; Wright, I P; Pillinger, C T

    2002-04-01

    We have developed a new technique in which a solid reagent, cobalt(III) fluoride, is used to prepare oxygen gas for isotope ratio measurement from water derived either from direct injection or from the pyrolysis of solid samples. The technique uses continuous flow, isotope ratio monitoring, gas chromatography/mass spectrometry (irmGC/MS) to measure the delta18O and delta17O of the oxygen gas. Water from appropriate samples is evolved by a procedure of stepped pyrolysis (0-1000 degrees C, typically in 50 degrees C increments) under a flowing stream of helium carrier gas. The method has considerable advantages over others used for water analysis in that it is quick; requires only small samples, typically 1-50 mg of whole rock samples (corresponding to approximately 0.2 micromol of H2O); and the reagent is easy and safe to handle. Reproducibility in isotope ratio measurement obtained from pyrolysis of samples of a terrestrial solid standard are delta18O +/- 0.54, delta17O +/- 0.33, and delta17O +/- 0.10/1000, 1sigma in all cases. The technique was developed primarily for the analysis of meteorites, and the efficiency of the method is illustrated herein by results from water standards, solid reference materials, and a sample of the Murchison CM2 meteorite.

  9. Simplifying Solid-Phase Extraction Method Development: Exploring the Use of Software

    National Research Council Canada - National Science Library

    Jeremy S Bierman; Michael V Campognone

    2009-01-01

      Solid-phase extraction (SPE) is a popular sample preparation technique, valued by analysts working with complex matrices for its ability to specifically select for target compounds, concentrate samples, and perform a solvent switch...

  10. Diffusion in Solids Fundamentals, Methods, Materials, Diffusion-Controlled Processes

    CERN Document Server

    Mehrer, Helmut

    2007-01-01

    Diffusion is a vital topic in solid-state physics and chemistry, physical metallurgy and materials science. Diffusion processes are ubiquitous in solids at elevated temperatures. A thorough understanding of diffusion in materials is crucial for materials development and engineering. This book first gives an account of the central aspects of diffusion in solids, for which the necessary background is a course in solid state physics. It then provides easy access to important information about diffuson in metals, alloys, semiconductors, ion-conducting materials, glasses and nanomaterials. Several diffusion-controlled phenomena, including ionic conduction, grain-boundary and dislocation pipe diffusion, are considered as well. Graduate students in solid-state physics, physical metallurgy, materials science, physical and inorganic chemistry or geophysics will benefit from this book as will physicists, chemists, metallurgists, materials engineers in academic and industrial research laboratories.

  11. Systems and methods for self-synchronized digital sampling

    Science.gov (United States)

    Samson, Jr., John R. (Inventor)

    2008-01-01

    Systems and methods for self-synchronized data sampling are provided. In one embodiment, a system for capturing synchronous data samples is provided. The system includes an analog to digital converter adapted to capture signals from one or more sensors and convert the signals into a stream of digital data samples at a sampling frequency determined by a sampling control signal; and a synchronizer coupled to the analog to digital converter and adapted to receive a rotational frequency signal from a rotating machine, wherein the synchronizer is further adapted to generate the sampling control signal, and wherein the sampling control signal is based on the rotational frequency signal.

  12. Mechanism to remove oxide inclusions from molten aluminum by solid fluxes refining method

    Directory of Open Access Journals (Sweden)

    Cong Li

    2017-07-01

    Full Text Available A novel flux charging method and a crucible quenching method were employed to study the mechanism of solid fluxes refining method regarding the removal of oxide inclusions (Al2O3 from molten aluminum. Electrochemical polishing method was adopted to prepare surfaces of the samples. Through experiments, the morphology of the residual solidified flux in the solidified samples as well as the wetting action of the molten flux during refining were observed for the first time. Three wetting regimes denoted by absorbing regime, engulfing regime and penetration regime correlating with the removal of oxide films (the most typical and common oxide inclusions in molten aluminum were proposed in terms of different types and distributions of oxide films and different size ratios of the molten flux to oxide films. Particularly, from a thermodynamic point of view, for the first time, the penetration regime provided concrete evidence that the practical oxide inclusions can be wet by molten flux under ambient fluid of molten aluminum. A spreading model was proposed, according to which ingredients and size parameters of practical solid fluxes can be optimized.

  13. Analysis of volatiles in dehydrated carrot samples by solid-phase microextraction followed by GC-MS.

    Science.gov (United States)

    Soria, Ana Cristina; Sanz, Jesús; Villamiel, Mar

    2008-10-01

    A solid-phase microextraction (SPME)-based method for the GC-MS analysis of volatiles in dehydrated carrot root samples has been developed and the effect of the most important factors (fibre coating, extraction temperature, equilibrium time and extraction time) on the fractionation of different volatiles has been studied. GC-MS chromatograms showed terpenoids relevant to carrot aroma such as alpha-pinene, sabinene, beta-myrcene, limonene, gamma-terpinene, terpinolene, trans-caryophyllene and beta-bisabolene, and several furan derivatives whose origin is discussed in this paper. As an example of application, this methodology has been used for the characterization of volatile composition of industrially dehydrated carrots. SPME followed by GC-MS is shown as an affordable, fast and solvent-free technique which can be performed with low sample amounts and be easily implemented at an industry for quality control purposes.

  14. Dynamic solid phase microextraction for sampling of airborne sarin with gas chromatography-mass spectrometry for rapid field detection and quantification.

    Science.gov (United States)

    Hook, Gary L; Jackson Lepage, Carmela; Miller, Stephen I; Smith, Philip A

    2004-08-01

    A portable dynamic air sampler and solid phase microextraction were used to simultaneously detect, identify, and quantify airborne sarin with immediate analysis of samples using a field portable gas chromatography-mass spectrometry system. A mathematical model was used with knowledge of the mass of sarin trapped, linear air velocity past the exposed sampling fiber, and sample duration allowing calculation of concentration estimates. For organizations with suitable field portable instrumentation, these methods are potentially useful for rapid onsite detection and quantification of high concern analytes, either through direct environmental sampling or through sampling of air collected in bags.

  15. DOE methods for evaluating environmental and waste management samples.

    Energy Technology Data Exchange (ETDEWEB)

    Goheen, S C; McCulloch, M; Thomas, B L; Riley, R G; Sklarew, D S; Mong, G M; Fadeff, S K [eds.; Pacific Northwest Lab., Richland, WA (United States)

    1994-04-01

    DOE Methods for Evaluating Environmental and Waste Management Samples (DOE Methods) provides applicable methods in use by. the US Department of Energy (DOE) laboratories for sampling and analyzing constituents of waste and environmental samples. The development of DOE Methods is supported by the Laboratory Management Division (LMD) of the DOE. This document contains chapters and methods that are proposed for use in evaluating components of DOE environmental and waste management samples. DOE Methods is a resource intended to support sampling and analytical activities that will aid in defining the type and breadth of contamination and thus determine the extent of environmental restoration or waste management actions needed, as defined by the DOE, the US Environmental Protection Agency (EPA), or others.

  16. Data analysis methods for solid-state nanopores

    Science.gov (United States)

    Plesa, Calin; Dekker, Cees

    2015-02-01

    We describe a number of techniques for the analysis of solid-state nanopore ionic current traces and introduce a new package of Matlab analysis scripts with GUI front ends. We discuss methods for the detection of the local baseline and propose a new detection algorithm that bypasses some of the classical weaknesses of moving-average detection. Our new approach removes detected events and re-creates an ideal event-free baseline subsequently used to recalculate the local baseline. Iterative operation of this algorithm causes both the moving average of the baseline current and its standard deviation to converge to their correct values. We explain different approaches to selecting events and building event populations, and we show the value of keeping track of the changes in parameters, such as the event rate and the pore resistance, throughout the course of the experiment. Finally, we introduce a new technique for separating unfolded events and detecting current spikes present within translocation events. This open source software package is available online at: http://ceesdekkerlab.tudelft.nl/downloads/

  17. Evaluation of the readsorption of plutonium and americium in dynamic fractionations of environmental solid samples.

    Science.gov (United States)

    Petersen, Roongrat; Hou, Xiaolin; Hansen, Elo Harald

    2008-07-01

    A dynamic extraction system exploiting sequential injection (SI) for sequential extractions incorporating a specially designed extraction column is developed to fractionate radionuclides in environmental solid samples such as soils and sediments. The extraction column can contain up to 5 g of a soil sample, and under optimal operational conditions it does not give rise to creation of back pressure. Attention has been placed on studies of the readsorption problems during sequential extraction using a modified Standards, Measurements and Testing (SM&T) scheme with four-step sequential extractions. The degree of readsorption in dynamic and conventional batch extraction systems is compared and evaluated by using a double-spiking technique. A high degree of readsorption of plutonium and americium (>75%) was observed in both systems, and they also exhibited similar distribution patterns of the two radionuclides. However, the dynamic system is fully automated, eliminates manual separations, significantly reduces the operational time required, and offers detailed kinetic information.

  18. A random spatial sampling method in a rural developing nation

    Science.gov (United States)

    Michelle C. Kondo; Kent D.W. Bream; Frances K. Barg; Charles C. Branas

    2014-01-01

    Nonrandom sampling of populations in developing nations has limitations and can inaccurately estimate health phenomena, especially among hard-to-reach populations such as rural residents. However, random sampling of rural populations in developing nations can be challenged by incomplete enumeration of the base population. We describe a stratified random sampling method...

  19. Solid phase extraction and determination of carbamate pesticides in water samples by reverse-phase HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Moreno-Tovar, J.; Santos-Delgado, M.J. [Departamento de Quimica Analitica, Facultad de ciencias Quimicas, Universidad Complutense de Madrid (Spain)

    1995-12-31

    Solid phase extraction. SPE. using C{sub 1}8 bonded silica cartridges for trace amounts determination of carbaryl, propoxur, thiram, propham and methiocarb in water samples was studied and the breakthrough volume of the cartridges was established. The high enrichment factor and large injection volume admissible in the isocratic reverse-phase HPLC system allows pesticides determination with UV detection at 22o nm even at a concentration lower than 0.05 mug/L. Purified tap natural and underground water samples were spiked with carbamate pesticides in the concentration range 0.16-16.0 mug/L. Large volumes of samples (up to 2L) were passed through available C{sub 1}8, cartridges and eluted with acetonitrile. The preconcentrated samples were analyzed by HPLC using a Spherisorb ODS column with a 42.58 acetonitrile-water mobile phase. From replicate samples, recovery for the pesticides ranged from 79.0 to 103.7% except for thiran which is not retained. Tehe relative standard deviation (n=4 at 0.16 to 1.61 mug/L concetration level) range from 1.1 to 6.8%. (Author) 14 refs.

  20. Analysis of Mars Analogue Soil Samples Using Solid-Phase Microextraction, Organic Solvent Extraction and Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Orzechowska, G. E.; Kidd, R. D.; Foing, B. H.; Kanik, I.; Stoker, C.; Ehrenfreund, P.

    2011-01-01

    Polycyclic aromatic hydrocarbons (PAHs) are robust and abundant molecules in extraterrestrial environments. They are found ubiquitously in the interstellar medium and have been identified in extracts of meteorites collected on Earth. PAHs are important target molecules for planetary exploration missions that investigate the organic inventory of planets, moons and small bodies. This study is part of an interdisciplinary preparation phase to search for organic molecules and life on Mars. We have investigated PAH compounds in desert soils to determine their composition, distribution and stability. Soil samples (Mars analogue soils) were collected at desert areas of Utah in the vicinity of the Mars Desert Research Station (MDRS), in the Arequipa region in Peru and from the Jutland region of Denmark. The aim of this study was to optimize the solid-phase microextraction (SPME) method for fast screening and determination of PAHs in soil samples. This method minimizes sample handling and preserves the chemical integrity of the sample. Complementary liquid extraction was used to obtain information on five- and six-ring PAH compounds. The measured concentrations of PAHs are, in general, very low, ranging from 1 to 60 ng g(sup -1). The texture of soils is mostly sandy loam with few samples being 100% silt. Collected soils are moderately basic with pH values of 8-9 except for the Salten Skov soil, which is slightly acidic. Although the diverse and variable microbial populations of the samples at the sample sites might have affected the levels and variety of PAHs detected, SPME appears to be a rapid, viable field sampling technique with implications for use on planetary missions.

  1. Experience sampling with elderly persons: an exploration of the method.

    Science.gov (United States)

    Hnatiuk, S H

    1991-01-01

    The daily lives of a sample of elderly widows (greater than 69 years of age) were studied using the method of experience sampling developed by Csikszentmihalyi and his colleagues. The purpose of the study was to investigate the response of elderly people to experience sampling as a means of collecting information about their activities, thoughts, and moods during the course of one week. The method proved acceptable to the majority of participants and yielded reliable, valid data about their home lives, particularly from among the younger, more physically able women. Experience sampling was, within certain limits, a useful method of obtaining information from elderly people.

  2. THE USE OF RANKING SAMPLING METHOD WITHIN MARKETING RESEARCH

    Directory of Open Access Journals (Sweden)

    CODRUŢA DURA

    2011-01-01

    Full Text Available Marketing and statistical literature available to practitioners provides a wide range of sampling methods that can be implemented in the context of marketing research. Ranking sampling method is based on taking apart the general population into several strata, namely into several subdivisions which are relatively homogenous regarding a certain characteristic. In fact, the sample will be composed by selecting, from each stratum, a certain number of components (which can be proportional or non-proportional to the size of the stratum until the pre-established volume of the sample is reached. Using ranking sampling within marketing research requires the determination of some relevant statistical indicators - average, dispersion, sampling error etc. To that end, the paper contains a case study which illustrates the actual approach used in order to apply the ranking sample method within a marketing research made by a company which provides Internet connection services, on a particular category of customers – small and medium enterprises.

  3. GROUND WATER PURGING AND SAMPLING METHODS: HISTORY VS. HYSTERIA

    Science.gov (United States)

    It has been over 10 years since the low-flow ground water purging and sampling method was initially reported in the literature. The method grew from the recognition that well purging was necessary to collect representative samples, bailers could not achieve well purging, and high...

  4. Neonatal blood gas sampling methods | Goenka | South African ...

    African Journals Online (AJOL)

    There is little published guidance that systematically evaluates the different methods of neonatal blood gas sampling, where each method has its individual benefits and risks. This review critically surveys the available evidence to generate a comparison between arterial and capillary blood gas sampling, focusing on their ...

  5. An efficient method for sampling the essential subspace of proteins

    NARCIS (Netherlands)

    Amadei, A; Linssen, A.B M; de Groot, B.L.; van Aalten, D.M.F.; Berendsen, H.J.C.

    A method is presented for a more efficient sampling of the configurational space of proteins as compared to conventional sampling techniques such as molecular dynamics. The method is based on the large conformational changes in proteins revealed by the ''essential dynamics'' analysis. A form of

  6. A combination of novel solid-state NMR methods and related software to study molecular assemblies and biomolecules

    NARCIS (Netherlands)

    Gradmann, S.H.E.

    2013-01-01

    Solid-state Nuclear Magnetic Resonance (ssNMR) is a versatile spectroscopic method that can be applied to various samples relevant in life and material science and provides atomic insight into molecular structure, dynamics and assembly. The present thesis describes the diversity and utility of ssNMR

  7. Neutron reflectivity as method to study in-situ adsorption of phospholipid layers to solid-liquid interfaces

    DEFF Research Database (Denmark)

    Gutberlet, Thomas; Klösgen, Beate Maria; Krastev, Rumen

    2004-01-01

    The use of neutron reflectivity as a method to study in-situ adsorption of phospholipid layers to solid-liquid interfaces was analyzed. The most important advantage of neutron reflectometry is the possibility to very the refractive index of the specific sample by isotope exchange, called contrast...

  8. Molecularly imprinted polymer for the extraction of parabens from environmental solid samples prior to their determination by high performance liquid chromatography-ultraviolet detection.

    Science.gov (United States)

    Núñez, L; Turiel, E; Martin-Esteban, A; Tadeo, J L

    2010-03-15

    An analytical methodology incorporating a molecularly imprinted solid-phase extraction procedure (MISPE) has been developed for the determination of parabens in environmental solid samples. Four different polymers were prepared combining the use of acetonitrile or toluene as porogen, and 4-vinylpyridine (VP) or methacrylic acid (MAA) as monomer, using benzylparaben (BzP) as a template molecule. Although all the polymers were able to recognize the template in rebinding experiments, the MIP prepared in toluene using MAA showed better performance. This polymer was also capable of recognizing other parabens (methyl, ethyl, isopropyl, propyl, isobutyl, butyl and benzylparaben) allowing to develop an appropriated MISPE procedure for this family of compounds. The extraction of the parabens from environmental solid samples was performed by ultrasonic assisted extraction in small columns (SAESC), and this procedure next to MISPE as clean-up step followed by HPLC-UV determination was successfully used for the determination of parabens in soil and sediment samples of different locations. Recoveries ranging from 80% to 90% have been achieved depending on the compound and the samples, and limits of detection (LODs) were under 1 ng g(-1) for all the compounds, making this method suitable for the determination of parabens in environmental solid matrices. The method was further applied to the determination of paraben contents in real samples, founding levels up to 11.5 ng g(-1) in sea sediments. Copyright (c) 2009 Elsevier B.V. All rights reserved.

  9. A method and fortran program for quantitative sampling in paleontology

    Science.gov (United States)

    Tipper, J.C.

    1976-01-01

    The Unit Sampling Method is a binomial sampling method applicable to the study of fauna preserved in rocks too well cemented to be disaggregated. Preliminary estimates of the probability of detecting each group in a single sampling unit can be converted to estimates of the group's volumetric abundance by means of correction curves obtained by a computer simulation technique. This paper describes the technique and gives the FORTRAN program. ?? 1976.

  10. Solid-phase extraction method for patulin in apple juice and unfiltered apple juice.

    Science.gov (United States)

    Trucksess, M W; Tang, Y

    1999-01-01

    Patulin, a mold metabolite, is commonly found in rotting apples. Some countries regulate patulin at levels ranging from 30 to 50 micrograms/L. Most analytical methods for patulin in apple juice include liquid-liquid partitions. A solid-phase extraction method has been developed for apple juice and unfiltered apple juice in the United States. A portion of the test sample (5 mL) was passed through a macroporous copolymer cartridge and was washed with 1 mL 1% sodium bicarbonate and then with 1 mL 1% acetic acid. Patulin was eluted with 3 mL 2% acetonitrile in anhydrous ethyl ether and was determined by reversed-phase liquid chromatography with UV detection at 276 nm. Recoveries ranged from 93 to 104% in test samples spiked at 20-100 micrograms/L.

  11. Final Report for X-ray Diffraction Sample Preparation Method Development

    Energy Technology Data Exchange (ETDEWEB)

    Ely, T. M.; Meznarich, H. K.; Valero, T.

    2018-01-30

    WRPS-1500790, “X-ray Diffraction Saltcake Sample Preparation Method Development Plan/Procedure,” was originally prepared with the intent of improving the specimen preparation methodology used to generate saltcake specimens suitable for XRD-based solid phase characterization. At the time that this test plan document was originally developed, packed powder in cavity supports with collodion binder was the established XRD specimen preparation method. An alternate specimen preparation method less vulnerable, if not completely invulnerable to preferred orientation effects, was desired as a replacement for the method.

  12. Method for Hot Real-Time Sampling of Gasification Products

    Energy Technology Data Exchange (ETDEWEB)

    Pomeroy, Marc D [National Renewable Energy Laboratory (NREL), Golden, CO (United States)

    2017-09-29

    The Thermochemical Process Development Unit (TCPDU) at the National Renewable Energy Laboratory (NREL) is a highly instrumented half-ton/day pilot scale plant capable of demonstrating industrially relevant thermochemical technologies from lignocellulosic biomass conversion, including gasification. Gasification creates primarily Syngas (a mixture of Hydrogen and Carbon Monoxide) that can be utilized with synthesis catalysts to form transportation fuels and other valuable chemicals. Biomass derived gasification products are a very complex mixture of chemical components that typically contain Sulfur and Nitrogen species that can act as catalysis poisons for tar reforming and synthesis catalysts. Real-time hot online sampling techniques, such as Molecular Beam Mass Spectrometry (MBMS), and Gas Chromatographs with Sulfur and Nitrogen specific detectors can provide real-time analysis providing operational indicators for performance. Sampling typically requires coated sampling lines to minimize trace sulfur interactions with steel surfaces. Other materials used inline have also shown conversion of sulfur species into new components and must be minimized. Sample line Residence time within the sampling lines must also be kept to a minimum to reduce further reaction chemistries. Solids from ash and char contribute to plugging and must be filtered at temperature. Experience at NREL has shown several key factors to consider when designing and installing an analytical sampling system for biomass gasification products. They include minimizing sampling distance, effective filtering as close to source as possible, proper line sizing, proper line materials or coatings, even heating of all components, minimizing pressure drops, and additional filtering or traps after pressure drops.

  13. Municipal solid waste composition: Sampling methodology, statistical analyses, and case study evaluation

    Energy Technology Data Exchange (ETDEWEB)

    Edjabou, Maklawe Essonanawe, E-mail: vine@env.dtu.dk [Department of Environmental Engineering, Technical University of Denmark, 2800 Kgs. Lyngby (Denmark); Jensen, Morten Bang; Götze, Ramona; Pivnenko, Kostyantyn [Department of Environmental Engineering, Technical University of Denmark, 2800 Kgs. Lyngby (Denmark); Petersen, Claus [Econet AS, Omøgade 8, 2.sal, 2100 Copenhagen (Denmark); Scheutz, Charlotte; Astrup, Thomas Fruergaard [Department of Environmental Engineering, Technical University of Denmark, 2800 Kgs. Lyngby (Denmark)

    2015-02-15

    Highlights: • Tiered approach to waste sorting ensures flexibility and facilitates comparison of solid waste composition data. • Food and miscellaneous wastes are the main fractions contributing to the residual household waste. • Separation of food packaging from food leftovers during sorting is not critical for determination of the solid waste composition. - Abstract: Sound waste management and optimisation of resource recovery require reliable data on solid waste generation and composition. In the absence of standardised and commonly accepted waste characterisation methodologies, various approaches have been reported in literature. This limits both comparability and applicability of the results. In this study, a waste sampling and sorting methodology for efficient and statistically robust characterisation of solid waste was introduced. The methodology was applied to residual waste collected from 1442 households distributed among 10 individual sub-areas in three Danish municipalities (both single and multi-family house areas). In total 17 tonnes of waste were sorted into 10–50 waste fractions, organised according to a three-level (tiered approach) facilitating comparison of the waste data between individual sub-areas with different fractionation (waste from one municipality was sorted at “Level III”, e.g. detailed, while the two others were sorted only at “Level I”). The results showed that residual household waste mainly contained food waste (42 ± 5%, mass per wet basis) and miscellaneous combustibles (18 ± 3%, mass per wet basis). The residual household waste generation rate in the study areas was 3–4 kg per person per week. Statistical analyses revealed that the waste composition was independent of variations in the waste generation rate. Both, waste composition and waste generation rates were statistically similar for each of the three municipalities. While the waste generation rates were similar for each of the two housing types (single

  14. Representation of solid and nutrient concentrations in irrigation water from tailwater recovery systems by surface water grab samples

    Science.gov (United States)

    Tailwater recovery (TWR) systems are being implemented on agricultural landscapes to create an additional source of irrigation water. Existing studies have sampled TWR systems using grab samples; however, the applicability of solids and nutrient concentrations in these samples to water being irrigat...

  15. A NEW SAMPLE CELL DESIGN FOR STUDYING SOLID-MATRIX ROOM TEMPERATURE PHOSPHORESCENCE MOISTURE QUENCHING. (R824100)

    Science.gov (United States)

    A new sample chamber was developed that can be used in the measurement of the effects of moisture on the room-temperature solid-matrix phosphorescence of phosphors adsorbed onto filter paper. The sample chamber consists of a sealed quartz cell that contains a special teflon sampl...

  16. Method and apparatus for imaging a sample on a device

    Science.gov (United States)

    Trulson, Mark; Stern, David; Fiekowsky, Peter; Rava, Richard; Walton, Ian; Fodor, Stephen P. A.

    2001-01-01

    A method and apparatus for imaging a sample are provided. An electromagnetic radiation source generates excitation radiation which is sized by excitation optics to a line. The line is directed at a sample resting on a support and excites a plurality of regions on the sample. Collection optics collect response radiation reflected from the sample I and image the reflected radiation. A detector senses the reflected radiation and is positioned to permit discrimination between radiation reflected from a certain focal plane in the sample and certain other planes within the sample.

  17. Determination of trace copper in food samples by flame atomic absorption spectrometry after solid phase extraction on modified soybean hull

    Energy Technology Data Exchange (ETDEWEB)

    Xiang Guoqiang, E-mail: xianggq@126.com [School of Chemistry and Chemical Engineering, Henan University of Technology, Zhengzhou 450001 (China); Zhang Yingming; Jiang Xiuming; He Lijun; Fan Lu; Zhao Wenjie [School of Chemistry and Chemical Engineering, Henan University of Technology, Zhengzhou 450001 (China)

    2010-07-15

    Soybean hull was chemically modified with citric acid and used as a solid phase extraction adsorbent for the determination of trace amounts of Cu{sup 2+} in food samples by flame absorption spectrometry (FAAS). The effect of pH, sample flow rate and volume, elution flow rate and volume and co-existing ions on the recovery of the analyte were investigated. The results showed that Cu{sup 2+} could be adsorbed on the modified soybean hull at pH 8.0 and eluted by 2.0 mL of 1.0 mol L{sup -1} HCl. Under the optimized conditions, the adsorption capacity of modified soybean hull was found to be 18.0 mg g{sup -1} for Cu{sup 2+}. The detection limit of the proposed method was 0.8 ng mL{sup -1} for Cu{sup 2+} with an enrichment factor of 18. The analytical result for the certified reference tea sample (GBW07605) was in a good agreement with the certified value. The proposed method has also been successfully applied to the determination of trace Cu{sup 2+} in dried sweet potato, lake water and milk powder, the recovery of Cu{sup 2+} for spiked samples was between 91% and 109.6%.

  18. Influence of sampling intake position on suspended solid measurements in sewers: two probability/time-series-based approaches.

    Science.gov (United States)

    Sandoval, Santiago; Bertrand-Krajewski, Jean-Luc

    2016-06-01

    Total suspended solid (TSS) measurements in urban drainage systems are required for several reasons. Aiming to assess uncertainties in the mean TSS concentration due to the influence of sampling intake vertical position and vertical concentration gradients in a sewer pipe, two methods are proposed: a simplified method based on a theoretical vertical concentration profile (SM) and a time series grouping method (TSM). SM is based on flow rate and water depth time series. TSM requires additional TSS time series as input data. All time series are from the Chassieu urban catchment in Lyon, France (time series from 2007 with 2-min time step, 89 rainfall events). The probability of measuring a TSS value lower than the mean TSS along the vertical cross section (TSS underestimation) is about 0.88 with SM and about 0.64 with TSM. TSM shows more realistic TSS underestimation values (about 39 %) than SM (about 269 %). Interquartile ranges (IQR) over the probability values indicate that SM is more uncertain (IQR = 0.08) than TSM (IQR = 0.02). Differences between the two methods are mainly due to simplifications in SM (absence of TSS measurements). SM assumes a significant asymmetry of the TSS concentration profile along the vertical axis in the cross section. This is compatible with the distribution of TSS measurements found in the TSM approach. The methods provide insights towards an indicator of the measurement performance and representativeness for a TSS sampling protocol.

  19. Methods for measurement of gas flow velocity, methods for energy conversion using gas flow over solid material, and device therefor

    OpenAIRE

    Sood, Ajay Kumar; Ghosh, Shankar

    2004-01-01

    The present invention relates to a methods for energy conversion by gas flow over solid materials and also to a method for measurement of velocity of a gas flow over solid material such as doped semiconductors, graphite, and the like as a function of the 5 electricity generated in the solid material due to the flow of the gas the surface thereof using a combination of the Seebeck effect and Bernoulli's principle.

  20. Evaluating Composite Sampling Methods of Bacillus spores at Low Concentrations

    Energy Technology Data Exchange (ETDEWEB)

    Hess, Becky M.; Amidan, Brett G.; Anderson, Kevin K.; Hutchison, Janine R.

    2016-10-13

    Restoring facility operations after the 2001 Amerithrax attacks took over three months to complete, highlighting the need to reduce remediation time. The most time intensive tasks were environmental sampling and sample analyses. Composite sampling allows disparate samples to be combined, with only a single analysis needed, making it a promising method to reduce response times. We developed a statistical experimental design to test three different composite sampling methods: 1) single medium single pass composite: a single cellulose sponge samples multiple coupons; 2) single medium multi-pass composite: a single cellulose sponge is used to sample multiple coupons; and 3) multi-medium post-sample composite: a single cellulose sponge samples a single surface, and then multiple sponges are combined during sample extraction. Five spore concentrations of Bacillus atrophaeus Nakamura spores were tested; concentrations ranged from 5 to 100 CFU/coupon (0.00775 to 0.155CFU/cm2, respectively). Study variables included four clean surface materials (stainless steel, vinyl tile, ceramic tile, and painted wallboard) and three grime coated/dirty materials (stainless steel, vinyl tile, and ceramic tile). Analysis of variance for the clean study showed two significant factors: composite method (p-value < 0.0001) and coupon material (p-value = 0.0008). Recovery efficiency (RE) was higher overall using the post-sample composite (PSC) method compared to single medium composite from both clean and grime coated materials. RE with the PSC method for concentrations tested (10 to 100 CFU/coupon) was similar for ceramic tile, painted wall board, and stainless steel for clean materials. RE was lowest for vinyl tile with both composite methods. Statistical tests for the dirty study showed RE was significantly higher for vinyl and stainless steel materials, but significantly lower for ceramic tile. These results suggest post-sample compositing can be used to reduce sample analysis time when

  1. Methanol synthesis catalyst manufacturing using the green solid-state method

    Directory of Open Access Journals (Sweden)

    Neda Mirhosseini

    2017-01-01

    Full Text Available In this research study, methanol synthesis catalysts were manufactured with various mole ratios of metal carbonates (zinc, copper and aluminum carbonate and ammonium hydrogen carbonate via a green solid-state method that employed a ball mill apparatus. Some parameters for the catalyst preparation, such as Al mole percent, Cu/Zn mole ratio, rotations milling speeds and aging time, were optimized to obtain the maximum catalyst activity. The prepared catalysts were compared with the best quality industrial catalyst under the same temperature and pressure condition in a titanium tabular fixed bed reactor. This novel method has many advantages in comparison to the conventional method. The main advantage of the solid-state method is that the methanol synthesis catalyst can be produced without using solvent. Furthermore, this new method reduces operating costs due to the elimination of the filtration and washing steps. Methanol synthesis catalytic activity was maximized at an optimized mole ratio of Cu/Zn of 1.9234 and an Al mole percent of 8 at the maximum grinding speed (450 rpm during an aging time of 30 min, which showed higher activity (240 gCH3OH/kg cat.h in comparison with an industrial catalyst sample (218 gCH3OH/kg cat.h. The production of a green catalyst, which requires less water and results in higher catalyst activity, can be widely used for methanol synthesis catalytic applications.

  2. Boson Sampling with Single-Photon Fock States from a Bright Solid-State Source.

    Science.gov (United States)

    Loredo, J C; Broome, M A; Hilaire, P; Gazzano, O; Sagnes, I; Lemaitre, A; Almeida, M P; Senellart, P; White, A G

    2017-03-31

    A boson-sampling device is a quantum machine expected to perform tasks intractable for a classical computer, yet requiring minimal nonclassical resources as compared to full-scale quantum computers. Photonic implementations to date employed sources based on inefficient processes that only simulate heralded single-photon statistics when strongly reducing emission probabilities. Boson sampling with only single-photon input has thus never been realized. Here, we report on a boson-sampling device operated with a bright solid-state source of single-photon Fock states with high photon-number purity: the emission from an efficient and deterministic quantum dot-micropillar system is demultiplexed into three partially indistinguishable single photons, with a single-photon purity 1-g^{(2)}(0) of 0.990±0.001, interfering in a linear optics network. Our demultiplexed source is between 1 and 2 orders of magnitude more efficient than current heralded multiphoton sources based on spontaneous parametric down-conversion, allowing us to complete the boson-sampling experiment faster than previous equivalent implementations.

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

    Science.gov (United States)

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

    2015-01-01

    This work describes the application of ultrasound-assisted matrix solid-phase dispersion as an extraction and sample preparation approach for aflatoxins (B1, B2, G1 and G2) and subsequent determination of them by high-performance liquid chromatography-fluorescence detection. A Box-Behnken design in combination with response surface methodology was used to determine the affecting parameters on the extraction procedure. The influence of different variables including type of dispersing phase, sample-to-dispersing phase ratio, type and quantity of clean-up phase, ultrasonication time, ultrasonication temperature, nature and volume of the elution solvent was investigated in the optimization study. C18, primary-secondary amine (PSA) and acetonitrile were selected as dispersing phase, clean-up phase and elution solvent, respectively. The obtained optimized values were sample-to-dispersing phase ratio of 1 : 1, 60 mg of PSA, 11 min ultrasonication time, 30°C ultrasonication temperature and 4 mL acetonitrile. Under the optimal conditions, the limits of detection were ranged from 0.09 to 0.14 ng g(-1) and the precisions [relative standard deviation (RSD%)] were aflatoxins in rice samples. © The Author [2014]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  4. Sampling Methods for Web and E-mail Surveys

    OpenAIRE

    Fricker, RD

    2012-01-01

    London: SAGE Publications. Reprinted from The SAGE Handbook of Online Research Methods, N. Fielding, R.M. Lee and G. Blank, eds., chapter 11, London: SAGE Publications, 195-216. This chapter is a comprehensive overview of sampling methods for web and e-mail (‘Internetbased’) surveys. It reviews the various types of sampling method – both probability and nonprobability – and examines their applicability to Internet-based surveys. Issues related to Internetbased survey samp...

  5. Evaluation of common methods for sampling invertebrate pollinator assemblages: net sampling out-perform pan traps.

    Directory of Open Access Journals (Sweden)

    Tony J Popic

    Full Text Available Methods for sampling ecological assemblages strive to be efficient, repeatable, and representative. Unknowingly, common methods may be limited in terms of revealing species function and so of less value for comparative studies. The global decline in pollination services has stimulated surveys of flower-visiting invertebrates, using pan traps and net sampling. We explore the relative merits of these two methods in terms of species discovery, quantifying abundance, function, and composition, and responses of species to changing floral resources. Using a spatially-nested design we sampled across a 5000 km(2 area of arid grasslands, including 432 hours of net sampling and 1296 pan trap-days, between June 2010 and July 2011. Net sampling yielded 22% more species and 30% higher abundance than pan traps, and better reflected the spatio-temporal variation of floral resources. Species composition differed significantly between methods; from 436 total species, 25% were sampled by both methods, 50% only by nets, and the remaining 25% only by pans. Apart from being less comprehensive, if pan traps do not sample flower-visitors, the link to pollination is questionable. By contrast, net sampling functionally linked species to pollination through behavioural observations of flower-visitation interaction frequency. Netted specimens are also necessary for evidence of pollen transport. Benefits of net-based sampling outweighed minor differences in overall sampling effort. As pan traps and net sampling methods are not equivalent for sampling invertebrate-flower interactions, we recommend net sampling of invertebrate pollinator assemblages, especially if datasets are intended to document declines in pollination and guide measures to retain this important ecosystem service.

  6. Determination of Pt, Pd and Rh in Brassica Napus using solid sampling electrothermal vaporization inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Nischkauer, Winfried [Vienna University of Technology, Institute of Chemical Technologies and Analytics, Division of Instrumental Analytical Chemistry, Getreidemarkt 9/164-IAC, A-1060 Vienna (Austria); Herincs, Esther [Vienna University of Technology, Institute of Chemical Technologies and Analytics, Division of Instrumental Analytical Chemistry, Getreidemarkt 9/164-IAC, A-1060 Vienna (Austria); University of Natural Resources and Life Sciences, Department of Forest and Soil Sciences, Institute of Soil Research, Konrad Lorenz Straße 24, A-3430 Tulln (Austria); Puschenreiter, Markus; Wenzel, Walter [University of Natural Resources and Life Sciences, Department of Forest and Soil Sciences, Institute of Soil Research, Konrad Lorenz Straße 24, A-3430 Tulln (Austria); Limbeck, Andreas, E-mail: A.Limbeck@tuwien.ac.at [Vienna University of Technology, Institute of Chemical Technologies and Analytics, Division of Instrumental Analytical Chemistry, Getreidemarkt 9/164-IAC, A-1060 Vienna (Austria)

    2013-11-01

    Conventional approaches for the analysis of platinum group elements (PGEs) in plant material suffer from sample digestion which results in sample dilution and therefore requires high sample intakes to maintain the sensitivity. The presented solid-sampling method avoids sample digestion while improving sensitivity when compared to digestion-based inductively coupled plasma optical emission spectrometry (ICP-OES) methods and allows the analysis of sample masses of 5 mg or less. Detection limits of 0.38 μg g{sup −1}, 0.14 μg g{sup −1} and 0.13 μg g{sup −1} were obtained for Pt, Pd and Rh, respectively using a sample intake of 5 mg. The reproducibility of the procedure ranged between 4.7% (Pd) relative standard deviation (RSD, n = 7) and 7.1% (Rh) RSD for 25 ng analytes. For quantification, aqueous standards were applied on paper filter strips and dried. Only the dried filters were introduced into the electrothermal vaporization unit. This approach successfully removed memory-effects observed during analysis of platinum which occurred only if liquid standards came into contact with the graphite material of the furnace. The presented method for overcoming the Pt-memory-effects may be of further interest for the analysis of other carbide-forming analytes as it does not require any technical modification of the graphite furnace (e.g., metal inlays, pyrolytic coating). Owing to lack of suitable certified reference materials, the proposed method was compared with conventional ICP-OES analysis of digested samples and a good agreement was obtained. As a result of the low sample consumption, it was possible to determine the spatial distribution of PGEs within a single plant. Significant differences in PGE concentrations were observed between the shoots (stem, leaves) and the roots. Pd was mainly found in the roots, whereas Pt and Rh were also found in higher concentrations in the shoots. - Highlights: • The uptake of Pt, Pd and Rh by hydroponically grown plants was

  7. Modified zeolitic imidazolate framework-8 as solid-phase microextraction Arrow coating for sampling of amines in wastewater and food samples followed by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Lan, Hangzhen; Rönkkö, Tuukka; Parshintsev, Jevgeni; Hartonen, Kari; Gan, Ning; Sakeye, Motolani; Sarfraz, Jawad; Riekkola, Marja-Liisa

    2017-02-24

    In this study, a novel solid phase microextration (SPME) Arrow was prepared for the sampling of volatile low molecular weight alkylamines (trimethylamine (TMA) and triethylamine (TEA)) in wastewater, salmon and mushroom samples before gas chromatographic separation with mass spectrometer as detector. Acidified zeolitic imidazolate framework-8 (A-ZIF-8) was utilized as adsorbent and poly(vinyl chloride) (PVC) as the adhesive. The custom SPME Arrow was fabricated via a physical adhesion: (1) ZIF-8 particles were suspended in a mixture of tetrahydrofuran (THF) and PVC to form a homogeneous suspension, (2) a non-coated stainless steel SPME Arrow was dipped in the ZIF-8/PVC suspension for several times to obtain a uniform and thick coating, (3) the pore size of ZIF-8 was modified by headspace exposure to hydrochloric acid in order to increase the extraction efficiency for amines. The effect of ZIF-8 concentration in PVC solution, dipping cycles and aging temperature on extraction efficiency was investigated. In addition, sampling parameters such as NaCl concentration, sample volume, extraction time, potassium hydroxide concentration, desorption temperature and desorption time were optimized. The Arrow-to-Arrow reproducibilities (RSDs) for five ZIF-8 coated Arrows were 15.6% and 13.3% for TMA and TEA, respectively. The extraction with A-ZIF-8/PVC Arrow was highly reproducible for at least 130 cycles without noticeable decrease of performance (RSD<12.5%). Headspace SPME of 7.5mL sample solution with the fabricated ZIF-8 coated Arrow achieved linear ranges of 1-200ngmL(-1) for both TMA and TEA. The limit of quantitation (LOQ) was 1ngmL(-1) for both TMA and TEA. The method was successfully applied to the determination of TMA and TEA in wastewater, salmon and mushroom samples giving satisfactory selectivity towards the studied amines. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Development of a selective molecularly imprinted polymer-based solid-phase extraction for indomethacin from water samples.

    Science.gov (United States)

    Yang, Tao; Li, Ya-Hui; Wei, Shuang; Li, Yuan; Deng, Anping

    2008-08-01

    A selective molecularly imprinted solid-phase extraction (MISPE) for indomethacin (IDM) from water samples was developed. Using IDM as template molecule, acrylamide (AM) or methacrylic acid (MAA) as functional monomer, ethylene dimethacrylate (EDMA) as crosslinker, and bulk or suspension polymerization as the synthetic method, three molecularly imprinted polymers (MIPs) were synthesized and characterized with a rebinding experiment. It was found that the MIP of AM-EDMA produced by bulk polymerization showed the highest binding capacity for IDM, and so it was chosen for subsequent experiments, such as those testing the selectivity and recognition binding sites. Scatchard analysis revealed that at least two kinds of binding sites formed in the MIP, with the dissociation constants of 7.8 micromol L(-1) and 127.2 micromol L(-1), respectively. Besides IDM, three structurally related compounds--acemetacin, oxaprozin and ibuprofen--were employed for selectivity tests. It was observed that the MIP exhibited the highest selective rebinding to IDM. Accordingly, the MIP was used as a solid-phase extraction sorbent for the extraction and enrichment of IDM in water samples. The extraction conditions of the MISPE column for IDM were optimized to be: chloroform or water as loading solvent, chloroform with 20% acetonitrile as washing solution, and methanol as eluting solvent. Water samples with or without spiking were extracted by the MISPE column and analyzed by HPLC. No detectable IDM was observed in tap water and the content of IDM in a river water sample was found to be 1.8 ng mL(-1). The extraction efficiencies of the MISPE column for IDM in spiked tap and river water were acceptable (87.2% and 83.5%, respectively), demonstrating the feasibility of the prepared MIP for IDM extraction.

  9. WIPP Sampling and Analysis Plan for Solid Waste Management Units and Areas of Concern

    Energy Technology Data Exchange (ETDEWEB)

    None, None

    2000-05-23

    This Sampling and Analysis Plan (SAP) has been prepared to fulfill requirements of Module VII, Section VII.M.2 and Table VII.1, requirement 4 of the Waste Isolation Pilot Plant (WIPP) Hazardous Waste Permit, NM4890139088-TSDF (the Permit); (NMED [New Mexico Environment Department], 1999a). This SAP describes the approach for investigation of the Solid Waste Management Units (SWMU) and Areas of Concern (AOC) specified in the Permit. This SAP addresses the current Permit requirements for a RCRA Facility Investigation(RFI) investigation of SWMUs and AOCs. It uses the results of previous investigations performed at WIPP and expands the investigations as required by the Permit. As an alternative to the RFI specified in Module VII of the Permit, current NMED guidance identifies an Accelerated Corrective Action Approach (ACAA) that may be used for any SWMU or AOC (NMED, 1998). This accelerated approach is used to replace the standard RFI work plan and report sequence with a more flexible decision-making approach. The ACAA process allows a facility to exit the schedule of compliance contained in the facility's Hazardous and Solid Waste Amendments (HSWA) permit module and proceed on an accelerated time frame. Thus, the ACAA process can beentered either before or after a RFI work plan. According to NMED's guidance, a facility can prepare a RFI work plan or SAP for any SWMU or AOC (NMED, 1998).

  10. A solid-phase microextraction method for the chromatographic determination of organophosphorus pesticides in fish, water, potatoes, guava and coffee

    OpenAIRE

    Capobiango,Helena L. V.; Cardeal, Zenilda L.

    2005-01-01

    This paper describes a Solid Phase Microextraction method (SPME-CG) to the determination of organophosphorus pesticides in samples of fresh-water fish, water, potatoes, guava and coffee by capillary gas chromatography with nitrogen phosphorus detector. The samples were collected from October 2002 to April 2003 in the tributaries and sub-tributaries of the Paranaiba River, which supplies the city of Patos de Minas, Minas Gerais, Brazil. The determination of the pesticides: co-ral (O,O-diethyl ...

  11. Local atomic structure of solid solutions with overlapping shells by EXAFS: The regularization method

    Energy Technology Data Exchange (ETDEWEB)

    Babanov, Yu.A., E-mail: babanov@imp.uran.ru [M.N. Miheev Institute of Metal Physics, Ural Branch, Russian Academy of Sciences, Ekaterinburg 620990 (Russian Federation); Ponomarev, D.A.; Ustinov, V.V. [M.N. Miheev Institute of Metal Physics, Ural Branch, Russian Academy of Sciences, Ekaterinburg 620990 (Russian Federation); Baranov, A.N. [M.V. Lomonosov Moscow State University, Moscow 119991 (Russian Federation); Zubavichus, Ya.V. [Russian Research Centre “Kurchatov Institute”, 123182 Moscow (Russian Federation)

    2016-08-15

    Highlights: • A method for determining bond lengths from combined EXAFS spectra for solid oxide solutions is proposed. • We have demonstrated a high resolution in r-space of close spacing atoms in the Periodical Table. • These results were obtained without any assumptions concerning interatomic distances for multi-component systems. • Coordinates ions for the solid solution with rock salt structure are determined. - Abstract: The regularization method of solving ill-posed problem is used to determine five partial interatomic distances on the basis of combined two EXAFS spectra. Mathematical algorithm and experimental results of the EXAFS analysis for Ni{sub c}Zn{sub 1−c}O (c = 0.0, 0.3, 0.5, 0.7, 1.0) solid solutions with the rock salt (rs) crystal structure are discussed. Samples were synthesized from the binary oxide powders at pressure of 7.7 GPa and temperatures 1450–1650 K. The measurements were performed using synchrotron facilities (Russian Research Centre “Kurchatov Institute”, Moscow). The Ni and Zn K absorption spectra were recorded in transmission mode under room temperature. It is shown, the ideal rock salt lattice is distorted and long-range order exists only in the average (Vegard law). In order to determine coordinates ions for the solid solution with rock salt structure, we used the Pauling model. The simulation is performed for 343,000 cluster of oxide ions. The distribution functions for ions (Ni−O, Ni−Ni, Ni−Zn, Zn−Zn, Zn−O, O−O) depending on the distance are obtained. The width of the Gaussian distribution function is determined by the difference of the radii of the metal ions. The results are consistent with the data both X-ray diffraction and the EXAFS spectroscopy.

  12. Method for using polarization gating to measure a scattering sample

    Science.gov (United States)

    Baba, Justin S.

    2015-08-04

    Described herein are systems, devices, and methods facilitating optical characterization of scattering samples. A polarized optical beam can be directed to pass through a sample to be tested. The optical beam exiting the sample can then be analyzed to determine its degree of polarization, from which other properties of the sample can be determined. In some cases, an apparatus can include a source of an optical beam, an input polarizer, a sample, an output polarizer, and a photodetector. In some cases, a signal from a photodetector can be processed through attenuation, variable offset, and variable gain.

  13. Bovine liver sample preparation and micro-homogeneity study for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Nomura, Cassiana S.; Silva, Cíntia S.; Nogueira, Ana R. A.; Oliveira, Pedro V.

    2005-06-01

    This work describes a systematic study for the bovine liver sample preparation for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry. The main parameters investigated were sample drying, grinding process, particle size, sample size, microsample homogeneity, and their relationship with the precision and accuracy of the method. A bovine liver sample was prepared using different drying procedures: (1) freeze drying, and (2) drying in a household microwave oven followed by drying in a stove at 60 °C until constant mass. Ball and cryogenic mills were used for grinding. Less sensitive wavelengths for Cu (216.5 nm) and Zn (307.6 nm), and Zeeman-based three-field background correction for Cu were used to diminish the sensitivities. The pyrolysis and atomization temperatures adopted were 1000 °C and 2300 °C for Cu, and 700 °C and 1700 °C for Zn, respectively. For both elements, it was possible to calibrate the spectrometer with aqueous solutions. The use of 250 μg of W + 200 μg of Rh as permanent chemical modifier was imperative for Zn. Under these conditions, the characteristic mass and detection limit were 1.4 ng and 1.6 ng for Cu, and 2.8 ng and 1.3 ng for Zn, respectively. The results showed good agreement (95% confidence level) for homogeneity of the entire material (> 200 mg) when the sample was dried in microwave/stove and ground in a cryogenic mill. The microsample homogeneity study showed that Zn is more dependent on the sample pretreatment than Cu. The bovine liver sample prepared in microwave/stove and ground in a cryogenic mill presented results with the lowest relative standard deviation for Cu than Zn. Good accuracy and precision were observed for bovine liver masses higher than 40 μg for Cu and 30 μg for Zn. The concentrations of Cu and Zn in the prepared bovine liver sample were 223 mg kg - 1 and 128 mg kg - 1, respectively. The relative standard deviations were lower than 6% ( n = 5). The accuracy of the entire

  14. Method for preconcentrating a sample for subsequent analysis

    Science.gov (United States)

    Zaromb, Solomon

    1990-01-01

    A system for analysis of trace concentration of contaminants in air includes a portable liquid chromatograph and a preconcentrator for the contaminants to be analyzed. The preconcentrator includes a sample bag having an inlet valve and an outlet valve for collecting an air sample. When the sample is collected the sample bag is connected in series with a sorbing apparatus in a recirculation loop. The sorbing apparatus has an inner gas-permeable container containing a sorbent material and an outer gas-impermeable container. The sample is circulated through the outer container and around the inner container for trapping and preconcentrating the contaminants in the sorbent material. The sorbent material may be a liquid having the same composition as the mobile phase of the chromatograph for direct injection thereinto. Alternatively, the sorbent material may be a porous, solid body, to which mobile phase liquid is added after preconcentration of the contaminants for dissolving the contaminants, the liquid solution then being withdrawn for injection into the chromatograph.

  15. Preparation and Characterization of Solid Dispersions of Artemether by Freeze-Dried Method

    Directory of Open Access Journals (Sweden)

    Muhammad Tayyab Ansari

    2015-01-01

    Full Text Available Solid dispersions of artemether and polyethylene glycol 6000 (PEG6000 were prepared in ratio 12 : 88 (group-1. Self-emulsified solid dispersions of artemether were prepared by using polyethylene glycol 6000, Cremophor-A25, olive oil, Transcutol, and hydroxypropyl methylcellulose (HPMC in ratio 12 : 75 : 5 : 4 : 2 : 2, respectively (group-2. In third group, only Cremophor-A25 was replaced with Poloxamer 188 compared to group-2. The solid dispersions and self-emulsified solid dispersions were prepared by physical and freeze dried methods, respectively. All samples were characterized by X-ray diffraction, attenuated total reflectance Fourier transform infrared spectroscopy, differential scanning calorimeter, scanning electron microscopy, and solubility, dissolution, and stability studies. X-ray diffraction pattern revealed artemether complete crystalline, whereas physical mixture and freeze-dried mixture of all three groups showed reduced peak intensities. In attenuated total reflectance Fourier transform infrared spectroscopy spectra, C–H stretching vibrations of artemether were masked in all prepared samples, while C–H stretching vibrations were representative of polyethylene glycol 6000, Cremophor-A25, and Poloxamer 188. Differential scanning calorimetry showed decreased melting endotherm and increased enthalpy change (ΔH in both physical mixture and freeze-dried mixtures of all groups. Scanning electron microscopy of freeze-dried mixtures of all samples showed glassy appearance, size reduction, and embedment, while their physical mixture showed size reduction and embedment of artemether by excipients. In group-1, solubility was improved up to 15 times, whereas group-2 showed up to 121 times increase but, in group-3, when Poloxamer 188 was used instead of Cremophor-A25, solubility of freeze-dried mixtures was increased up to 135 times. In fasted state simulated gastric fluid at pH 1.6, the dissolution of physical

  16. [Respondent-Driven Sampling: a new sampling method to study visible and hidden populations].

    Science.gov (United States)

    Mantecón, Alejandro; Juan, Montse; Calafat, Amador; Becoña, Elisardo; Román, Encarna

    2008-01-01

    The paper introduces a variant of chain-referral sampling: respondent-driven sampling (RDS). This sampling method shows that methods based on network analysis can be combined with the statistical validity of standard probability sampling methods. In this sense, RDS appears to be a mathematical improvement of snowball sampling oriented to the study of hidden populations. However, we try to prove its validity with populations that are not within a sampling frame but can nonetheless be contacted without difficulty. The basics of RDS are explained through our research on young people (aged 14 to 25) who go clubbing, consume alcohol and other drugs, and have sex. Fieldwork was carried out between May and July 2007 in three Spanish regions: Baleares, Galicia and Comunidad Valenciana. The presentation of the study shows the utility of this type of sampling when the population is accessible but there is a difficulty deriving from the lack of a sampling frame. However, the sample obtained is not a random representative one in statistical terms of the target population. It must be acknowledged that the final sample is representative of a 'pseudo-population' that approximates to the target population but is not identical to it.

  17. Calibration of laser ablation inductively coupled plasma mass spectrometry using dried solution aerosols for the quantitative analysis of solid samples

    Energy Technology Data Exchange (ETDEWEB)

    Leach, James [Iowa State Univ., Ames, IA (United States)

    1999-02-12

    Inductively coupled plasma mass spectrometry (ICP-MS) has become the method of choice for elemental and isotopic analysis. Several factors contribute to its success. Modern instruments are capable of routine analysis at part per trillion levels with relative detection limits in part per quadrillion levels. Sensitivities in these instruments can be as high as 200 million counts per second per part per million with linear dynamic ranges up to eight orders of magnitude. With standards for only a few elements, rapid semiquantitative analysis of over 70 elements in an individual sample can be performed. Less than 20 years after its inception ICP-MS has shown to be applicable to several areas of science. These include geochemistry, the nuclear industry, environmental chemistry, clinical chemistry, the semiconductor industry, and forensic chemistry. In this introduction, the general attributes of ICP-MS will be discussed in terms of instrumentation and sample introduction. The advantages and disadvantages of current systems are presented. A detailed description of one method of sample introduction, laser ablation, is given. The paper also gives conclusions and suggestions for future work. Chapter 2, Quantitative analysis of solids by laser ablation inductively coupled plasma mass spectrometry using dried solution aerosols for calibration, has been removed for separate processing.

  18. A random spatial sampling method in a rural developing nation.

    Science.gov (United States)

    Kondo, Michelle C; Bream, Kent D W; Barg, Frances K; Branas, Charles C

    2014-04-10

    Nonrandom sampling of populations in developing nations has limitations and can inaccurately estimate health phenomena, especially among hard-to-reach populations such as rural residents. However, random sampling of rural populations in developing nations can be challenged by incomplete enumeration of the base population. We describe a stratified random sampling method using geographical information system (GIS) software and global positioning system (GPS) technology for application in a health survey in a rural region of Guatemala, as well as a qualitative study of the enumeration process. This method offers an alternative sampling technique that could reduce opportunities for bias in household selection compared to cluster methods. However, its use is subject to issues surrounding survey preparation, technological limitations and in-the-field household selection. Application of this method in remote areas will raise challenges surrounding the boundary delineation process, use and translation of satellite imagery between GIS and GPS, and household selection at each survey point in varying field conditions. This method favors household selection in denser urban areas and in new residential developments. Random spatial sampling methodology can be used to survey a random sample of population in a remote region of a developing nation. Although this method should be further validated and compared with more established methods to determine its utility in social survey applications, it shows promise for use in developing nations with resource-challenged environments where detailed geographic and human census data are less available.

  19. Headspace solid-phase microextraction of halogenated toluenes in environmental aqueous samples with polypropylene microporous membranes.

    Science.gov (United States)

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

    2009-04-03

    The optimization of the polypropylene microporous membrane based solid-phase microextraction (MMSPE) of several halogenated (Cl(-) and Br(-)) toluenes was carried out. The influence of several factors such as sampling mode, sample volume, stirring rate, ionic strength, exposure time, etc. on the performance of the microextraction process was thoroughly investigated. Under optimized conditions, analytes were concentrated onto a 2-cm long membrane exposed to the headspace (HS) of the sample vial containing 80mL of water with a 30% of sodium chloride. Equilibrium was achieved after a sampling period of 1h, at room temperature and vigorous magnetic stirring. After analytes desorption, with just 250 microL of n-hexane, they were determined by gas chromatography with micro-electron capture detection (GC-mu-ECD). The developed methodology was characterized and validated also by gas chromatography-mass spectrometry (GC-MS). The proposed approach presented good precision (RSDs of 6-15% and 2-8% under reproducibility and repeatability conditions, respectively) and linear responses (R(2): 0.990-0.999) over more than two order of magnitude concentration ranges for di- to penta-substituted species either with GC-MS or GC-mu-ECD detection. The absolute extraction efficiency was directly related with the lipophilic nature of the studied species and their volatile character, ranging between 27% and 47% for di- to pentahalotoluenes. Despite being an adsorption based methodology, no matrix effects were observed for complex environmental water matrices such as river water or treated wastewater. The proposed approach provided a very simple and low-cost microextraction alternative rendering adequate limits of quantification, in the low/sub ngL(-1) level, for environmental sample analysis of poly-halogenated toluenes.

  20. Development of a solid-phase extraction coupling chemiluminescent enzyme immunoassay for determination of organophosphorus pesticides in environmental water samples.

    Science.gov (United States)

    Xu, Zhen-Lin; Sun, Wen-Jia; Yang, Jin-Yi; Jiang, Yue-Ming; Campbell, Katrina; Shen, Yu-Dong; Lei, Hong-Tao; Zeng, Dao-Ping; Wang, Hong; Sun, Yuan-Ming

    2012-03-07

    Solid-phase extraction (SPE) and direct competitive chemiluminescence enzyme immunoassay (dcCL-EIA) were combined for the detection of organophosphorus pesticides (OPs) in environmental water samples. dcCL-EIA based on horseradish peroxidase labeled with a broad-specificity monoclonal antibody against OPs was developed, and the effects of several physicochemical parameters on dcCL-EIA performance were studied. SPE was used for the pretreatment of water samples to remove interfering substances and to concentrate the OP analytes. The coupling of SPE and dcCL-EIA can detect seven OPs (parathion, coumaphos, phoxim, quinalphos, triazophos, dichlofenthion, and azinphos-ethyl) with the limit of quantitation below 0.1 ng/mL. The recoveries of OPs from spiked water samples ranged from 62.5% to 131.7% by SPE-dcCL-EIA and 69.5% to 112.3% by SPE-HPLC-MS/MS. The screening of OP residues in real-world environmental water samples by the developed SPE-dcCL-EIA and their confirmatory analysis using SPE-HPLC-MS/MS demonstrated that the assay is ideally suited as a monitoring method for OP residues prior to chromatographic analysis.

  1. A solid phase extraction-ion chromatography with conductivity detection procedure for determining cationic surfactants in surface water samples.

    Science.gov (United States)

    Olkowska, Ewa; Polkowska, Żaneta; Namieśnik, Jacek

    2013-11-15

    A new analytical procedure for the simultaneous determination of individual cationic surfactants (alkyl benzyl dimethyl ammonium chlorides) in surface water samples has been developed. We describe this methodology for the first time: it involves the application of solid phase extraction (SPE-for sample preparation) coupled with ion chromatography-conductivity detection (IC-CD-for the final determination). Mean recoveries of analytes between 79% and 93%, and overall method quantification limits in the range from 0.0018 to 0.038 μg/mL for surface water and CRM samples were achieved. The methodology was applied to the determination of individual alkyl benzyl quaternary ammonium compounds in environmental samples (reservoir water) and enables their presence in such types of waters to be confirmed. In addition, it is a simpler, less time-consuming, labour-intensive, avoiding use of toxic chloroform and significantly less expensive methodology than previously described approaches (liquid-liquid extraction coupled with liquid chromatography-mass spectrometry). Copyright © 2013 Elsevier B.V. All rights reserved.

  2. [Biological Advisory Subcommittee Sampling Methods : Results, Resolutions, and Correspondences : 2002

    Data.gov (United States)

    US Fish and Wildlife Service, Department of the Interior — This document contains a variety of information concerning Biological Advisory Subcommittee sampling methods at the Rocky Mountain Arsenal Refuge in 2002. Multiple...

  3. A cryopreservation method for Pasteurella multocida from wetland samples

    Science.gov (United States)

    Moore, Melody K.; Shadduck, D.J.; Goldberg, D.R.; Samuel, M.D.

    1998-01-01

    A cryopreservation method and improved isolation techniques for detection of Pasteurella multocida from wetland samples were developed. Wetland water samples were collected in the field, diluted in dimethyl sulfoxide (DMSO, final concentration 10%), and frozen at -180 C in a liquid nitrogen vapor shipper. Frozen samples were transported to the laboratory where they were subsequently thawed and processed in Pasteurella multocida selective broth (PMSB) to isolate P. multocida. This method allowed for consistent isolation of 2 to 18 organisms/ml from water seeded with known concentrations of P. multocida. The method compared favorably with the standard mouse inoculation method and allowed for preservation of the samples until they could be processed in the laboratory.

  4. Methods for collection and analysis of water samples

    Science.gov (United States)

    Rainwater, Frank Hays; Thatcher, Leland Lincoln

    1960-01-01

    This manual contains methods used by the U.S. Geological Survey to collect, preserve, and analyze water samples. Throughout, the emphasis is on obtaining analytical results that accurately describe the chemical composition of the water in situ. Among the topics discussed are selection of sampling sites, frequency of sampling, field equipment, preservatives and fixatives, analytical techniques of water analysis, and instruments. Seventy-seven laboratory and field procedures are given for determining fifty-three water properties.

  5. Field evaluation of personal sampling methods for multiple bioaerosols.

    Directory of Open Access Journals (Sweden)

    Chi-Hsun Wang

    Full Text Available Ambient bioaerosols are ubiquitous in the daily environment and can affect health in various ways. However, few studies have been conducted to comprehensively evaluate personal bioaerosol exposure in occupational and indoor environments because of the complex composition of bioaerosols and the lack of standardized sampling/analysis methods. We conducted a study to determine the most efficient collection/analysis method for the personal exposure assessment of multiple bioaerosols. The sampling efficiencies of three filters and four samplers were compared. According to our results, polycarbonate (PC filters had the highest relative efficiency, particularly for bacteria. Side-by-side sampling was conducted to evaluate the three filter samplers (with PC filters and the NIOSH Personal Bioaerosol Cyclone Sampler. According to the results, the Button Aerosol Sampler and the IOM Inhalable Dust Sampler had the highest relative efficiencies for fungi and bacteria, followed by the NIOSH sampler. Personal sampling was performed in a pig farm to assess occupational bioaerosol exposure and to evaluate the sampling/analysis methods. The Button and IOM samplers yielded a similar performance for personal bioaerosol sampling at the pig farm. However, the Button sampler is more likely to be clogged at high airborne dust concentrations because of its higher flow rate (4 L/min. Therefore, the IOM sampler is a more appropriate choice for performing personal sampling in environments with high dust levels. In summary, the Button and IOM samplers with PC filters are efficient sampling/analysis methods for the personal exposure assessment of multiple bioaerosols.

  6. Adaptive cluster sampling: An efficient method for assessing inconspicuous species

    Science.gov (United States)

    Andrea M. Silletti; Joan Walker

    2003-01-01

    Restorationistis typically evaluate the success of a project by estimating the population sizes of species that have been planted or seeded. Because total census is raely feasible, they must rely on sampling methods for population estimates. However, traditional random sampling designs may be inefficient for species that, for one reason or another, are challenging to...

  7. Effective phospholipid removal from plasma samples by solid phase extraction with the use of copper (II) modified silica gel cartridges.

    Science.gov (United States)

    Flieger, Jolanta; Tatarczak-Michalewska, Małgorzata; Kowalska, Anna; Madejska, Anna; Śniegocki, Tomasz; Sroka-Bartnicka, Anna; Szymańska-Chargot, Monika

    2017-12-01

    The new sorbent for solid phase extraction (SPE), based on silica gel modified with a copper (II), was obtained and its application for phospholipids removal from the human plasma was tested. SPE column conditioning requirements, the volume of the plasma, the composition of the elution solvent were all established. The efficacy of the removal of phospholipids was compared for different methods such as standard protein precipitation or HybridSPE Phospholipid Ultra and HybridSPE-PPT. The sample clean-up was verified by mass spectrometry (MS) and by monitoring of chromatograms in the region between 190nm and 400nm. The Fourier Transform Infrared Spectroscopy FT-IR and confocal Raman microscopy were used to evaluating the silica gel modifications and to show the structure of lipids confined in the silica pores. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Band structure computation of polygonal solid-solid phononic crystal with features using frequency domain spectral superelement method

    Science.gov (United States)

    Mukherjee, Sushovan; Gopalakrishnan, S.

    2017-04-01

    Phononic crystals are synthetic materials with a periodic structure having spatial variations of elasto-inertial properties of constituent materials, aimed at developing devices and bulk material with engineered acoustic/ elastic properties. Multi-material structures with sides of a space filling polygonal tessellation, can constitute solid-solid phononic crystal. Coupled with inclusions and features, phononic crystals show rich and varied band structure phenomenon. We use frequency domain spectral superelement method and Bloch theory to efficiently calculate the band structures of such phononic crystals. We particularly investigate hexagonal honeycombs to assess the impacts of joint elasticity, inertia and circular and elliptical holes on band gap behavior.

  9. Direct determination of chromium in infant formulas employing high-resolution continuum source electrothermal atomic absorption spectrometry and solid sample analysis.

    Science.gov (United States)

    Silva, Arlene S; Brandao, Geovani C; Matos, Geraldo D; Ferreira, Sergio L C

    2015-11-01

    The present work proposed an analytical method for the direct determination of chromium in infant formulas employing the high-resolution continuum source electrothermal atomic absorption spectrometry combined with the solid sample analysis (SS-HR-CS ET AAS). Sample masses up to 2.0mg were directly weighted on a solid sampling platform and introduced into the graphite tube. In order to minimize the formation of carbonaceous residues and to improve the contact of the modifier solution with the solid sample, a volume of 10 µL of a solution containing 6% (v/v) H2O2, 20% (v/v) ethanol and 1% (v/v) HNO3 was added. The pyrolysis and atomization temperatures established were 1600 and 2400 °C, respectively, using magnesium as chemical modifier. The calibration technique was evaluated by comparing the slopes of calibration curves established using aqueous and solid standards. This test revealed that chromium can be determined employing the external calibration technique using aqueous standards. Under these conditions, the method developed allows the direct determination of chromium with limit of quantification of 11.5 ng g(-1), precision expressed as relative standard deviation (RSD) in the range of 4.0-17.9% (n=3) and a characteristic mass of 1.2 pg of chromium. The accuracy was confirmed by analysis of a certified reference material of tomato leaves furnished by National Institute of Standards and Technology. The method proposed was applied for the determination of chromium in five different infant formula samples. The chromium content found varied in the range of 33.9-58.1 ng g(-1) (n=3). These samples were also analyzed employing ICP-MS. A statistical test demonstrated that there is no significant difference between the results found by two methods. The chromium concentrations achieved are lower than the maximum limit permissible for chromium in foods by Brazilian Legislation. Copyright © 2015. Published by Elsevier B.V.

  10. Gold nanoparticles based solid-phase microextraction coatings for determining organochlorine pesticides in aqueous environmental samples.

    Science.gov (United States)

    Gutiérrez-Serpa, Adrián; Rocío-Bautista, Priscilla; Pino, Verónica; Jiménez-Moreno, Francisco; Jiménez-Abizanda, Ana I

    2017-05-01

    The use of solid-phase microextraction coatings based on gold nanoparticles was investigated, focusing the attention on the preparation of nanoparticles with nonclassical reduction agents of HAuCl4 such as gallic acid and H2 O2 , rather than the conventional sodium citrate. All nanoparticles were characterized by diode array spectroscopy, whereas novel nanoparticles prepared with gallic acid and H2 O2 were also characterized by microscopic techniques. Solid-phase microextraction coatings were prepared with a layer-by-layer approach. Gallic acid permitted the preparation of stable nanoparticles with milder experimental conditions (1 min, room temperature) and provided the most uniform coatings (thickness ∼3 μm). Seven organochlorine pesticides were determined in different environmental waters using gas chromatography with electron capture detection. Despite the low thickness of the coatings, limits of detection of the entire method down to 0.13 μg/L were obtained. A comparison with the commercial polyacrylate in terms of the partition coefficients of the analytes to the coatings gave logarithm of the partition coefficient values two times higher with gallic acid than polyacrylate (although the commercial fiber is 28 times thicker). Interfiber relative standard deviation values ranged from 8.67 to 21.3%. Optimum fibers also presented an adequate lifetime (>100 extractions). © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Blood plasma sample preparation method to determine thyroid hormone-disrupting compounds in Effect-Directed Analysis

    NARCIS (Netherlands)

    Simon, E.; Bytingsvik, J.; Jonker, W.; Leonards, P.E.G.; de Boer, J.; Jenssen, B.M.; Lie, E.; Aars, J.; Hamers, T.H.M.; Lamoree, M.H.

    2011-01-01

    A sample preparation method combining solid-phase extraction (SPE) and liquid-liquid extraction (LLE) was developed to be used in Effect-Directed Analysis (EDA) of blood plasma. Until now such a method was not available. It can be used for extraction of a broad range of thyroid hormone

  12. DOE methods for evaluating environmental and waste management samples

    Energy Technology Data Exchange (ETDEWEB)

    Goheen, S.C.; McCulloch, M.; Thomas, B.L.; Riley, R.G.; Sklarew, D.S.; Mong, G.M.; Fadeff, S.K. [eds.

    1994-10-01

    DOE Methods for Evaluating Environmental and Waste Management Samples (DOE Methods) is a resource intended to support sampling and analytical activities for the evaluation of environmental and waste management samples from U.S. Department of Energy (DOE) sites. DOE Methods is the result of extensive cooperation from all DOE analytical laboratories. All of these laboratories have contributed key information and provided technical reviews as well as significant moral support leading to the success of this document. DOE Methods is designed to encompass methods for collecting representative samples and for determining the radioisotope activity and organic and inorganic composition of a sample. These determinations will aid in defining the type and breadth of contamination and thus determine the extent of environmental restoration or waste management actions needed, as defined by the DOE, the U.S. Environmental Protection Agency, or others. The development of DOE Methods is supported by the Analytical Services Division of DOE. Unique methods or methods consolidated from similar procedures in the DOE Procedures Database are selected for potential inclusion in this document. Initial selection is based largely on DOE needs and procedure applicability and completeness. Methods appearing in this document are one of two types, {open_quotes}Draft{close_quotes} or {open_quotes}Verified{close_quotes}. {open_quotes}Draft{close_quotes} methods that have been reviewed internally and show potential for eventual verification are included in this document, but they have not been reviewed externally, and their precision and bias may not be known. {open_quotes}Verified{close_quotes} methods in DOE Methods have been reviewed by volunteers from various DOE sites and private corporations. These methods have delineated measures of precision and accuracy.

  13. Structural, Optical, and Magnetic Properties of Co Doped CdTe Alloy Powders Prepared by Solid-State Reaction Method

    Directory of Open Access Journals (Sweden)

    M. Rigana Begam

    2013-01-01

    Full Text Available Co doped CdTe powder samples were prepared by solid-state reaction method. In the present work effect of Co doping on structural, optical, and magnetic properties has been studied. X-ray diffraction studies confirm zinc blend structure for all the samples. The lattice parameter showed linear increase with the increase in Co content. The elemental constituents were characterized by EDAX. Optical studies showed the increase in band gap with increase in Co level. The samples were diluted magnetic semiconductors and exhibited clear hysteresis loop showing room temperature ferromagnetism as confirmed by vibrating sample magnetometer.

  14. Method and sample spinning apparatus for measuring the NMR spectrum of an orientationally disordered sample

    Science.gov (United States)

    Pines, Alexander; Samoson, Ago

    1990-01-01

    An improved NMR apparatus and method are described which substantially improve the resolution of NMR measurements made on powdered or amorphous or otherwise orientationally disordered samples. The apparatus spins the sample about an axis. The angle of the axis is mechanically varied such that the time average of two or more Legendre polynomials are zero.

  15. Selective solid-phase extraction using molecularly imprinted polymer as a sorbent for the analysis of fenarimol in food samples.

    Science.gov (United States)

    Khan, Shagufta; Bhatia, Tejasvi; Trivedi, Purushottam; Satyanarayana, G N V; Mandrah, Kapil; Saxena, Prem Narayan; Mudiam, Mohana Krishna Reddy; Roy, Somendu Kumar

    2016-05-15

    In the present communication, a non-covalent fenarimol-imprinted polymer was synthesized by precipitation polymerization technique using methacrylic acid (MAA) as a functional monomer, ethylene glycol dimethacrylate (EGDMA) as a cross-linker, and azobisisobutyronitrile (AIBN) as an initiator in different porogenic solvent. Binding study of molecularly imprinted and non-imprinted polymer (MIP and NIP) showed that MIP possesses a higher affinity towards this analyte compared to NIP. The binding affinity of MIP was calculated by static and kinetic adsorption study. Further, a MIP based cartridge was designed to use in extraction process, necessary for specific determination and quantification of the fungicide in food matrices. Under the optimum conditions, developed method was found to be linear (R(2)=0.9999-0.9994). Limit of detection (LOD) and limit of quantitation (LOQ) in samples were 0.03-0.06 and 0.12-0.21 μg mL(-1), respectively. The rate of recovery of fenarimol was 91.16-99.52% on MIPs. The validated method of molecularly imprinted solid-phase extraction (MISPE) cartridge was successfully applied to the food matrices and compared with commercial sorbent (RP18 and Oasis HLB). However we feel, this method has promising applications in the routine analysis of food samples in industry. Copyright © 2015 Elsevier Ltd. All rights reserved.

  16. Methods for sample size determination in cluster randomized trials.

    Science.gov (United States)

    Rutterford, Clare; Copas, Andrew; Eldridge, Sandra

    2015-06-01

    The use of cluster randomized trials (CRTs) is increasing, along with the variety in their design and analysis. The simplest approach for their sample size calculation is to calculate the sample size assuming individual randomization and inflate this by a design effect to account for randomization by cluster. The assumptions of a simple design effect may not always be met; alternative or more complicated approaches are required. We summarise a wide range of sample size methods available for cluster randomized trials. For those familiar with sample size calculations for individually randomized trials but with less experience in the clustered case, this manuscript provides formulae for a wide range of scenarios with associated explanation and recommendations. For those with more experience, comprehensive summaries are provided that allow quick identification of methods for a given design, outcome and analysis method. We present first those methods applicable to the simplest two-arm, parallel group, completely randomized design followed by methods that incorporate deviations from this design such as: variability in cluster sizes; attrition; non-compliance; or the inclusion of baseline covariates or repeated measures. The paper concludes with methods for alternative designs. There is a large amount of methodology available for sample size calculations in CRTs. This paper gives the most comprehensive description of published methodology for sample size calculation and provides an important resource for those designing these trials. © The Author 2015. Published by Oxford University Press on behalf of the International Epidemiological Association.

  17. Matrix solid phase dispersion method for determination of polycyclic aromatic hydrocarbons in moss.

    Science.gov (United States)

    Concha-Graña, Estefanía; Muniategui-Lorenzo, Soledad; De Nicola, Flavia; Aboal, Jesús R; Rey-Asensio, Ana Isabel; Giordano, Simonetta; Reski, Ralf; López-Mahía, Purificación; Prada-Rodríguez, Darío

    2015-08-07

    In this work a matrix solid-phase dispersion extraction method, followed by programmed temperature vaporization-gas chromatography-tandem mass spectrometry determination is proposed for the analysis of polycyclic aromatic hydrocarbons (PAHs) in moss samples. A devitalized, cultivated Sphagnum palustre L. moss clone obtained from the "Mossclone" EU-FP7 Project was used for the optimization and validation of the proposed method. Good trueness (84-116%), precision (intermediate precision lower than 11%) and sensitivity (quantitation limits lower than 1.7ngg(-1)) were obtained. The proposed method was compared with other procedures applied for this complex matrix, achieving a considerable reduction of sample amount, solvent volume and time consumption. The procedure was successfully tested for the analysis of PAHs in exposed moss clone samples for the monitoring of air pollution. Finally, the method was also tested for its suitability in the analysis of PAHs in other moss species as well as a lichen species. Copyright © 2015 Elsevier B.V. All rights reserved.

  18. System and method for measuring fluorescence of a sample

    Energy Technology Data Exchange (ETDEWEB)

    Riot, Vincent J.

    2017-06-27

    The present disclosure provides a system and a method for measuring fluorescence of a sample. The sample may be a polymerase-chain-reaction (PCR) array, a loop-mediated-isothermal amplification array, etc. LEDs are used to excite the sample, and a photodiode is used to collect the sample's fluorescence. An electronic offset signal is used to reduce the effects of background fluorescence and the noises from the measurement system. An integrator integrates the difference between the output of the photodiode and the electronic offset signal over a given period of time. The resulting integral is then converted into digital domain for further processing and storage.

  19. Soil separator and sampler and method of sampling

    Science.gov (United States)

    O'Brien, Barry H [Idaho Falls, ID; Ritter, Paul D [Idaho Falls, ID

    2010-02-16

    A soil sampler includes a fluidized bed for receiving a soil sample. The fluidized bed may be in communication with a vacuum for drawing air through the fluidized bed and suspending particulate matter of the soil sample in the air. In a method of sampling, the air may be drawn across a filter, separating the particulate matter. Optionally, a baffle or a cyclone may be included within the fluidized bed for disentrainment, or dedusting, so only the finest particulate matter, including asbestos, will be trapped on the filter. The filter may be removable, and may be tested to determine the content of asbestos and other hazardous particulate matter in the soil sample.

  20. System and method for measuring fluorescence of a sample

    Science.gov (United States)

    Riot, Vincent J

    2015-03-24

    The present disclosure provides a system and a method for measuring fluorescence of a sample. The sample may be a polymerase-chain-reaction (PCR) array, a loop-mediated-isothermal amplification array, etc. LEDs are used to excite the sample, and a photodiode is used to collect the sample's fluorescence. An electronic offset signal is used to reduce the effects of background fluorescence and the noises from the measurement system. An integrator integrates the difference between the output of the photodiode and the electronic offset signal over a given period of time. The resulting integral is then converted into digital domain for further processing and storage.

  1. Modified Sample Preparation Approach for the Determination of the Phenolic and Humic-Like Substances in Natural Organic Materials By the Folin Ciocalteu Method.

    Science.gov (United States)

    Pontoni, Ludovico; Panico, Antonio; Matanò, Alessia; van Hullebusch, Eric D; Fabbricino, Massimiliano; Esposito, Giovanni; Pirozzi, Francesco

    2017-12-06

    A novel modification of the sample preparation procedure for the Folin-Ciocalteu colorimetric assay for the determination of total phenolic compounds in natural solid and semisolid organic materials (e.g., foods, organic solid waste, soils, plant tissues, agricultural residues, manure) is proposed. In this method, the sample is prepared by adding sodium sulfate as a solid diluting agent before homogenization. The method allows for the determination of total phenols (TP) in samples with high solids contents, and it provides good accuracy and reproducibility. Additionally, this method permits analyses of significant amounts of sample, which reduces problems related to heterogeneity. We applied this method to phenols-rich lignocellulosic and humic-like solids and semisolid samples, including rice straw (RS), peat-rich soil (PS), and food waste (FW). The TP concentrations measured with the solid dilution (SD) preparation were substantially higher (increases of 41.4%, 15.5%, and 59.4% in RS, PS and FW, respectively) than those obtained with the traditional method (solids suspended in water). These results showed that the traditional method underestimates the phenolic contents in the studied solids.

  2. Using re-sampling methods in mortality studies.

    Directory of Open Access Journals (Sweden)

    Igor Itskovich

    Full Text Available Traditional methods of computing standardized mortality ratios (SMR in mortality studies rely upon a number of conventional statistical propositions to estimate confidence intervals for obtained values. Those propositions include a common but arbitrary choice of the confidence level and the assumption that observed number of deaths in the test sample is a purely random quantity. The latter assumption may not be fully justified for a series of periodic "overlapping" studies. We propose a new approach to evaluating the SMR, along with its confidence interval, based on a simple re-sampling technique. The proposed method is most straightforward and requires neither the use of above assumptions nor any rigorous technique, employed by modern re-sampling theory, for selection of a sample set. Instead, we include all possible samples that correspond to the specified time window of the study in the re-sampling analysis. As a result, directly obtained confidence intervals for repeated overlapping studies may be tighter than those yielded by conventional methods. The proposed method is illustrated by evaluating mortality due to a hypothetical risk factor in a life insurance cohort. With this method used, the SMR values can be forecast more precisely than when using the traditional approach. As a result, the appropriate risk assessment would have smaller uncertainties.

  3. Heat-capacity measurements on small samples: The hybrid method

    NARCIS (Netherlands)

    Klaasse, J.C.P.; Brück, E.H.

    2008-01-01

    A newly developed method is presented for measuring heat capacities on small samples, particularly where thermal isolation is not sufficient for the use of the traditional semiadiabatic heat-pulse technique. This "hybrid technique" is a modification of this heat-pulse method in case the temperature

  4. Method of determining an electrical property of a test sample

    DEFF Research Database (Denmark)

    2010-01-01

    A method of obtaining an electrical property of a test sample, comprising a non-conductive area and a conductive or semi-conductive test area, byperforming multiple measurements using a multi-point probe. The method comprising the steps of providing a magnetic field having field lines passing...... the electrical property of the test area....

  5. Efficiency of snake sampling methods in the Brazilian semiarid region.

    Science.gov (United States)

    Mesquita, Paula C M D; Passos, Daniel C; Cechin, Sonia Z

    2013-09-01

    The choice of sampling methods is a crucial step in every field survey in herpetology. In countries where time and financial support are limited, the choice of the methods is critical. The methods used to sample snakes often lack objective criteria, and the traditional methods have apparently been more important when making the choice. Consequently researches using not-standardized methods are frequently found in the literature. We have compared four commonly used methods for sampling snake assemblages in a semiarid area in Brazil. We compared the efficacy of each method based on the cost-benefit regarding the number of individuals and species captured, time, and financial investment. We found that pitfall traps were the less effective method in all aspects that were evaluated and it was not complementary to the other methods in terms of abundance of species and assemblage structure. We conclude that methods can only be considered complementary if they are standardized to the objectives of the study. The use of pitfall traps in short-term surveys of the snake fauna in areas with shrubby vegetation and stony soil is not recommended.

  6. A multi-dimensional sampling method for locating small scatterers

    Science.gov (United States)

    Song, Rencheng; Zhong, Yu; Chen, Xudong

    2012-11-01

    A multiple signal classification (MUSIC)-like multi-dimensional sampling method (MDSM) is introduced to locate small three-dimensional scatterers using electromagnetic waves. The indicator is built with the most stable part of signal subspace of the multi-static response matrix on a set of combinatorial sampling nodes inside the domain of interest. It has two main advantages compared to the conventional MUSIC methods. First, the MDSM is more robust against noise. Second, it can work with a single incidence even for multi-scatterers. Numerical simulations are presented to show the good performance of the proposed method.

  7. Advanced Markov chain Monte Carlo methods learning from past samples

    CERN Document Server

    Liang, Faming; Carrol, Raymond J

    2010-01-01

    This book provides comprehensive coverage of simulation of complex systems using Monte Carlo methods. Developing algorithms that are immune to the local trap problem has long been considered as the most important topic in MCMC research. Various advanced MCMC algorithms which address this problem have been developed include, the modified Gibbs sampler, the methods based on auxiliary variables and the methods making use of past samples. The focus of this book is on the algorithms that make use of past samples. This book includes the multicanonical algorithm, dynamic weighting, dynamically weight

  8. Novel materials and methods for solid-phase extraction and liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Ambrose, Diana [Iowa State Univ., Ames, IA (United States)

    1997-06-24

    This report contains a general introduction which discusses solid-phase extraction and solid-phase micro-extraction as sample preparation techniques for high-performance liquid chromatography, which is also evaluated in the study. This report also contains the Conclusions section. Four sections have been removed and processed separately: silicalite as a sorbent for solid-phase extraction; a new, high-capacity carboxylic acid functionalized resin for solid-phase extraction; semi-micro solid-phase extraction of organic compounds from aqueous and biological samples; and the high-performance liquid chromatographic determination of drugs and metabolites in human serum and urine using direct injection and a unique molecular sieve.

  9. An analytical protocol for the determination of total mercury concentrations in solid peat samples

    DEFF Research Database (Denmark)

    Roos-Barraclough, F; Givelet, N; Martinez-Cortizas, A

    2002-01-01

    Traditional peat sample preparation methods such as drying at high temperatures and milling may be unsuitable for Hg concentration determination in peats due to the possible presence of volatile Hg species, which could be lost during drying. Here, the effects of sample preparation and natural....... A comparison of two Hg profiles from an Arctic peat core, measured in frozen samples and in air-dried samples, revealed that no Hg losses occurred upon air-drying. A comparison of Hg concentrations in several plant species that make up peat, showed that some species (Pinus mugo, Sphagnum recurvum...... concentration in individual peat slices. Several subsamples from each peat slice are air dried, combined and measured for Hg using the AMA254, using a program of 30 s (drying), 125 s (decomposition) and 45 s (waiting). Bulk density and water content measurements are performed on every slice using separate...

  10. Preparation of Biological Samples Containing Metoprolol and Bisoprolol for Applying Methods for Quantitative Analysis

    Directory of Open Access Journals (Sweden)

    Corina Mahu Ştefania

    2015-12-01

    Full Text Available Arterial hypertension is a complex disease with many serious complications, representing a leading cause of mortality. Selective beta-blockers such as metoprolol and bisoprolol are frequently used in the management of hypertension. Numerous analytical methods have been developed for the determination of these substances in biological fluids, such as liquid chromatography coupled with mass spectrometry, gas chromatography coupled with mass spectrometry, high performance liquid chromatography. Due to the complex composition of biological fluids a biological sample pre-treatment before the use of the method for quantitative determination is required in order to remove proteins and potential interferences. The most commonly used methods for processing biological samples containing metoprolol and bisoprolol were identified through a thorough literature search using PubMed, ScienceDirect, and Willey Journals databases. Articles published between years 2005-2015 were reviewed. Protein precipitation, liquid-liquid extraction and solid phase extraction are the main techniques for the extraction of these drugs from plasma, serum, whole blood and urine samples. In addition, numerous other techniques have been developed for the preparation of biological samples, such as dispersive liquid-liquid microextraction, carrier-mediated liquid phase microextraction, hollow fiber-protected liquid phase microextraction, on-line molecularly imprinted solid phase extraction. The analysis of metoprolol and bisoprolol in human plasma, urine and other biological fluids provides important information in clinical and toxicological trials, thus requiring the application of appropriate extraction techniques for the detection of these antihypertensive substances at nanogram and picogram levels.

  11. Experimental Protocol for Detecting Cyanobacteria in Liquid and Solid Samples with an Antibody Microarray Chip.

    Science.gov (United States)

    Blanco, Yolanda; Moreno-Paz, Mercedes; Parro, Victor

    2017-02-07

    Global warming and eutrophication make some aquatic ecosystems behave as true bioreactors that trigger rapid and massive cyanobacterial growth; this has relevant health and economic consequences. Many cyanobacterial strains are toxin producers, and only a few cells are necessary to induce irreparable damage to the environment. Therefore, water-body authorities and administrations require rapid and efficient early-warning systems providing reliable data to support their preventive or curative decisions. This manuscript reports an experimental protocol for the in-field detection of toxin-producing cyanobacterial strains by using an antibody microarray chip with 17 antibodies (Abs) with taxonomic resolution (CYANOCHIP). Here, a multiplex fluorescent sandwich microarray immunoassay (FSMI) for the simultaneous monitoring of 17 cyanobacterial strains frequently found blooming in freshwater ecosystems, some of them toxin producers, is described. A microarray with multiple identical replicates (up to 24) of the CYANOCHIP was printed onto a single microscope slide to simultaneously test a similar number of samples. Liquid samples can be tested either by direct incubation with the antibodies (Abs) or after cell concentration by filtration through a 1- to 3-μm filter. Solid samples, such as sediments and ground rocks, are first homogenized and dispersed by a hand-held ultrasonicator in an incubation buffer. They are then filtered (5 - 20 μm) to remove the coarse material, and the filtrate is incubated with Abs. Immunoreactions are revealed by a final incubation with a mixture of the 17 fluorescence-labeled Abs and are read by a portable fluorescence detector. The whole process takes around 3 h, most of it corresponding to two 1-h periods of incubation. The output is an image, where bright spots correspond to the positive detection of cyanobacterial markers.

  12. Sample size formulae for the Bayesian continual reassessment method.

    Science.gov (United States)

    Cheung, Ying Kuen

    2013-01-01

    In the planning of a dose finding study, a primary design objective is to maintain high accuracy in terms of the probability of selecting the maximum tolerated dose. While numerous dose finding methods have been proposed in the literature, concrete guidance on sample size determination is lacking. With a motivation to provide quick and easy calculations during trial planning, we present closed form formulae for sample size determination associated with the use of the Bayesian continual reassessment method (CRM). We examine the sampling distribution of a nonparametric optimal design and exploit it as a proxy to empirically derive an accuracy index of the CRM using linear regression. We apply the formulae to determine the sample size of a phase I trial of PTEN-long in pancreatic cancer patients and demonstrate that the formulae give results very similar to simulation. The formulae are implemented by an R function 'getn' in the package 'dfcrm'. The results are developed for the Bayesian CRM and should be validated by simulation when used for other dose finding methods. The analytical formulae we propose give quick and accurate approximation of the required sample size for the CRM. The approach used to derive the formulae can be applied to obtain sample size formulae for other dose finding methods.

  13. Comparison of Column Solid-Phase Extraction Procedures for Spectrophotometric Determination of E129 (Allura Red) in Foodstuff, Pharmaceutical, and Energy Drink Samples.

    Science.gov (United States)

    Bişgin, Abdullah Taner; Uçan, Mustafa; Narin, İbrahim

    2015-01-01

    Two novel spectrophotometric determination procedures based on retention of Allura Red onto Amberlite XAD-1180 and XAD-16 resins for its preconcentration, purification, and separation were developed. Analytical parameters of the methods including pH, eluent type, sample volume, and sample and eluent flow rates, were investigated and optimized. Interference effects of some cations, anions, and widely used food dyes were also investigated. Detection limits of the two methods were found to be 1.2 and 1.5 μg/L for XAD-1180 and XAD-16 columns, respectively, under optimum conditions. Linear calibration curve ranges of the methods were 0.4-8.0 and 0.5-6.0 μg/mL of Allura Red for XAD-1180 and XAD-16 resins, respectively. Preconcentration factors were found as 80 for both the XAD-1180 and XAD-16 columns using maximum sample volume and minimum eluent volume. RSDs of the methods were below 6% throughout all experiments. All absorbance measurements were performed at 506 nm. Validations of the methods were performed comparatively with determination of the Allura Red contents of some foodstuff, pharmaceutical, and energy drink samples. Allura Red concentrations in investigated solid and liquid samples ranged from 298 to 501 μg/g and 53.8 to 508 μg/mL, respectively. Satisfactory results were obtained from the real samples analysis. Allura Red contents of samples were determined to be highly similar using the two extraction methods. Comparisons of the methods were performed by analysis of Allura Red contents of the real samples. In addition to analytical parameters, adsorption isotherm studies were performed for the two kinds of Amberlite resins. It was observed that developed methods fit the linear form of the Freundlich adsorption isotherm model. All of the experimental results suggested that the developed SPE procedures are suitable for separation, preconcentration, and determination of Allura Red in solid and liquid matrixes.

  14. Development of solid materials for UF6 sampling: FY16 Annual Report

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Nicholas [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Savina, Joseph [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Hebden, Andrew [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division

    2016-10-31

    A handheld implementation of the ABACC-developed Cristallini method, which captures uranium hexafluoride samples as an inert salt, was organized in FY17 and succeeded in demonstrating the handheld sampler concept with reactive hexafluoride gases. The Cristallini method relies on the use of a hydrated substrate to react the incoming hexafluoride resulting in the formation of a stable uranyl fluoride salt. The Cristallini method has been demonstrated as a facility modification installed near the sampling tap of a gas centrifuge enrichment plant. While very successful in reducing the hazards of uranium hexafluoride sample, the method still takes a considerable amount of time and can only be used in facilities where the apparatus has been installed; this arrangement generally prohibits the sampling of filled cylinders that have already exited the facility and have been deposited in the on-site tank storage yard. The handheld unit under development will allow the use of the Cristallini method at facilities that have not been converted as well as tanks in the storage yard. The handheld system utilizes an active vacuum system, rather than a passive vacuum system in the facility setup, to drive the uranium hexafluoride onto the adsorbing media. The handheld unit will be battery operated for fully autonomous operation and will include onboard pressure sensing and flushing capability. To date, the system concept of operations was demonstrated with tungsten hexafluoride that showed the active vacuum pump with multiple cartridges of adsorbing media was viable. Concurrently, the hardened prototype system was developed and tested; removable sample cartridges were developed (the only non-COTS component to date); and preparations were made for uranium tests and a domestic field test.

  15. Determination of MS-222 in Water Samples by Solid-phase Extraction Coupled with Liquid Chromatography/Tandem Mass Spectrometry.

    Science.gov (United States)

    Zhao, Dong-Hao; Wang, Qiang; Wang, Xu-Feng; Li, Zhi-Guang; Li, Yong-Xian; Huang, Ke; Li, Liu-Dong

    2017-09-01

    A practical solid-phase extraction (SPE) method coupled with liquid chromatography/tandem mass spectrometry (LC-MS/MS) has been developed for the determination of the fish anesthetic MS-222 in water. Water samples were concentrated and purified using three SPE cartridges of different specifications. Elution curves of MS-222 were constructed using various methanol-water solutions on the different cartridges, and SPE conditions were optimized in accordance with the elution curves. The mobile phase containing methanol and 0.1% formic acid solution with a linear gradient elution was utilized to separate MS-222 on a C18 column. Detection was carried out by a triple-quadrupole mass spectrometry with an electrospray ion source in positive mode. Recoveries of three MS-222 fortified levels of 0.05, 0.5 and 5 μg/L ranged of 82.6-101% with relative standard deviations (RSDs) below 9.36%. The limit of detection (LOD) and limit of quantification (LOQ) of MS-222 were 0.01 μg/L and 0.03 μg/L, respectively. This method was satisfactorily applied to the determination of MS-222 in actual water samples collected from aquatic product transportation vehicles or from the natural water catchments. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  16. Rapid determination of 54 pharmaceutical and personal care products in fish samples using microwave-assisted extraction-Hollow fiber-Liquid/solid phase microextraction.

    Science.gov (United States)

    Zhang, Yi; Guo, Wen; Yue, Zhenfeng; Lin, Li; Zhao, Fengjuan; Chen, Peijin; Wu, Weidong; Zhu, Hong; Yang, Bo; Kuang, Yanyun; Wang, Jiong

    2017-04-15

    In this paper, a simple, rapid, solvent-less and environmental friendliness microextraction method, microwave-assisted extraction-hollow fiber-liquid/solid phase microextraction (MAE-HF-L/SME), was developed for simultaneous extraction and enrichment of 54 trace hydrophilic/lipophilic pharmaceutical and personal care products (PPCPs) from fish samples. A solid-phase extraction material, solid-phase microextraction (SPME) fiber, was synthesized. The SPME fiber had a homogeneous, loose structure and good mechanical properties, and they exhibited a good adsorption capacity for most PPCPs selected. The material formed the basis for the method of MAE-HF-L/SME. A method of liquid chromatography-high resolution mass spectroscopy (LC-HRMS) for analysis of 54 PPCPs. Under optimal synthesis and extraction conditions, the limits of detection (LODs, n=3) and the limits of quantitation (LOQs, n=10) for the 54 PPCPs were between 0.01-0.50μg·kg-1 and 0.052.00μg·kg-1, respectively. Percent recoveries and the relative standard deviations (RSDs) in spiked fish samples (n=6) were between 56.3%-119.9% and 0.3%-17.1%, respectively. The microextraction process of 54 PPCPs in MAE-HF-L/SME took approximately 12min. The method has a low matrix interference and high enrichment factor and may be applicable for determination of 54 different PPCPs in fish samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Quantitative methods for compensation of matrix effects and self-absorption in LIBS signals of solids

    Science.gov (United States)

    Takahashi, Tomoko; Thornton, Blair

    2017-12-01

    This paper reviews methods to compensate for matrix effects and self-absorption during quantitative analysis of compositions of solids measured using Laser Induced Breakdown Spectroscopy (LIBS) and their applications to in-situ analysis. Methods to reduce matrix and self-absorption effects on calibration curves are first introduced. The conditions where calibration curves are applicable to quantification of compositions of solid samples and their limitations are discussed. While calibration-free LIBS (CF-LIBS), which corrects matrix effects theoretically based on the Boltzmann distribution law and Saha equation, has been applied in a number of studies, requirements need to be satisfied for the calculation of chemical compositions to be valid. Also, peaks of all elements contained in the target need to be detected, which is a bottleneck for in-situ analysis of unknown materials. Multivariate analysis techniques are gaining momentum in LIBS analysis. Among the available techniques, principal component regression (PCR) analysis and partial least squares (PLS) regression analysis, which can extract related information to compositions from all spectral data, are widely established methods and have been applied to various fields including in-situ applications in air and for planetary explorations. Artificial neural networks (ANNs), where non-linear effects can be modelled, have also been investigated as a quantitative method and their applications are introduced. The ability to make quantitative estimates based on LIBS signals is seen as a key element for the technique to gain wider acceptance as an analytical method, especially in in-situ applications. In order to accelerate this process, it is recommended that the accuracy should be described using common figures of merit which express the overall normalised accuracy, such as the normalised root mean square errors (NRMSEs), when comparing the accuracy obtained from different setups and analytical methods.

  18. Time-weighted average sampling of airborne propylene glycol ethers by a solid-phase microextraction device.

    Science.gov (United States)

    Shih, H C; Tsai, S W; Kuo, C H

    2012-01-01

    A solid-phase microextraction (SPME) device was used as a diffusive sampler for airborne propylene glycol ethers (PGEs), including propylene glycol monomethyl ether (PGME), propylene glycol monomethyl ether acetate (PGMEA), and dipropylene glycol monomethyl ether (DPGME). Carboxen-polydimethylsiloxane (CAR/PDMS) SPME fiber was selected for this study. A polytetrafluoroethylene (PTFE) tubing was used as the holder, and the SPME fiber assembly was inserted into the tubing as a diffusive sampler. The diffusion path length and area of the sampler were 0.3 cm and 0.00086 cm(2), respectively. The theoretical sampling constants at 30°C and 1 atm for PGME, PGMEA, and DPGME were 1.50 × 10(-2), 1.23 × 10(-2) and 1.14 × 10(-2) cm(3) min(-1), respectively. For evaluations, known concentrations of PGEs around the threshold limit values/time-weighted average with specific relative humidities (10% and 80%) were generated both by the air bag method and the dynamic generation system, while 15, 30, 60, 120, and 240 min were selected as the time periods for vapor exposures. Comparisons of the SPME diffusive sampling method to Occupational Safety and Health Administration (OSHA) organic Method 99 were performed side-by-side in an exposure chamber at 30°C for PGME. A gas chromatography/flame ionization detector (GC/FID) was used for sample analysis. The experimental sampling constants of the sampler at 30°C were (6.93 ± 0.12) × 10(-1), (4.72 ± 0.03) × 10(-1), and (3.29 ± 0.20) × 10(-1) cm(3) min(-1) for PGME, PGMEA, and DPGME, respectively. The adsorption of chemicals on the stainless steel needle of the SPME fiber was suspected to be one of the reasons why significant differences between theoretical and experimental sampling rates were observed. Correlations between the results for PGME from both SPME device and OSHA organic Method 99 were linear (r = 0.9984) and consistent (slope = 0.97 ± 0.03). Face velocity (0-0.18 m/s) also proved to have no effects on the sampler

  19. RAPID METHOD FOR DETERMINATION OF RADIOSTRONTIUM IN EMERGENCY MILK SAMPLES

    Energy Technology Data Exchange (ETDEWEB)

    Maxwell, S.; Culligan, B.

    2008-07-17

    A new rapid separation method for radiostrontium in emergency milk samples was developed at the Savannah River Site (SRS) Environmental Bioassay Laboratory (Aiken, SC, USA) that will allow rapid separation and measurement of Sr-90 within 8 hours. The new method uses calcium phosphate precipitation, nitric acid dissolution of the precipitate to coagulate residual fat/proteins and a rapid strontium separation using Sr Resin (Eichrom Technologies, Darien, IL, USA) with vacuum-assisted flow rates. The method is much faster than previous method that use calcination or cation exchange pretreatment, has excellent chemical recovery, and effectively removes beta interferences. When a 100 ml sample aliquot is used, the method has a detection limit of 0.5 Bq/L, well below generic emergency action levels.

  20. Characterizing lentic freshwater fish assemblages using multiple sampling methods.

    Science.gov (United States)

    Fischer, Jesse R; Quist, Michael C

    2014-07-01

    Characterizing fish assemblages in lentic ecosystems is difficult, and multiple sampling methods are almost always necessary to gain reliable estimates of indices such as species richness. However, most research focused on lentic fish sampling methodology has targeted recreationally important species, and little to no information is available regarding the influence of multiple methods and timing (i.e., temporal variation) on characterizing entire fish assemblages. Therefore, six lakes and impoundments (48-1,557 ha surface area) were sampled seasonally with seven gear types to evaluate the combined influence of sampling methods and timing on the number of species and individuals sampled. Probabilities of detection for species indicated strong selectivities and seasonal trends that provide guidance on optimal seasons to use gears when targeting multiple species. The evaluation of species richness and number of individuals sampled using multiple gear combinations demonstrated that appreciable benefits over relatively few gears (e.g., to four) used in optimal seasons were not present. Specifically, over 90 % of the species encountered with all gear types and season combinations (N = 19) from six lakes and reservoirs were sampled with nighttime boat electrofishing in the fall and benthic trawling, modified-fyke, and mini-fyke netting during the summer. Our results indicated that the characterization of lentic fish assemblages was highly influenced by the selection of sampling gears and seasons, but did not appear to be influenced by waterbody type (i.e., natural lake, impoundment). The standardization of data collected with multiple methods and seasons to account for bias is imperative to monitoring of lentic ecosystems and will provide researchers with increased reliability in their interpretations and decisions made using information on lentic fish assemblages.

  1. Determination of higher carboxylic acids in snow samples using solid-phase extraction and LC/MS-TOF.

    Science.gov (United States)

    Kippenberger, Matthias; Winterhalter, Richard; Moortgat, Geert K

    2008-12-01

    The objective of this work was to develop a method to determine the concentrations of higher organic acids in snow samples. The target species are the homologous aliphatic alpha,omega-dicarboxylic acids from C(5) to C(13), pinonic acid, pinic acid and phthalic acid. A preconcentration procedure utilizing solid phase extraction was developed and optimized using solutions of authentic standards. The influences of different parameters such as flow rate during extraction and the concentration of the eluent on the efficiency of the extraction procedure were investigated. The compounds of interest were separated by HPLC and detected by a quadrupole time-of-flight mass spectrometer (qTOF-MS). The recovery rate (extraction efficiency) of the extraction procedure was found to vary between 41% for tridecanedioic acid and 102% for adipic acid. The limits of detection were determined for all compounds and were between 0.9 nmol/L (dodecanedioic acid) and 29.5 nmol/L (pinonic acid). An exception is pinic acid, for which a considerably higher detection limit of 103.9 nmol/L was calculated. Snow samples were collected in December 2006 and January 2007 at the Fee glacier (Switzerland) from locations at heights from 3056 to 3580 m asl and from different depths within the snow layer. In total, the analysis of 61 single snow samples was performed, and the following compounds could be quantified: homologous aliphatic alpha,omega-dicarboxylic acids with 5-12 carbon atoms and phthalic acid. Tridecanedioic acid, pinonic and pinic acid were identified in the samples but were not quantified due to their low concentrations. The three most abundant acids found in the molten snow samples were glutaric acid (C(5)-di; 3.90 nmol/L), adipic acid (C(6)-di; 3.35 nmol/L) and phthalic acid (Ph; 3.04 nmol/L).

  2. Preconcentration and analysis of Rhodamine B in water and red wine samples by using magnesium hydroxide/carbon nanotube composites as a solid-phase extractant.

    Science.gov (United States)

    Wu, Zhi-Liang; Liu, Qi; Chen, Xiao-Qing; Yu, Jin-Gang

    2015-10-01

    A convenient and accurate analysis approach that combined solid-phase extraction and high-performance liquid chromatography was developed to determine the amount of Rhodamine B in red wine and Xiang-jiang river water samples. A novel composite, magnesium hydroxide/carbon nanotube composites, was synthesized and used as the solid-phase extractant for the preconcentration/analysis of Rhodamine B. Magnesium hydroxide/carbon nanotube composites, which combined the merits of carbon nanotubes and magnesium hydroxide, exhibited acceptable adsorption and desorption efficiencies for Rhodamine B. The linear range of the proposed solid-phase extraction with high-performance liquid chromatography method for Rhodamine B was 0.05-20.0 mg/L, with a limit of detection of 3.6 μg/L. The precision and reproducibility of the developed solid-phase extraction with high-performance liquid chromatography method and the batch-to-batch reproducibility of the solid-phase extractant were also validated at spiking levels of 0.5 and 2.0 mg/L. The recovery of Rhodamine B was 94.33-106.7%, and the recovery relative standard deviations of the intra- and interday precisions were ≤ 3.83 and ≤ 6.01%, respectively. The relative standard deviation of the batch-to-batch reproducibility was ≤ 7.98%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Self-contained cryogenic gas sampling apparatus and method

    Science.gov (United States)

    McManus, G.J.; Motes, B.G.; Bird, S.K.; Kotter, D.K.

    1996-03-26

    Apparatus for obtaining a whole gas sample, is composed of: a sample vessel having an inlet for receiving a gas sample; a controllable valve mounted for controllably opening and closing the inlet; a valve control coupled to the valve for opening and closing the valve at selected times; a portable power source connected for supplying operating power to the valve control; and a cryogenic coolant in thermal communication with the vessel for cooling the interior of the vessel to cryogenic temperatures. A method is described for obtaining an air sample using the apparatus described above, by: placing the apparatus at a location at which the sample is to be obtained; operating the valve control to open the valve at a selected time and close the valve at a selected subsequent time; and between the selected times maintaining the vessel at a cryogenic temperature by heat exchange with the coolant. 3 figs.

  4. Fluidics platform and method for sample preparation and analysis

    Science.gov (United States)

    Benner, W. Henry; Dzenitis, John M.; Bennet, William J.; Baker, Brian R.

    2014-08-19

    Herein provided are fluidics platform and method for sample preparation and analysis. The fluidics platform is capable of analyzing DNA from blood samples using amplification assays such as polymerase-chain-reaction assays and loop-mediated-isothermal-amplification assays. The fluidics platform can also be used for other types of assays and analyzes. In some embodiments, a sample in a sealed tube can be inserted directly. The following isolation, detection, and analyzes can be performed without a user's intervention. The disclosed platform may also comprises a sample preparation system with a magnetic actuator, a heater, and an air-drying mechanism, and fluid manipulation processes for extraction, washing, elution, assay assembly, assay detection, and cleaning after reactions and between samples.

  5. New methods and materials for solid phase extraction and high performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Dumont, Philip John [Iowa State Univ., Ames, IA (United States)

    1996-04-23

    This paper describes methods for solid phase extraction and high performance liquid chromatography (HPLC). The following are described: Effects of Resin Sulfonation on the Retention of Polar Organic Compounds in Solid Phase Extraction; Ion-Chromatographic Separation of Alkali Metals In Non-Aqueous Solvents; Cation-Exchange Chromatography in Non-Aqueous Solvents; and Silicalite As a Stationary Phase For HPLC.

  6. Methods for Sampling and Measurement of Compressed Air Contaminants

    Energy Technology Data Exchange (ETDEWEB)

    Stroem, L.

    1976-10-15

    In order to improve the technique for measuring oil and water entrained in a compressed air stream, a laboratory study has been made of some methods for sampling and measurement. For this purpose water or oil as artificial contaminants were injected in thin streams into a test loop, carrying dry compressed air. Sampling was performed in a vertical run, down-stream of the injection point. Wall attached liquid, coarse droplet flow, and fine droplet flow were sampled separately. The results were compared with two-phase flow theory and direct observation of liquid behaviour. In a study of sample transport through narrow tubes, it was observed that, below a certain liquid loading, the sample did not move, the liquid remaining stationary on the tubing wall. The basic analysis of the collected samples was made by gravimetric methods. Adsorption tubes were used with success to measure water vapour. A humidity meter with a sensor of the aluminium oxide type was found to be unreliable. Oil could be measured selectively by a flame ionization detector, the sample being pretreated in an evaporation- condensation unit

  7. Modelling the Solid Waste Flow into Sungai Ikan Landfill Sites by Material Flow Analysis Method

    Science.gov (United States)

    Ghani, Latifah A.; Ali, Nora’aini; Hassan, Nur Syafiqah A.

    2017-12-01

    The purpose of this paper is to model the material flow of solid waste flows at Kuala Terengganu by using Material Flow Analysis (MFA) method, generated by STAN Software Analysis. Sungai Ikan Landfill has been operated for about 10 years. Average, Sungai Ikan Landfill receive an amount around 260 tons per day of solid waste. As for the variety source of the solid waste coming from, leachates that accumulated has been tested and measured. Highest reading of pH of the leachate is 8.29 which is still in the standard level before discharging the leachate to open water which pH in between 8.0-9.0. The percentages of the solid waste has been calculated and seven different types of solid waste has been segregated. That is, plastics, organic waste, paper, polystyrene, wood, fabric and can. The estimation of the solid waste that will be end as a residue are around 244 tons per day.

  8. SOLID PHASE MICROEXTRACTION SAMPLING OF FIRE DEBRIS RESIDUES IN THE PRESENCE OF RADIONUCLIDE SURROGATE METALS

    Energy Technology Data Exchange (ETDEWEB)

    Duff, M; Keisha Martin, K; S Crump, S

    2007-03-23

    The Federal Bureau of Investigation (FBI) Laboratory currently does not have on site facilities for handling radioactive evidentiary materials and there are no established FBI methods or procedures for decontaminating highly radioactive fire debris (FD) evidence while maintaining evidentiary value. One experimental method for the isolation of FD residue from radionuclide metals involves using solid phase microextraction (SPME) fibers to remove the residues of interest. Due to their high affinity for organics, SPME fibers should have little affinity for most (radioactive) metals. The focus of this research was to develop an examination protocol that was applicable to safe work in facilities where high radiation doses are shielded from the workers (as in radioactive shielded cells or ''hot cells''). We also examined the affinity of stable radionuclide surrogate metals (Co, Ir, Re, Ni, Ba, Cs, Nb, Zr and Nd) for sorption by the SPME fibers. This was done under exposure conditions that favor the uptake of FD residues under conditions that will provide little contact between the SPME and the FD material (such as charred carpet or wood that contains commonly-used accelerants). Our results from mass spectrometric analyses indicate that SPME fibers show promise for use in the room temperature head space uptake of organic FD residue (namely, diesel fuel oil, kerosene, gasoline and paint thinner) with subsequent analysis by gas chromatography (GC) with mass spectrometric (MS) detection. No inorganic forms of ignitable fluids were included in this study.

  9. Sampling gaseous compounds from essential oils evaporation by solid phase microextraction devices

    Science.gov (United States)

    Cheng, Wen-Hsi; Lai, Chin-Hsing

    2014-12-01

    Needle trap samplers (NTS) are packed with 80-100 mesh divinylbenzene (DVB) particles to extract indoor volatile organic compounds (VOCs). This study compared extraction efficiency between an NTS and a commercially available 100 μm polydimethylsiloxane-solid phase microextration (PDMS-SPME) fiber sampler used to sample gaseous products in heated tea tree essential oil in different evaporation modes, which were evaporated respectively by free convection inside a glass evaporation dish at 27 °C, by evaporation diffuser at 60 °C, and by thermal ceramic wicks at 100 °C. The experimental results indicated that the NTS performed better than the SPME fiber samplers and that the NTS primarily adsorbed 5.7 ng ethylbenzene, 5.8 ng m/p-xylenes, 11.1 ng 1,2,3-trimethylbenzene, 12.4 ng 1,2,4-trimethylbenzene and 9.99 ng 1,4-diethylbenzene when thermal ceramic wicks were used to evaporate the tea tree essential oil during a 1-hr evaporation period. The experiment also indicated that the temperature used to heat the essential oils should be as low as possible to minimize irritant VOC by-products. If the evaporation temperature does not exceed 100 °C, the concentrations of main by-products trimethylbenzene and diethylbenzene are much lower than the threshold limit values recommended by the National Institute for Occupational Safety and Health (NIOSH).

  10. Microcapillary reactors using solid-phase DNA sequencing for direct sample introduction into slab gels.

    Science.gov (United States)

    Xu, Y; Bruch, R C; Soper, S A

    2000-05-01

    Solid-phase micro-reactors have been prepared in glass capillaries for DNA sequencing applications using slab gel electrophoresis, which consisted of a fused silica capillary (i.d. = 100 microns; o.d. = 365 microns; length = 15 cm; volume = 1.2 microL) that contained a covalently bound biotin molecule. With the addition of streptavidin to the capillary, an anchoring site was produced for the tethering of biotinylated DNA sequencing templates to the wall of the capillary. Using a four-lane, single dye primer chemistry sequencing strategy, the individual tracts were prepared in the capillaries using cycle sequencing (20 thermal cycles) on a PCR-generated lambda-bacteriophage template (about 1000 bp). The dye label in this case was a fluorescent tag that displayed emission properties in the near-IR and could be processed on an automated sequencer. The read length was found to be 589 bases, which was determined primarily by the fractionating power of the gel. It was also found that the tethering system was very stable to typical cycle sequencing conditions, with the amount of tethered DNA lost amounting to 40% after 120 thermal cycles. The ability to use dye terminator chemistry was also investigated by using a near-IR dye-labeled terminator (ddGTP). It was found that the quality of the ladder that was generated was comparable to that obtained in a conventional sample preparation format. However, ethanol precipitation was required before gel loading to remove excess terminator.

  11. Development and Physicochemical Characterization of Sirolimus Solid Dispersions Prepared by Solvent Evaporation Method

    Directory of Open Access Journals (Sweden)

    Shahram Emami

    2014-12-01

    Full Text Available Purpose: The aim of the present investigation was preparation and characterization of sirolimus solid dispersions by solvent evaporation technique to improve its dissolution properties. Methods: Polyvinylpyrrolidone (PVP, Poloxamer 188 and Cremophore RH40 were used to prepare the solid dispersions of sirolimus. In vitro dissolution study using USP type I apparatus, were performed in distilled water (containing SLS 0.4% for pure sirolimus, physical mixtures, Rapamune and prepared solid dispersions. The characterization of solid dispersions was performed using Fourier Transform Infrared (FTIR Spectroscopy and Differential Scanning Calorimetry (DSC. Results: More than 75% of sirolimus was released within 30 minutes from all prepared solid dispersions. The dissolution rate of all prepared solid dispersion powders were more than physical mixtures. The absence of sirolimus peak in the DSC spectrum of solid dispersions indicated the conversion of crystalline form of sirolimus into amorphous form. The results from FT-IR spectroscopy showed that there was no significant change in the FT-IR spectrum of solid dispersions indicating absence of well-defined interaction between drug and carriers. Conclusion: It was concluded that solid dispersion method, using PVP, Poloxamer 188 and Cremophore RH40 can improve dissolution rate of sirolimus.

  12. Synthesis of GaN:ZnO solid solution by solution combustion method and characterization for photocatalytic application

    Science.gov (United States)

    Menon, Sumithra Sivadas; Anitha, R.; Gupta, Bhavana; Baskar, K.; Singh, Shubra

    2016-05-01

    GaN-ZnO solid solution has emerged as a successful and reproducible photocatalyst for overall water splitting by one-step photoexcitation, with a bandgap in visible region. When the solid solution is formed, some of the Zn and O ions are replaced by Ga and N ions respectively and there is a narrowing of bandgap which is hypothesized as due to Zn3d-N2p repulsion. The traditional method of synthesis of GaN-ZnO solid solution is by nitridation of the starting oxides under constant ammonia flow. Here we report a solution combustion technique for the synthesis of the solid solution at a temperature about 500 ° C in a muffle furnace with metal nitrates as precursors and urea as the fuel. The as prepared samples showed change in color with the increased concentration of ZnO in the solution. The structural, microstructural, morphological and optical properties of the samples were realized by Powder X ray diffraction, Scanning electron microscopy, Energy dispersive X ray analysis, Transmission electron microscopy and Photoluminescence. Finally the hydrogen production efficiency of the GaN-ZnO nanopowders by water splitting was found, using methanol as a scavenger. The apparent quantum yield (AQY) of 0.048% is obtained for GaN-ZnO solid solution.

  13. Synthesis of GaN:ZnO solid solution by solution combustion method and characterization for photocatalytic application

    Energy Technology Data Exchange (ETDEWEB)

    Menon, Sumithra Sivadas; Anitha, R.; Baskar, K.; Singh, Shubra, E-mail: shubra6@gmail.com [Crystal Growth Centre, Anna University, Chennai-600025 (India); Gupta, Bhavana [Material Science Division, Indira Gandhi Centre for Atomic Research, Kalpakkam 603102 (India)

    2016-05-23

    GaN-ZnO solid solution has emerged as a successful and reproducible photocatalyst for overall water splitting by one-step photoexcitation, with a bandgap in visible region. When the solid solution is formed, some of the Zn and O ions are replaced by Ga and N ions respectively and there is a narrowing of bandgap which is hypothesized as due to Zn3d-N2p repulsion. The traditional method of synthesis of GaN-ZnO solid solution is by nitridation of the starting oxides under constant ammonia flow. Here we report a solution combustion technique for the synthesis of the solid solution at a temperature about 500 ° C in a muffle furnace with metal nitrates as precursors and urea as the fuel. The as prepared samples showed change in color with the increased concentration of ZnO in the solution. The structural, microstructural, morphological and optical properties of the samples were realized by Powder X ray diffraction, Scanning electron microscopy, Energy dispersive X ray analysis, Transmission electron microscopy and Photoluminescence. Finally the hydrogen production efficiency of the GaN-ZnO nanopowders by water splitting was found, using methanol as a scavenger. The apparent quantum yield (AQY) of 0.048% is obtained for GaN-ZnO solid solution.

  14. Water-equivalent solid sources prepared by means of two distinct methods

    Energy Technology Data Exchange (ETDEWEB)

    Koskinas, Marina F.; Yamazaki, Ione M.; Potiens Junior, Ademar, E-mail: koskinas@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2014-07-01

    The Nuclear Metrology Laboratory at IPEN is involved in developing radioactive water-equivalent solid sources prepared from an aqueous solution of acrylamide using two distinct methods for polymerization. One of them is the polymerization by high dose of {sup 60}Co irradiation; in the other method the solid matrix-polyacrylamide is obtained from an aqueous solution composed by acrylamide, catalyzers and an aliquot of a radionuclide. The sources have been prepared in cylindrical geometry. In this paper, the study of the distribution of radioactive material in the solid sources prepared by both methods is presented. (author)

  15. Optimal sparse sampling for estimating ganciclovir/valganciclovir AUC in solid organ transplant patients using NONMEN.

    Science.gov (United States)

    Padullés Caldés, Ariadna; Colom, Helena; Caldes, Anna; Cerezo, Gema; Torras, Joan; Grinyó, Josep M; Lloberas, Núria

    2014-06-01

    Ganciclovir and valganciclovir (GCV/VGCV) are used for the treatment and prophylaxis of cytomegalovirus in solid organ transplant (SOT) patients. An area under the time-concentration curve of 40-50 μg × h/mL is related to efficacy. Therapeutic drug monitoring could prevent suboptimal drug exposure and adverse events, but obtaining full concentration profiles is not feasible. Sampling optimization by developing a reliable and clinically applicable limited sampling strategy (LSS) may simplify dose adjustment. An LSS was developed using an original pharmacokinetic (PK) data set of 40 full profiles from 20 adult SOT patients. The LSS was developed based on population and Bayesian prediction approaches. Population PK parameters from a previous model were used for simulation or as priors (NONMEM version 7.2). Median percentage of prediction error and median of absolute percentage prediction error were calculated for plasma clearance (CL) and central compartment distribution volume (V(2)). Bias and precisions were compared using 1-way analysis of variance (SPSSv19.0). Sampling windows were designed according to the PK profile previously observed with the entire set of data. The 4 windows selected were distributed from 0.5 to 1.5 hours, 2 to 3 hours, 4 to 5 hours, and 6 to 8 hours. Predose and concentrations beyond 8 hours were not considered in any case because simulated negative concentrations occurred in both cases. Predicted exposure using 3 sampling times (0.5-1.5, 4-5, and 6-8 hours) showed the best predictive performance, by either the population or Bayesian approaches. Bias and imprecision for CL and V(2) were 0 and 0.60%, and -0.78% and 0.78%, respectively. GCV/VCG area under the time-concentration curve in SOT patients could be predicted with acceptable accuracy for clinical management and dose individualization using LSS. The estimator of GCV/VGC, using 3 concentrations measured at 0.5-1.5, 4-5, and 6-8 hours after drug intake, could be used for dose

  16. Eriochrome Blue Black modified activated carbon as solid phase extractor for removal of Pb(II ions from water samples

    Directory of Open Access Journals (Sweden)

    Hassan M. Albishri

    2017-05-01

    Full Text Available In the current study, a sensitive and simple method for the removal of lead Pb(II, from water samples prior to its determination by inductively coupled plasma optical emission spectrometry (ICP-OES, was investigated. The method utilized activated carbon (AC physically modified with Eriochrome Blue Black (EBB as a solid-phase extractant. Surface properties of the AC-EBB phase were characterized by FT-IR and SEM. The separation parameters for effective adsorption of lead Pb(II, including effects of pH, initial concentration of Pb(II, coexisting ions and shaking time using batch method were studied. The optimum pH value for the separation of Pb(II on the new sorbent was 7.0, and the maximum static adsorption capacity of Pb(II onto the AC-EBB was 127.896 mg/g at this pH and after 1 h contact time. The Pb(II adsorption data were modeled using Langmuir adsorption isotherms. Results demonstrated that the adsorption of Pb(II onto activated carbon followed pseudo second-order kinetic model.

  17. Extraction, separation and characterization of endotoxins in water samples using solid phase extraction and capillary electrophoresis-laser induced fluorescence.

    Science.gov (United States)

    Fung, Fun Man; Su, Min; Feng, Hua-Tao; Li, Sam Fong Yau

    2017-09-07

    This study focuses on one of the key environmental threats, endotoxins, also known as lipopolysaccharides (LPS). A capillary electrophoresis method in combination with laser induced fluorescence (LIF) detection was developed for the analysis of endotoxins from 16 different bacterial strains. LPSs were derivatized with the amino-reactive fluorescent dye, fluorescein isothiocyanate (FITC), separated by capillary zone electrophoresis (CZE) under the optimized conditions with the use of 50 mM sodium tetraborate buffer (pH 9.30), and detected by LIF detector. To improve the sensitivity of CZE-LIF detection for the determination of trace amounts of endotoxins and to remove possible interference materials in environmental samples, a solid phase extraction (SPE) pre-concentration technique was applied successfully. The SPE targeted at polysaccharide moieties of LPSs and showed LPS enrichment effects too. CE migration time could also reveal the O-antigen chain lengths of LPSs. This CE method and SPE pretreatment showed linearity at 99.84%, and repeatabilities at 8.44% and 11.0% for endotoxins from E. Coli O55:B5 and E. Coli O26:B6. The limit of detection (LOD) could reach around 5 ng/mL at optimized condition. The method was applied successfully to the determination of LPS levels in tap water and wastewater, and demonstrated sensitive, reproducible and reliable results.

  18. Isotopic abundance measurements on solid nuclear-type samples by glow discharge mass spectrometry.

    Science.gov (United States)

    Betti, M; Rasmussen, G; Koch, L

    1996-07-01

    A double-focusing Glow Discharge Mass Spectrometer (GDMS) installed in a glovebox for nuclear sample screening has been employed for isotopic measurements. Isotopic compositions of zirconium, silicon, lithium, boron, uranium and plutonium which are elements of nuclear concern have been determined. Interferences arising from the matrix sample and the discharge gas (Ar) for each of these elements are discussed. The GDMS results are compared with those from Thermal Ionization Mass Spectrometry (TIMS). For boron and lithium at microg/g-ng/g levels, the two methods gave results in good agreement. In samples containing uranium the isotopic composition obtained by GDMS was in agreement with those from TIMS independently of the enrichment. Attempts for the determination of plutonium isotopic composition were also made. In this case, due to the interferences of uranium at mass 238 and americium at mass 241, the GDMS raw data are complementary with those values obtained from physical non-destructive techniques.

  19. Evidence on unusual way of cocaine smuggling: cocaine-polymethyl methacrylate (PMMA) solid solution--study of clandestine laboratory samples.

    Science.gov (United States)

    Gostic, T; Klemenc, S

    2007-07-04

    An abandoned clandestine laboratory was seized in Slovenia. All confiscated exhibits were analysed in a forensic laboratory, where the following analytical methods were applied: capillary gas chromatography coupled with mass spectrometry (GC-MS) combined also by solid-phase micro extraction (SPME) and pyrolysis (Py) technique, Fourier transform infrared spectrometry (FTIR) and scanning electron microscopy with energy dispersive X-ray detector (SEM-EDX). The most interesting analytical findings can be summarised as follows: at the crime scene some plastic pieces, which contained cocaine dissolved (as solid solution) in polymethyl methacrylate-plexiglass (PMMA), were found. The highest cocaine concentration measured in the plastic sample was about 15% by weight. Two larger lumps of material (12 and 3 kg) were composed mainly of PMMA and CaCO3 and contained only 0.4 and 0.5% of cocaine, respectively. As for the low cocaine concentration, we assume that those two lumps of material represent discarded waste product--residue after the isolation of cocaine from plastic. Higher quantities of pure solvents (41 l) and solvent mixtures (87 l) were seized. We identified three types of pure solvents (acetone, gasoline and benzine) and two different types of solvent mixtures (benzine/acetone and gasoline/acetone). The total seized volume (87 l) of solvent mixtures holds approximately 395 g of solid residue formed mainly of PMMA and cocaine. Obviously solvent mixtures were used for isolation of cocaine from the plastic. Small quantities of relatively pure cocaine base were identified on different objects. There were two cotton sheets, most probably used for filtration. One sheet had traces of cocaine base (76% purity) on the surface, while cocaine in hydrochloride form (96%) was identified on the other sheet. GC-MS analyses of micro traces isolated from analytical balances showed the presence of cocaine and some common adulterants: phenacetine, lidocaine and procaine. A cocaine

  20. RAPID SEPARATION METHOD FOR EMERGENCY WATER AND URINE SAMPLES

    Energy Technology Data Exchange (ETDEWEB)

    Maxwell, S.; Culligan, B.

    2008-08-27

    The Savannah River Site Environmental Bioassay Lab participated in the 2008 NRIP Emergency Response program administered by the National Institute for Standards and Technology (NIST) in May, 2008. A new rapid column separation method was used for analysis of actinides and {sup 90}Sr the NRIP 2008 emergency water and urine samples. Significant method improvements were applied to reduce analytical times. As a result, much faster analysis times were achieved, less than 3 hours for determination of {sup 90}Sr and 3-4 hours for actinides. This represents a 25%-33% improvement in analysis times from NRIP 2007 and a {approx}100% improvement compared to NRIP 2006 report times. Column flow rates were increased by a factor of two, with no significant adverse impact on the method performance. Larger sample aliquots, shorter count times, faster cerium fluoride microprecipitation and streamlined calcium phosphate precipitation were also employed. Based on initial feedback from NIST, the SRS Environmental Bioassay Lab had the most rapid analysis times for actinides and {sup 90}Sr analyses for NRIP 2008 emergency urine samples. High levels of potential matrix interferences may be present in emergency samples and rugged methods are essential. Extremely high levels of {sup 210}Po were found to have an adverse effect on the uranium results for the NRIP-08 urine samples, while uranium results for NRIP-08 water samples were not affected. This problem, which was not observed for NRIP-06 or NRIP-07 urine samples, was resolved by using an enhanced {sup 210}Po removal step, which will be described.

  1. Adsorptive behavior and solid-phase microextraction of bare stainless steel sample loop in high performance liquid chromatography.

    Science.gov (United States)

    Zhang, Wenpeng; Zhang, Zixin; Meng, Jiawei; Zhou, Wei; Chen, Zilin

    2014-10-24

    In this work, we interestingly happened to observe the adsorption of stainless steel sample loop of HPLC. The adsorptive behaviors of the stainless steel loop toward different kinds of compounds were studied, including polycyclic aromatic hydrocarbons (PAHs), halogeno benzenes, aniline derivatives, benzoic acid derivatives, phenols, benzoic acid ethyl ester, benzaldehyde, 1-phenyl-ethanone and phenethyl alcohol. The adsorptive mechanism was probably related to hydrophobic interaction, electron-rich element-metal interaction and hydrogen bond. Universal adsorption of stainless steels was also testified. Inspired by its strong adsorptive capability, bare stainless steel loop was developed as a modification-free in-tube device for solid-phase microextraction (SPME), which served as both the substrate and sorbent and possessed ultra-high strength and stability. Great extraction efficiency toward PAHs was obtained by stainless steel loop without any modification, with enrichment factors of 651-834. By connecting the stainless steel loop onto a six-port valve, an online SPME-HPLC system was set up and an SPME-HPLC method has been validated for determination of PAHs. The method has exceptionally low limits of detection of 0.2-2pg/mL, which is significantly lower than that of reported methods with different kinds of sorbents. Wide linear range (0.5-500 and 2-1000pg/mL), good linearity (R(2)≥0.9987) and good reproducibility (RSD≤2.9%) were also obtained. The proposed method has been applied to determine PAHs in environmental samples. Good recoveries were obtained, ranging from 88.5% to 93.8%. Copyright © 2014 Elsevier B.V. All rights reserved.

  2. Development of a simple analytical method for determining trihalomethanes in beer using a headspace solid-phase microextraction technique

    Directory of Open Access Journals (Sweden)

    Marcel Silveira dos Santos

    2013-01-01

    Full Text Available We developed a simple, rapid, and solventless method for analyzing trihalomethanes in beer samples using headspace solid-phase microextraction. The effects of varying experimental parameters, such as extraction temperature and time, addition of sodium chloride, and agitation speed, on extraction yield were studied using a univariate experimental design. Limits of detection between 0.22 and 0.46 µg L- 1 and wide linear ranges were achieved for trihalomethanes. We measured the trihalomethane recoveries and precision (as the standard deviation of repeat measurements and demonstrated the applicability of the proposed method by analyzing 32 beer samples.

  3. NEW COLUMN SEPARATION METHOD FOR EMERGENCY URINE SAMPLES

    Energy Technology Data Exchange (ETDEWEB)

    Maxwell, S; Brian Culligan, B

    2007-08-28

    The Savannah River Site Environmental Bioassay Lab participated in the 2007 NRIP Emergency Response program administered by the National Institute for Standards and Technology (NIST) in May, 2007. A new rapid column separation method was applied directly to the NRIP 2007 emergency urine samples, with only minimal sample preparation to reduce preparation time. Calcium phosphate precipitation, previously used to pre-concentrate actinides and Sr-90 in NRIP 2006 urine and water samples, was not used for the NRIP 2007 urine samples. Instead, the raw urine was acidified and passed directly through the stacked resin columns (TEVA+TRU+SR Resins) to separate the actinides and strontium from the NRIP urine samples more quickly. This improvement reduced sample preparation time for the NRIP 2007 emergency urine analyses significantly. This approach works well for small volume urine samples expected during an emergency response event. Based on initial feedback from NIST, the SRS Environmental Bioassay Lab had the most rapid analysis times for actinides and strontium-90 analyses for NRIP 2007 urine samples.

  4. Simultaneous determination of V, Ni and Fe in fuel fly ash using solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Cárdenas Valdivia, A; Vereda Alonso, E; López Guerrero, M M; Gonzalez-Rodriguez, J; Cano Pavón, J M; García de Torres, A

    2018-03-01

    A green and simple method has been proposed in this work for the simultaneous determination of V, Ni and Fe in fuel ash samples by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry (SS HR CS GFAAS). The application of fast programs in combination with direct solid sampling allows eliminating pretreatment steps, involving minimal manipulation of sample. Iridium treated platforms were applied throughout the present study, enabling the use of aqueous standards for calibration. Correlation coefficients for the calibration curves were typically better than 0.9931. The concentrations found in the fuel ash samples analysed ranged from 0.66% to 4.2% for V, 0.23-0.7% for Ni and 0.10-0.60% for Fe. Precision (%RSD) were 5.2%, 10.0% and 9.8% for V, Ni and Fe, respectively, obtained as the average of the %RSD of six replicates of each fuel ash sample. The optimum conditions established were applied to the determination of the target analytes in fuel ash samples. In order to test the accuracy and applicability of the proposed method in the analysis of samples, five ash samples from the combustion of fuel in power stations, were analysed. The method accuracy was evaluated by comparing the results obtained using the proposed method with the results obtained by ICP OES previous acid digestion. The results showed good agreement between them. The goal of this work has been to develop a fast and simple methodology that permits the use of aqueous standards for straightforward calibration and the simultaneous determination of V, Ni and Fe in fuel ash samples by direct SS HR CS GFAAS. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Determination of heavy metals in solid emission and immission samples using atomic absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Fara, M.; Novak, F. [EGU Prague, PLC, Bichovice, Prague (Czechoslovakia)

    1995-12-01

    Both flame and electrothermal methods of atomic absorption spectroscopy (AAS) have been applied to the determination of Al, As, Be, Ca, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, TI, Se, V and Zn in emission and emission (deposition) samples decomposed in open PTFE test-tubes by individual fuming-off hydrofluoric, perchloroic and nitric acid. An alternative hydride technique was also used for As and Se determination and Hg was determined using a self-contained AAS analyzer. A graphite platform proved good to overcome non-spectral interferences in AAS-ETA. Methods developed were verified by reference materials (inc. NBS 1633a).

  6. Surge block method for controlling well clogging and sampling sediment during bioremediation.

    Science.gov (United States)

    Wu, Wei-Min; Watson, David B; Luo, Jian; Carley, Jack; Mehlhorn, Tonia; Kitanidis, Peter K; Jardine, Phlip M; Criddle, Craig S

    2013-11-01

    A surge block treatment method (i.e. inserting a solid rod plunger with a flat seal that closely fits the casing interior into a well and stocking it up and down) was performed for the rehabilitation of wells clogged with biomass and for the collection of time series sediment samples during in situ bioremediation tests for U(VI) immobilization at a the U.S. Department of Energy site in Oak Ridge, TN. The clogging caused by biomass growth had been controlled by using routine surge block treatment for 18 times over a nearly four year test period. The treatment frequency was dependent of the dosage of electron donor injection and microbial community developed in the subsurface. Hydraulic tests showed that the apparent aquifer transmissivity at a clogged well with an inner diameter (ID) of 10.16 cm was increased by 8-13 times after the rehabilitation, indicating the effectiveness of the rehabilitation. Simultaneously with the rehabilitation, the surge block method was successfully used for collecting time series sediment samples composed of fine particles (clay and silt) from wells with ID 1.9-10.16 cm for the analysis of mineralogical and geochemical composition and microbial community during the same period. Our results demonstrated that the surge block method provided a cost-effective approach for both well rehabilitation and frequent solid sampling at the same location. Copyright © 2013 Elsevier Ltd. All rights reserved.

  7. Surge Block Method for Controlling Well Clogging and Sampling Sediment during Bioremediation

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Wei-min [Stanford University; Watson, David B [ORNL; Luo, Jian [Stanford University; Carley, Jack M [ORNL; Mehlhorn, Tonia L [ORNL; Kitanidis, Peter K. [Stanford University; Jardine, Philip [University of Tennessee, Knoxville (UTK); Criddle, Craig [Stanford University

    2013-01-01

    A surge block treatment method (i.e. inserting a solid rod plunger with a flat seal that closely fits the casing interior into a well and stocking it up and down) was performed for the rehabilitation of wells clogged with biomass and for the collection of time series sediment samples during in situ bioremediation tests for U(VI) immobilization at a the U.S. Department of Energy site in Oak Ridge, TN. The clogging caused by biomass growth had been controlled by using routine surge block treatment for18 times over a nearly four year test period. The treatment frequency was dependent of the dosage of electron donor injection and microbial community developed in the subsurface. Hydraulic tests showed that the apparent aquifer transmissivity at a clogged well with an inner diameter (ID) of 10.16 cm was increased by 8 13 times after the rehabilitation, indicating the effectiveness of the rehabilitation. Simultaneously with the rehabilitation, the surge block method was successfully used for collecting time series sediment samples composed of fine particles (clay and silt) from wells with ID 1.9 10.16 cm for the analysis of mineralogical and geochemical composition and microbial community during the same period. Our results demonstrated that the surge block method provided a cost-effective approach for both well rehabilitation and frequent solid sampling at the same location.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-05-15

    Three new methods to sample and prepare various carbonyl compounds for radiocarbon measurements were developed and tested. Two of these procedures utilized the Strecker synthetic method to form amino acids from carbonyl compounds with either sodium cyanide or trimethylsilyl cyanide. The third procedure used semicarbazide to form crystalline carbazones with the carbonyl compounds. The resulting amino acids and semicarbazones were then separated and purified using thin layer chromatography. The separated compounds were then combusted to CO{sub 2} and reduced to graphite to determine {sup 14}C content by accelerator mass spectrometry (AMS). All of these methods were also compared with the standard carbonyl compound sampling method wherein a compound is derivatized with 2,4-dinitrophenylhydrazine and then separated by high-performance liquid chromatography (HPLC).

  9. Method of extruding and packaging a thin sample of reactive material including forming the extrusion die

    Science.gov (United States)

    Lewandowski, Edward F.; Peterson, Leroy L.

    1985-01-01

    This invention teaches a method of cutting a narrow slot in an extrusion die with an electrical discharge machine by first drilling spaced holes at the ends of where the slot will be, whereby the oil can flow through the holes and slot to flush the material eroded away as the slot is being cut. The invention further teaches a method of extruding a very thin ribbon of solid highly reactive material such as lithium or sodium through the die in an inert atmosphere of nitrogen, argon or the like as in a glovebox. The invention further teaches a method of stamping out sample discs from the ribbon and of packaging each disc by sandwiching it between two aluminum sheets and cold welding the sheets together along an annular seam beyond the outer periphery of the disc. This provides a sample of high purity reactive material that can have a long shelf life.

  10. Global metabolite analysis of yeast: evaluation of sample preparation methods

    DEFF Research Database (Denmark)

    Villas-Bôas, Silas Granato; Højer-Pedersen, Jesper; Åkesson, Mats Fredrik

    2005-01-01

    Sample preparation is considered one of the limiting steps in microbial metabolome analysis. Eukaryotes and prokaryotes behave very differently during the several steps of classical sample preparation methods for analysis of metabolites. Even within the eukaryote kingdom there is a vast diversity...... of cell structures that make it imprudent to blindly adopt protocols that were designed for a specific group of microorganisms. We have therefore reviewed and evaluated the whole sample preparation procedures for analysis of yeast metabolites. Our focus has been on the current needs in metabolome analysis......, which is the analysis of a large number of metabolites with very diverse chemical and physical properties. This work reports the leakage of intracellular metabolites observed during quenching yeast cells with cold methanol solution, the efficacy of six different methods for the extraction...

  11. Sampling and analysis methods for geothermal fluids and gases

    Energy Technology Data Exchange (ETDEWEB)

    Shannon, D. W.

    1978-01-01

    The data obtained for the first round robin sample collected at Mesa 6-2 wellhead, East Mesa Test Site, Imperial Valley are summarized. Test results are listed by method used for cross reference to the analytic methods section. Results obtained for radioactive isotopes present in the brine sample are tabulated. The data obtained for the second round robin sample collected from the Woolsey No. 1 first stage flash unit, San Diego Gas and Electric Niland Test Facility are presented in the same manner. Lists of the participants of the two round robins are given. Data from miscellaneous analyses are included. Summaries of values derived from the round robin raw data are presented. (MHR)

  12. A Frequency Domain Design Method For Sampled-Data Compensators

    DEFF Research Database (Denmark)

    Niemann, Hans Henrik; Jannerup, Ole Erik

    1990-01-01

    A new approach to the design of a sampled-data compensator in the frequency domain is investigated. The starting point is a continuous-time compensator for the continuous-time system which satisfy specific design criteria. The new design method will graphically show how the discrete...

  13. Effect of method of sample preparation on ruminal in situ ...

    African Journals Online (AJOL)

    The objective of this study was to investigate the effect of method of sample preparation on the degradation kinetics of herbage when applying the in situ technique. Ryegrass (Lolium multiflorum cv. Midmar) was harvested at three and four weeks after cutting and fertilizing with 200 kg nitrogen (N)/ha. Freshly cut herbage ...

  14. Neonatal blood gas sampling methods | Goenka | South African ...

    African Journals Online (AJOL)

    Indwelling arterial catheters are a practical, reliable and accurate method of measuring acid-base parameters, provided they are inserted and maintained with the proper care. Capillary blood gas sampling is accurate, and a good substitute for radial 'stab' arterial puncture, avoiding many of the complications of repeated ...

  15. A General Linear Method for Equating with Small Samples

    Science.gov (United States)

    Albano, Anthony D.

    2015-01-01

    Research on equating with small samples has shown that methods with stronger assumptions and fewer statistical estimates can lead to decreased error in the estimated equating function. This article introduces a new approach to linear observed-score equating, one which provides flexible control over how form difficulty is assumed versus estimated…

  16. Protein precipitation methods for sample pretreatment of grass pea ...

    African Journals Online (AJOL)

    Protein precipitation methods for sample pretreatment of grass pea extracts. Negussie Wodajo, Ghirma Moges, Theodros Solomon. Abstract. Bull. Chem. Soc. Ethiop. 1996, 10(2), 129-134. Full Text: EMAIL FREE FULL TEXT EMAIL FREE FULL TEXT · DOWNLOAD FULL TEXT DOWNLOAD FULL TEXT. Article Metrics.

  17. Determination of Volatile Compounds in Four Commercial Samples of Japanese Green Algae Using Solid Phase Microextraction Gas Chromatography Mass Spectrometry

    Science.gov (United States)

    Yoshikawa, Keisuke; Fujita, Akira; Mase, Nobuyuki; Watanabe, Naoharu

    2014-01-01

    Green algae are of great economic importance. Seaweed is consumed fresh or as seasoning in Japan. The commercial value is determined by quality, color, and flavor and is also strongly influenced by the production area. Our research, based on solid phase microextraction gas chromatography mass spectrometry (SPME-GC-MS), has revealed that volatile compounds differ intensely in the four varieties of commercial green algae. Accordingly, 41 major volatile compounds were identified. Heptadecene was the most abundant compound from Okayama (Ulva prolifera), Tokushima (Ulva prolifera), and Ehime prefecture (Ulva linza). Apocarotenoids, such as ionones, and their derivatives were prominent volatiles in algae from Okayama (Ulva prolifera) and Tokushima prefecture (Ulva prolifera). Volatile, short chained apocarotenoids are among the most potent flavor components and contribute to the flavor of fresh, processed algae, and algae-based products. Benzaldehyde was predominant in seaweed from Shizuoka prefecture (Monostroma nitidum). Multivariant statistical analysis (PCA) enabled simple discrimination of the samples based on their volatile profiles. This work shows the potential of SPME-GC-MS coupled with multivariant analysis to discriminate between samples of different geographical and botanical origins and form the basis for development of authentication methods of green algae products, including seasonings. PMID:24592162

  18. Rational design of heteropolyacid-based nanosorbent for hollow fiber solid phase microextraction of organophosphorus residues in hair samples.

    Science.gov (United States)

    Ebrahimi, Mahmoud; Es'haghi, Zarrin; Samadi, Fatemeh; Bamoharram, Fatemeh Farrash; Hosseini, Mohammad-Saeid

    2012-02-17

    A novel heteropolyacid-based supported ionic liquid (IL) mediated sol-gel hybrid organic-inorganic material is presented for effective use in hollow fiber solid phase microextraction (HF-SPME). We examined a Keggin-based IL that was evaluated in conjunction with sol-gel. This study shows that Keggin-based IL sol-gel generated porous morphology pro effective extraction media. The method was developed for the extraction of the organophosphorus pesticides (OPs); diazinon, fenitrothion and malathion from human hair samples. The OPs were subsequently analyzed with high performance liquid chromatography and photodiode array detection (HPLC-PDA). In the basic condition (pH 10-11), the gel growth process in the presence of IL was initiated. Afterward, this sol was injected into a polypropylene hollow fiber segment for in situ-gelation process. Parameters affecting the efficiency of HF-SPME were thoroughly investigated. Linearity was observed over a range of 0.02-50,000 μg/g and 0.0001-25,000 ng/mL with detection limits between 0.0074-1.3000 μg/g and 0.00034-0.84 ng/mL for the OPs in hair and aqueous matrices, respectively. The relative recoveries in the real samples, for OPs in the storekeeper hair ranged from 86 to 95.2%. Copyright © 2011 Elsevier B.V. All rights reserved.

  19. Determination of volatile compounds in four commercial samples of Japanese green algae using solid phase microextraction gas chromatography mass spectrometry.

    Science.gov (United States)

    Yamamoto, Masayoshi; Baldermann, Susanne; Yoshikawa, Keisuke; Fujita, Akira; Mase, Nobuyuki; Watanabe, Naoharu

    2014-01-01

    Green algae are of great economic importance. Seaweed is consumed fresh or as seasoning in Japan. The commercial value is determined by quality, color, and flavor and is also strongly influenced by the production area. Our research, based on solid phase microextraction gas chromatography mass spectrometry (SPME-GC-MS), has revealed that volatile compounds differ intensely in the four varieties of commercial green algae. Accordingly, 41 major volatile compounds were identified. Heptadecene was the most abundant compound from Okayama (Ulva prolifera), Tokushima (Ulva prolifera), and Ehime prefecture (Ulva linza). Apocarotenoids, such as ionones, and their derivatives were prominent volatiles in algae from Okayama (Ulva prolifera) and Tokushima prefecture (Ulva prolifera). Volatile, short chained apocarotenoids are among the most potent flavor components and contribute to the flavor of fresh, processed algae, and algae-based products. Benzaldehyde was predominant in seaweed from Shizuoka prefecture (Monostroma nitidum). Multivariant statistical analysis (PCA) enabled simple discrimination of the samples based on their volatile profiles. This work shows the potential of SPME-GC-MS coupled with multivariant analysis to discriminate between samples of different geographical and botanical origins and form the basis for development of authentication methods of green algae products, including seasonings.

  20. Determination of Volatile Compounds in Four Commercial Samples of Japanese Green Algae Using Solid Phase Microextraction Gas Chromatography Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Masayoshi Yamamoto

    2014-01-01

    Full Text Available Green algae are of great economic importance. Seaweed is consumed fresh or as seasoning in Japan. The commercial value is determined by quality, color, and flavor and is also strongly influenced by the production area. Our research, based on solid phase microextraction gas chromatography mass spectrometry (SPME-GC-MS, has revealed that volatile compounds differ intensely in the four varieties of commercial green algae. Accordingly, 41 major volatile compounds were identified. Heptadecene was the most abundant compound from Okayama (Ulva prolifera, Tokushima (Ulva prolifera, and Ehime prefecture (Ulva linza. Apocarotenoids, such as ionones, and their derivatives were prominent volatiles in algae from Okayama (Ulva prolifera and Tokushima prefecture (Ulva prolifera. Volatile, short chained apocarotenoids are among the most potent flavor components and contribute to the flavor of fresh, processed algae, and algae-based products. Benzaldehyde was predominant in seaweed from Shizuoka prefecture (Monostroma nitidum. Multivariant statistical analysis (PCA enabled simple discrimination of the samples based on their volatile profiles. This work shows the potential of SPME-GC-MS coupled with multivariant analysis to discriminate between samples of different geographical and botanical origins and form the basis for development of authentication methods of green algae products, including seasonings.

  1. Solid-phase microextraction of methadone in urine samples by electrochemically co-deposited sol-gel/Cu nanocomposite fiber.

    Science.gov (United States)

    Mohammadiazar, Sirwan; Hasanli, Fateme; Maham, Mehdi; Payami Samarin, Somayeh

    2017-08-01

    Electrochemically co-deposited sol-gel/Cu nanocomposites have been introduced as a novel, simple and single-step technique for preparation of solid-phase microextraction (SPME) coating to extract methadone (MDN) (a synthetic opioid) in urine samples. The porous surface structure of the sol-gel/Cu nanocomposite coating was revealed by scanning electron microscopy. Direct immersion SPME followed by HPLC-UV determination was employed. The factors influencing the SPME procedure, such as the salt content, desorption solvent type, pH and equilibration time, were optimized. The best conditions were obtained with no salt content, acetonitrile as desorption solvent type, pH 9 and 10 min equilibration time. The calibration graphs for urine samples showed good linearity. The detection limit was about 0.2 ng mL(-1) . Also, the novel method for preparation of nanocomposite fiber was compared with previously reported techniques for MDN determination. The results show that the novel nanocomposite fiber has relatively high extraction efficiency. Copyright © 2016 John Wiley & Sons, Ltd.

  2. Electrospun polycaprolactam-manganese oxide fiber for headspace-solid phase microextraction of phthalate esters in water samples.

    Science.gov (United States)

    Eskandarpour, Niloufar; Sereshti, Hassan

    2018-01-01

    The nanofibrous polycaprolactam (polyamide 6 (PA6)) incorporated with manganese oxide (MnO) nanoparticles was fabricated by electrospinning and used as a new fiber coating for headspace-solid phase microextraction (HS-SPME) of the selected phthalate esters (PEs) in water samples prior to GC-μECD. The adsorbent was fully characterized using scanning electron microscopy (SEM), Fourier transform-infrared (FT-IR) spectroscopy and thermogravimetric analysis (TGA). The main parameters that affect the HS-SPME efficiency such as extraction temperature, ionic strength, extraction and desorption times were investigated. The analytical figures of merit were obtained under the optimized conditions as follows: linear dynamic range (LDR), 0.500-5.00 × 102 ng mL-1; relative standard deviations (RSDs, n = 3), 1.86-10.9%; limits of detection (LODs), 0.0400-0.193 ng mL-1. The method was applied for determination of the target analytes in river water, bottled water, mineral water and soda samples and the relative recoveries were obtained between 90.3 and 107%. Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. Low-impact sampling under an active solid low-level radioactive waste disposal unit using horizontal drilling technology

    Energy Technology Data Exchange (ETDEWEB)

    Puglisi, C.V.; Vold, E.L.

    1995-12-01

    The purpose of this project was to determine the performance of the solid low-level radioactive waste (LLRW) disposal units located on a mesa top at TA-54, Area G, Los Alamos National Laboratory (LANL), Los Alamos, NM, and to provide in-situ (vadose zone) site characterization information to Area G`s Performance Assessment. The vadose zone beneath an active disposal unit (DU 37), was accessed by utilizing low-impact, air-rotary horizontal drilling technology. Core samples were pulled, via wire-line core method, in 3 horizontal holes fanning out below DU 37 at approximately 5 foot intervals depending on recovery percentage. Samples were surveyed and prepared in-field following Environmental Restoration (ER) guidelines. Samples were transferred from the field to the CST-9 Radvan for initial radiological screening. Following screening, samples were delivered to CST-3 analytical lab for analyses including moisture content, 23 inorganics, 60 volatile organic compounds (VOC`s), 68 semivolatile organic compounds (SVOC`s), tritium, lead 210, radium 226 & 228, cesium 137, isotopic plutonium, americium 241, strontium 90, isotopic uranium, and isotopic thorium. Other analyses included matric potential, alpha spectroscopy, gamma spectroscopy, and gross alpha/beta. The overall results of the analysis identified only tritium as having migrated from the DU. Am-241, Eu-152, and Pu-238 were possibly identified above background but the results are not definitive. Of all organics analysed for, only ethyl acetate was tentatively identified slightly above background. All inorganics were found to be well below regulatory limits. Based on the results of the above mentioned analyses, it was determined that Area G`s disposal units are performing well and no significant liquid phase migration of contaminants has occurred.

  4. Sample Selected Averaging Method for Analyzing the Event Related Potential

    Science.gov (United States)

    Taguchi, Akira; Ono, Youhei; Kimura, Tomoaki

    The event related potential (ERP) is often measured through the oddball task. On the oddball task, subjects are given “rare stimulus” and “frequent stimulus”. Measured ERPs were analyzed by the averaging technique. In the results, amplitude of the ERP P300 becomes large when the “rare stimulus” is given. However, measured ERPs are included samples without an original feature of ERP. Thus, it is necessary to reject unsuitable measured ERPs when using the averaging technique. In this paper, we propose the rejection method for unsuitable measured ERPs for the averaging technique. Moreover, we combine the proposed method and Woody's adaptive filter method.

  5. Comparison of DNA preservation methods for environmental bacterial community samples

    Science.gov (United States)

    Gray, Michael A.; Pratte, Zoe A.; Kellogg, Christina A.

    2013-01-01

    Field collections of environmental samples, for example corals, for molecular microbial analyses present distinct challenges. The lack of laboratory facilities in remote locations is common, and preservation of microbial community DNA for later study is critical. A particular challenge is keeping samples frozen in transit. Five nucleic acid preservation methods that do not require cold storage were compared for effectiveness over time and ease of use. Mixed microbial communities of known composition were created and preserved by DNAgard™, RNAlater®, DMSO–EDTA–salt (DESS), FTA® cards, and FTA Elute® cards. Automated ribosomal intergenic spacer analysis and clone libraries were used to detect specific changes in the faux communities over weeks and months of storage. A previously known bias in FTA® cards that results in lower recovery of pure cultures of Gram-positive bacteria was also detected in mixed community samples. There appears to be a uniform bias across all five preservation methods against microorganisms with high G + C DNA. Overall, the liquid-based preservatives (DNAgard™, RNAlater®, and DESS) outperformed the card-based methods. No single liquid method clearly outperformed the others, leaving method choice to be based on experimental design, field facilities, shipping constraints, and allowable cost.

  6. SURVEY OF HEAVY METALS CONCENTRATION IN MUNICIPAL SOLID WASTES LEACHATE OF ISFAHAN CITY AND THEIR REDUCTION METHOD

    Directory of Open Access Journals (Sweden)

    A.A.R PARVARESH

    2001-12-01

    Full Text Available Introduction In duration steps of collection, transfer and disposal of solid wastes and also change of solid wastes to compost, produced leachate includes various pollutants such as heavy metals. The amounts of heavy metals don"t easily degrate in environment and would be concentrated in food chain and caused many problems for environment and human. Thus, the goal of present research is to investigation of heavy metals concentration in municipal solid wastes leachate of Isfahan city and reduction method for this case. Methods. leachate from four transfer station and composting plant was sampled ten times and in the first stage, quality of samples was evaluated from pH, COD, total solids (TS, total volatile solids (TYS, total fixed solids (TFS and heavy metals such as Cadmium, Chromium, Zinc, Copper and Nickel viewpoints. Chemical coagulants such as lime, alum and ferric chloride were applied using the Jar test to reduce heavy metals concentration. Results. The results revealed that mean concentration of heavy metals Cd, Cr. Zn Cu and Ni in leachate was equal to 0.63, 1.22, 7.42, 2.15 and 2.22 mg/l respectively and also the results of statistical analysis (ANOVA showed no significant difference between heavy metals concentration in various stations (P > 0.05. The results of Jar test revealed that optimum pH for chemical precipitation, and also optimum concentration of the three coagulants were 2400, 1400 and 1000 mg/l respectively. Discussion. Under this study elements concentration of leachate as compared with effluent standard (Environmental Protection Agency were exceeded the limits. Alum with 75-95 percent removal has the highest effciency as compared to other coagulants, lime with 70-88 percent removal and ferric chloride with 65-85 percent removal are in next order. Erom economical aspect, lime is cost benefit, ferric chloride and alum are in raked next respectively.

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

    Science.gov (United States)

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

    2017-10-09

    Often in hair analysis, a small hair sample is available while the analysis of a multitude of structurally diverse substances with different concentration ranges is demanded. The analysis of the different substances often requires different sample preparation methods, increasing the amount of required hair sample. When segmental hair analysis is necessary, the amount of hair sample needed is further increased. Therefore, the required sample amount for a full analysis can quickly exceed what is available. To combat this problem, a method for the combined hair sample preparation using a single extraction procedure for analysis of ethyl glucuronide with liquid chromatography-multistage fragmentation mass spectrometry/multiple reaction monitoring (LC-MS3 /MRM) and common drugs of abuse with LC-MRM was developed. The combined sample preparation is achieved by separating ethyl glucuronide from the drugs of abuse into separate extracts by fractionation in the solid-phase extraction step during sample clean-up. A full validation for all substances for the parameters selectivity, linearity, limit of detection, limit of quantification, accuracy, precision, matrix effects, and recovery was successfully completed. The following drugs of abuse were included in the method: Amphetamine; methamphetamine; 3,4-methylenedioxy-N-methylamphetamine (MDMA); 3,4-methylenedioxyamphetamine (MDA); 3,4-methylenedioxy-N-ethylamphetamine (MDE); morphine; 6-monoacetylmorphine; codeine; acetylcodeine; cocaine; benzoylecgonine; norcocaine; cocaethylene; methadone; 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP) and methylphenidate. In conclusion, as only 1 sample preparation is needed with 1 aliquot of hair, the presented sample preparation allows an optimal analysis of both ethyl glucuronide and of the drugs of abuse, even when the sample amount is a limiting factor. Copyright © 2017 John Wiley & Sons, Ltd.

  8. Transuranic waste characterization sampling and analysis methods manual. Revision 1

    Energy Technology Data Exchange (ETDEWEB)

    Suermann, J.F.

    1996-04-01

    This Methods Manual provides a unified source of information on the sampling and analytical techniques that enable Department of Energy (DOE) facilities to comply with the requirements established in the current revision of the Transuranic Waste Characterization Quality Assurance Program Plan (QAPP) for the Waste Isolation Pilot Plant (WIPP) Transuranic (TRU) Waste Characterization Program (the Program) and the WIPP Waste Analysis Plan. This Methods Manual includes all of the testing, sampling, and analytical methodologies accepted by DOE for use in implementing the Program requirements specified in the QAPP and the WIPP Waste Analysis Plan. The procedures in this Methods Manual are comprehensive and detailed and are designed to provide the necessary guidance for the preparation of site-specific procedures. With some analytical methods, such as Gas Chromatography/Mass Spectrometry, the Methods Manual procedures may be used directly. With other methods, such as nondestructive characterization, the Methods Manual provides guidance rather than a step-by-step procedure. Sites must meet all of the specified quality control requirements of the applicable procedure. Each DOE site must document the details of the procedures it will use and demonstrate the efficacy of such procedures to the Manager, National TRU Program Waste Characterization, during Waste Characterization and Certification audits.

  9. Sequential injection system incorporating a micro extraction column for automatic fractionation of metal ions in solid samples

    DEFF Research Database (Denmark)

    Chomchoei, Roongrat; Miró, Manuel; Hansen, Elo Harald

    2005-01-01

    Recently a novel approach to perform sequential extractions (SE) of elements in solid samples was developed by this group, based upon the use of a sequential injection (SI) system incorporating a specially designed extraction microcolumn. Entailing a number of distinct advantages as compared to c...

  10. Analysis of permethrin isomers in composite diet samples by molecularly imprinted solid-phase extraction and isotope dilution gas chromatography-ion trap mass spectrometry.

    Science.gov (United States)

    Vonderheide, Anne P; Boyd, Brian; Ryberg, Anna; Yilmaz, Ecevit; Hieber, Thomas E; Kauffman, Peter E; Garris, Sherry T; Morgan, Jeffrey N

    2009-05-29

    Determination of an individual's aggregate dietary ingestion of pesticides entails analysis of a difficult sample matrix. Permethrin-specific molecularly imprinted polymer (MIP) solid-phase extraction cartridges were developed for use as a sample preparation technique for a composite food matrix. Vortexing with acetonitrile and centrifugation were found to provide optimal extraction of the permethrin isomers from the composite foods. The acetonitrile (with 1% acetic acid) was mostly evaporated and the analytes reconstituted in 90:10 water/acetonitrile in preparation for molecularly imprinted solid-phase extraction. Permethrin elution was accomplished with acetonitrile and sample extracts were analyzed by isotope dilution gas chromatography-ion trap mass spectrometry. Quantitation of product ions provided definitive identification of the pesticide isomers. The final method parameters were tested with fortified composite food samples of varying fat content (1%, 5%, and 10%) and recoveries ranged from 99.3% to 126%. Vegetable samples with incurred pesticide levels were also analyzed with the given method and recoveries were acceptable (81.0-95.7%). Method detection limits were demonstrated in the low ppb range. Finally, the applicability of the MIP stationary phase to extract other pyrethroids, specifically cyfluthrin and cypermethrin, was also investigated.

  11. Development of an automated data processing method for sample to sample comparison of seized methamphetamines.

    Science.gov (United States)

    Choe, Sanggil; Lee, Jaesin; Choi, Hyeyoung; Park, Yujin; Lee, Heesang; Pyo, Jaesung; Jo, Jiyeong; Park, Yonghoon; Choi, Hwakyung; Kim, Suncheun

    2012-11-30

    The information about the sources of supply, trafficking routes, distribution patterns and conspiracy links can be obtained from methamphetamine profiling. The precursor and synthetic method for the clandestine manufacture can be estimated from the analysis of minor impurities contained in methamphetamine. Also, the similarity between samples can be evaluated using the peaks that appear in chromatograms. In South Korea, methamphetamine was the most popular drug but the total seized amount of methamphetamine whole through the country was very small. Therefore, it would be more important to find the links between samples than the other uses of methamphetamine profiling. Many Asian countries including Japan and South Korea have been using the method developed by National Research Institute of Police Science of Japan. The method used gas chromatography-flame ionization detector (GC-FID), DB-5 column and four internal standards. It was developed to increase the amount of impurities and minimize the amount of methamphetamine. After GC-FID analysis, the raw data have to be processed. The data processing steps are very complex and require a lot of time and effort. In this study, Microsoft Visual Basic Application (VBA) modules were developed to handle these data processing steps. This module collected the results from the data into an Excel file and then corrected the retention time shift and response deviation generated from the sample preparation and instruments analysis. The developed modules were tested for their performance using 10 samples from 5 different cases. The processed results were analyzed with Pearson correlation coefficient for similarity assessment and the correlation coefficient of the two samples from the same case was more than 0.99. When the modules were applied to 131 seized methamphetamine samples, four samples from two different cases were found to have the common origin and the chromatograms of the four samples were appeared visually identical

  12. Determination of artificial sweeteners in water samples by solid-phase extraction and liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Ordóñez, Edgar Y; Quintana, José Benito; Rodil, Rosario; Cela, Rafael

    2012-09-21

    The development and performance evaluation of an analytical method for the determination of six artificial sweeteners in environmental waters using solid-phase extraction (SPE) followed by liquid chromatography-tandem mass spectrometry are presented. To this end, different SPE alternatives have been evaluated: polymeric reversed-phase (Oasis HLB, Env+, Plexa and Strata X), and mixed-mode with either weak (Oasis WAX) or strong anionic-exchange (Oasis MAX and Plexa PAX) sorbents. Among them, reversed-phase sorbents, particularly Oasis HLB and Strata X, showed the best performance. Oasis HLB provided good trueness (recoveries: 73-112%), precision (RSD<10%) and limits of quantification (LOQ: 0.01-0.5 μg/L). Moreover, two LC separation mechanisms were evaluated: reversed-phase (RPLC) and hydrophilic interaction (HILIC), with RPLC providing better performance than HILIC. The final application of the method showed the presence of acesulfame, cyclamate, saccharin and sucralose in the wastewater and surface water samples analyzed at concentrations up to 54 μg/L. Copyright © 2012 Elsevier B.V. All rights reserved.

  13. Standard methods for sampling freshwater fishes: Opportunities for international collaboration

    Science.gov (United States)

    Bonar, Scott A.; Mercado-Silva, Norman; Hubert, Wayne A.; Beard, Douglas; Dave, Göran; Kubečka, Jan; Graeb, Brian D. S.; Lester, Nigel P.; Porath, Mark T.; Winfield, Ian J.

    2017-01-01

    With publication of Standard Methods for Sampling North American Freshwater Fishes in 2009, the American Fisheries Society (AFS) recommended standard procedures for North America. To explore interest in standardizing at intercontinental scales, a symposium attended by international specialists in freshwater fish sampling was convened at the 145th Annual AFS Meeting in Portland, Oregon, in August 2015. Participants represented all continents except Australia and Antarctica and were employed by state and federal agencies, universities, nongovernmental organizations, and consulting businesses. Currently, standardization is practiced mostly in North America and Europe. Participants described how standardization has been important for management of long-term data sets, promoting fundamental scientific understanding, and assessing efficacy of large spatial scale management strategies. Academics indicated that standardization has been useful in fisheries education because time previously used to teach how sampling methods are developed is now more devoted to diagnosis and treatment of problem fish communities. Researchers reported that standardization allowed increased sample size for method validation and calibration. Group consensus was to retain continental standards where they currently exist but to further explore international and intercontinental standardization, specifically identifying where synergies and bridges exist, and identify means to collaborate with scientists where standardization is limited but interest and need occur.

  14. Soybean yield modeling using bootstrap methods for small samples

    Energy Technology Data Exchange (ETDEWEB)

    Dalposso, G.A.; Uribe-Opazo, M.A.; Johann, J.A.

    2016-11-01

    One of the problems that occur when working with regression models is regarding the sample size; once the statistical methods used in inferential analyzes are asymptotic if the sample is small the analysis may be compromised because the estimates will be biased. An alternative is to use the bootstrap methodology, which in its non-parametric version does not need to guess or know the probability distribution that generated the original sample. In this work we used a set of soybean yield data and physical and chemical soil properties formed with fewer samples to determine a multiple linear regression model. Bootstrap methods were used for variable selection, identification of influential points and for determination of confidence intervals of the model parameters. The results showed that the bootstrap methods enabled us to select the physical and chemical soil properties, which were significant in the construction of the soybean yield regression model, construct the confidence intervals of the parameters and identify the points that had great influence on the estimated parameters. (Author)

  15. Analytical determination of Chemical Oxygen Demand in samples considered to be difficult to analyse: solid substrates and liquid samples with high suspended solid concentrations

    DEFF Research Database (Denmark)

    Raposo, Francisco; Fernández-Cegrí, V.; De la Rubia, M.A.

    Chemical oxygen demand (COD) is a critical analytical parameter in the field of waste and wastewater treatment processes, and more specifically in anaerobic digestion processes. However, little is known about the COD measurement quality of anaerobic digestion samples. Taking into account the lack...

  16. A headspace solid-phase microextraction procedure coupled with gas chromatography-mass spectrometry for the analysis of volatile polycyclic aromatic hydrocarbons in milk samples

    Energy Technology Data Exchange (ETDEWEB)

    Aguinaga, N.; Campillo, N.; Vinas, P.; Hernandez-Cordoba, M. [University of Murcia, Department of Analytical Chemistry, Faculty of Chemistry, Murcia (Spain)

    2008-06-15

    A sensitive and solvent-free method for the determination of ten polycyclic aromatic hydrocarbons, namely, naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo[a]anthracene and chrysene, with up to four aromatic rings, in milk samples using headspace solid-phase microextraction and gas chromatography-mass spectrometry detection has been developed. A polydimethylsiloxane-divinylbenzene fiber was chosen and used at 75 C for 60 min. Detection limits ranging from 0.2 to 5 ng L{sup -1} were attained at a signal-to-noise ratio of 3, depending on the compound and the milk sample under analysis. The proposed method was applied to ten different milk samples and the presence of six of the analytes studied in a skimmed milk with vegetal fiber sample was confirmed. The reliability of the procedure was verified by analyzing two different certified reference materials and by recovery studies. (orig.)

  17. Eosinophilia in routine blood samples as a biomarker for solid tumor development - A study based on the Copenhagen Primary Care Differential Count (CopDiff) Database

    DEFF Research Database (Denmark)

    Andersen, Christen Lykkegaard; Siersma, Volkert Dirk; Hasselbalch, Hans Carl

    2014-01-01

    eosinophilia in routine blood samples as a potential biomarker of solid tumor development in a prospective design. MATERIAL AND METHODS: From the Copenhagen Primary Care Differential Count (CopDiff) Database, we identified 356 196 individuals with at least one differential cell count (DIFF) encompassing...... the eosinophil count during 2000-2007. From these, one DIFF was randomly chosen and categorized according to no (... was increased with mild eosinophilia [OR 1.93 (CI 1.29-2.89), p = 0.0013]. No associations with eosinophilia were observed for the remaining solid cancers. CONCLUSION: We demonstrate that eosinophilia in routine blood samples associates with an increased risk of bladder cancer. Our data emphasize...

  18. Determination of cadmium and zinc in fertilizer samples by FAAS after solid-phase extraction with freshly precipitated manganese-diethyldithiocarbamate.

    Science.gov (United States)

    Cesur, Hasan; Aksu, Cigdem

    2006-05-01

    Using freshly precipitated manganese-diethyldithiocarbamate (Mn(DDTC)(2)) as a new reagent, a solid phase extraction method (SPE) has been developed for the extraction of Cd(II) and Zn(II) in aqueous fertilizer samples. A sample solution of 300 mL was taken and 0.10 g of freshly precipitated Mn(DDTC)(2) was added. After adding a phosphate buffer solution, the mixture was stirred at 10 min, filtered with a glass filter and washed with deionized water. The solid product containing Mn(DDTC)(2)-Cd(DDTC)(2)-Zn(DDTC)(2) complexes was dissolved in concentrated nitric acid and its volume was made complete up to 10 mL with deionized water. The metal contents of the solution were measured by an atomic-absorption spectrometer.

  19. Rapid analysis of phthalates in beverage and alcoholic samples by multi-walled carbon nanotubes/silica reinforced hollow fibre-solid phase microextraction.

    Science.gov (United States)

    Li, Jia; Su, Qiong; Li, Ke-Yao; Sun, Chu-Feng; Zhang, Wen-Bo

    2013-12-15

    A novel procedure based on multi-walled carbon nanotubes (MWCNTs)/silica reinforced hollow fibre solid-phase microextraction combined with gas chromatography-mass spectrometry has been developed to analyse trace phthalate acid esters in beverage and alcoholic samples. Because of their excellent adsorption capability towards hydrophobic compounds, functionalized MWCNTs, acting as solid-phase sorbent, were co-deposited with silica particles in the pores of polypropylene hollow fibre through a layer-by-layer self-assembly technique. The parameters influencing the extraction efficiency, such as pH values and ionic strength of sample solution, extraction time, temperature and desorption solvent were optimised. Recoveries for phthalates at spiking levels in different matrices were satisfactory (between 68% and 115%). Moreover, the results were further confirmed by comparing them with those obtained using a solvent extraction method according to the national standard of China. Copyright © 2013 Elsevier Ltd. All rights reserved.

  20. Preparation and selective recognition of a novel solid-phase microextraction fiber combined with molecularly imprinted polymers for the extraction of parabens in soy sample.

    Science.gov (United States)

    He, Juan; Chen, Si; Jiang, Yili; Shen, Yanzheng; Zhu, Jing; Wei, Hongliang; Zhang, Hongxia; Lu, Kui

    2012-01-01

    A prepared molecularly imprinted polymer with ethyl p-hydroxybenzoate as template molecule was applied for the first time to a homemade solid-phase microextraction fiber. The molecularly imprinted polymer-coated solid-phase microextraction fiber was characterized by scanning electron microscopy and thermogravimetric analysis. Various parameters were investigated, including extraction temperature, extraction time, and desorption time. Under the optimum extraction conditions, the molecularly imprinted polymer-coated solid-phase microextraction fiber exhibited higher selectivity with greater extraction capacity toward parabens compared with the nonimprinted polymer-coated solid-phase microextraction fiber and commercial fibers. The molecularly imprinted polymer-coated solid-phase microextraction fiber was tested using gas chromatography to determine parabens, including methyl p-hydroxybenzoate, ethyl p-hydroxybenzoate, and propyl p-hydroxybenzoate. The linear ranges were 0.01-10 μg/mL with a correlation coefficient above 0.9943. The detection limits (under signal-to-noise ratio of 3) were below 0.30 μg/L. The fiber was successfully applied to the simultaneous analysis of three parabens in spiked soy samples with satisfactory recoveries of 95.48, 97.86, and 92.17%, respectively. The relative standard deviations (n=6) were within 2.83-3.91%. The proposed molecularly imprinted polymer-coated solid-phase microextraction method is suitable for selective extraction and determination of trace parabens in food samples. Copyright © 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. A Novel Fast Method for Point-sampled Model Simplification

    Directory of Open Access Journals (Sweden)

    Cao Zhi

    2016-01-01

    Full Text Available A novel fast simplification method for point-sampled statue model is proposed. Simplifying method for 3d model reconstruction is a hot topic in the field of 3D surface construction. But it is difficult as point cloud of many 3d models is very large, so its running time becomes very long. In this paper, a two-stage simplifying method is proposed. Firstly, a feature-preserved non-uniform simplification method for cloud points is presented, which simplifies the data set to remove the redundancy while keeping down the features of the model. Secondly, an affinity clustering simplifying method is used to classify the point cloud into a sharp point or a simple point. The advantage of Affinity Propagation clustering is passing messages among data points and fast speed of processing. Together with the re-sampling, it can dramatically reduce the duration of the process while keep a lower memory cost. Both theoretical analysis and experimental results show that after the simplification, the performance of the proposed method is efficient as well as the details of the surface are preserved well.

  2. The Sensitivity of Respondent-driven Sampling Method

    CERN Document Server

    Lu, Xin; Britton, Tom; Camitz, Martin; Kim, Beom Jun; Thorson, Anna; Liljeros, Fredrik

    2012-01-01

    Researchers in many scientific fields make inferences from individuals to larger groups. For many groups however, there is no list of members from which to take a random sample. Respondent-driven sampling (RDS) is a relatively new sampling methodology that circumvents this difficulty by using the social networks of the groups under study. The RDS method has been shown to provide unbiased estimates of population proportions given certain conditions. The method is now widely used in the study of HIV-related high-risk populations globally. In this paper, we test the RDS methodology by simulating RDS studies on the social networks of a large LGBT web community. The robustness of the RDS method is tested by violating, one by one, the conditions under which the method provides unbiased estimates. Results reveal that the risk of bias is large if networks are directed, or respondents choose to invite persons based on characteristics that are correlated with the study outcomes. If these two problems are absent, the RD...

  3. RAPID SEPARATION METHOD FOR ACTINIDES IN EMERGENCY SOIL SAMPLES

    Energy Technology Data Exchange (ETDEWEB)

    Maxwell, S.; Culligan, B.; Noyes, G.

    2009-11-09

    A new rapid method for the determination of actinides in soil and sediment samples has been developed at the Savannah River Site Environmental Lab (Aiken, SC, USA) that can be used for samples up to 2 grams in emergency response situations. The actinides in soil method utilizes a rapid sodium hydroxide fusion method, a lanthanum fluoride soil matrix removal step, and a streamlined column separation process with stacked TEVA, TRU and DGA Resin cartridges. Lanthanum was separated rapidly and effectively from Am and Cm on DGA Resin. Vacuum box technology and rapid flow rates are used to reduce analytical time. Alpha sources are prepared using cerium fluoride microprecipitation for counting by alpha spectrometry. The method showed high chemical recoveries and effective removal of interferences. This new procedure was applied to emergency soil samples received in the NRIP Emergency Response exercise administered by the National Institute for Standards and Technology (NIST) in April, 2009. The actinides in soil results were reported within 4-5 hours with excellent quality.

  4. Environmentally Friendly Method: Development and Application to Carbon Aerogel as Sorbent for Solid-Phase Extraction.

    Science.gov (United States)

    Dong, Sheying; Huang, Guiqi; Su, Meiling; Huang, Tinglin

    2015-10-14

    We developed two simple, fast, and environmentally friendly methods using carbon aerogel (CA) and magnetic CA (mCA) materials as sorbents for micro-solid-phase extraction (μ-SPE) and magnetic solid-phase extraction (MSPE) techniques. The material performances such as adsorption isotherm, adsorption kinetics, and specific surface area were discussed by N2 adsorption-desorption isotherm measurements, ultraviolet and visible (UV-vis) spectrophotometry, scanning electron microscopy (SEM), and high resolution transmission electron microscopy (HR-TEM). The experimental results proved that the heterogeneities of CA and mCA were well modeled with the Freundlich isotherm model, and the sorption process well followed the pseudo-second-order rate equation. Moreover, plant growth regulators (PGRs) such as kinetin (6-KT), 6-benzylaminopurine (6-BA), 2,4-dichlorophenoxyacetic acid (2,4-D), and uniconazole (UN) in a reservoir raw water sample were selected as the evaluation of applicability for the proposed μ-SPE and MSPE techniques using high performance liquid chromatography (HPLC). The experimental conditions of two methods such as the amount of sorbent, extraction time, pH, salt concentration, and desorption conditions were studied. Under the optimized conditions, two extraction methods provided high recoveries (89-103%), low the limits of detection (LODs) (0.01-0.2 μg L(-1)), and satisfactory analytical features in terms of precision (relative standard deviation, RSD, 1.7-5.1%, n=3). This work demonstrates the feasibility and the potential of CA and mCA materials as sorbents for μ-SPE and MSPE techniques. Besides, it also could serve as a basis for future development of other functional CAs in pretreatment technology and make them valuable for analysis of pollutants in environmental applications.

  5. Marine sediments monitoring studies for trace elements with the application of fast temperature programs and solid sampling high resolution continuum source atomic absorption spectrometry

    Science.gov (United States)

    Orani, Anna Maria; Han, Eunmi; Mandjukov, Petko; Vassileva, Emilia

    2015-01-01

    Analytical procedure for the determination of As, Cd, Cu, Ni, Co and Cr in marine sediment samples using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS AAS) and direct solid sample analysis has been developed. The application of fast programs in combination with direct solid sampling allows to eliminate the drying and pretreatment steps, however makes impossible the use of liquid standards for calibration. Iridium treated platforms were applied throughout the present study. Calibration technique based on the use of solid certified reference materials (marine sediments) similar to the nature of the analyzed sample and statistics of regression analysis were applied to the real sediment samples. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signals. The ISO-17025 requirements and Eurachem guidelines were followed in the validation of the proposed analytical procedure. Accordingly, blanks, selectivity, calibration, linearity, working range, trueness, repeatability reproducibility, limits of detection and quantification and expanded uncertainty (k = 2) for all investigated elements were assessed. Two different approaches for the estimation of measurement uncertainty were applied and obtained results compared. The major contributors to the combined uncertainty of the analyte mass fraction were found to be the homogeneity of the samples and the microbalance precision. The influence of sample particle sizes on the total combined uncertainty was also evaluated. Traceability to SI system of units of the obtained by the proposed analytical procedure results was demonstrated. Additionally, validation of the methodology developed was effectuated by the comparison of the obtained results with independent method e.g. ICP-MS with external calibration. The use of solid sampling HR CS AAS for the determination of trace elements in marine sediment matrix gives significant advantages

  6. Organic solid state optical switches and method for producing organic solid state optical switches

    Energy Technology Data Exchange (ETDEWEB)

    Wasielewski, M.R.; Gaines, G.L.; Niemczyk, M.P.; Johnson, D.G.; Gosztola, D.J.; O`Neil, M.P.

    1993-01-01

    This invention consists of a light-intensity dependent molecular switch comprised of a compound which shuttles an electron or a plurality of electrons from a plurality of electron donors to an electron acceptor upon being stimulated with light of predetermined wavelengths, and a method for making said compound.

  7. Luminescence studies on the europium doped strontium metasilicate phosphor prepared by solid state reaction method

    Directory of Open Access Journals (Sweden)

    Ishwar Prasad Sahu

    2017-03-01

    Full Text Available Europium doped strontium meta-silicate (namely SrSiO3:Eu3+ phosphor was prepared by a high temperature solid state reaction method. The sintered SrSiO3:Eu3+ phosphor possesses a monoclinic structure by the XRD. Energy dispersive X-ray spectrum (EDS confirms the presence of elements in the desired sample. Thermoluminescence (TL kinetic parameters such as activation energy (E, order of kinetics (b, and frequency factor (s were calculated by the peak shape method. The orange–red emission was shown to originate from the 5D0–7FJ (J = 0, 1, 2, 3, 4 transitions of Eu3+ ions as the sample was excited at 396 nm. The SrSiO3:Eu3+ phosphor with almost pure orange-red color purity (99.62% shows the quantum efficiency of 10.2% (excited by 396 nm, which is higher than those of commercial red phosphors Y2O3:Eu3+ and Y2O2S:Eu3+ with quantum efficiencies of 9.6% (excited by 394 nm and 4.2% (excited by 395 nm, respectively. Mechanoluminescence (ML intensity of the SrSiO3:Eu3+ phosphor was also found to increase linearly with increasing the impact velocity of the moving piston, suggesting that the discussed phosphor can be used as a stress sensor.

  8. Development and Validation of HPLC Method for Determination of Crocetin, a constituent of Saffron, in Human Serum Samples

    Directory of Open Access Journals (Sweden)

    Amir Hooshang Mohammadpour

    2013-01-01

    Full Text Available Objective(s:The present study reports the development and validation of a sensitive and rapid extraction method beside high performance liquid chromatographic method for the determination of crocetin in human serum. Materials and Methods:The HPLC method was carried out by using a C18 reversed-phase column and a mobile phase composed of methanol/water/acetic acid (85:14.5:0.5 v/v/v at the flow rate of 0.8 ml/min. The UV detector was set at 423 nm and 13-cis retinoic acid was used as the internal standard. Serum samples were pretreated with solid-phase extraction using Bond Elut C18 (200mg cartridges or with direct precipitation using acetonitrile. Results:The calibration curves were linear over the range of 0.05-1.25 µg/ml for direct precipitation method and 0.5-5 µg/ml for solid-phase extraction. The mean recoveries of crocetin over a concentration range of 0.05-5 µg/ml serum for direct precipitation method and 0.5-5 µg/ml for solid-phase extraction were above 70 % and 60 %, respectively. The intraday coefficients of variation were 0.37- 2.6% for direct precipitation method and 0.64 - 5.43% for solid-phase extraction. The inter day coefficients of variation were 1.69 – 6.03% for direct precipitation method and 5.13-12.74% for solid-phase extraction, respectively. The lower limit of quantification for crocetin was 0.05 µg/ml for direct precipitation method and 0.5 µg/ml for solid-phase extraction. Conclusion: The validated direct precipitation method for HPLC satisfied all of the criteria that were necessary for a bioanalytical method and could reliably quantitate crocetin in human serum for future clinical pharmacokinetic study

  9. Thinprep plus Papanicolaou stain method is more sensitive than cytospin-coupled Wright Giems stain method in cerebrospinal fluid cytology for diagnosis of leptomeningeal metastasis from solid tumors.

    Directory of Open Access Journals (Sweden)

    Zhenyu Pan

    Full Text Available The present study was designed to determine whether the Thinprep plus Papanicolaou stain (Thinprep method is more sensitive than the Cytospin-coupled Wright-Giemsa (WG stain (Cytospin method in diagnosis of leptomeningeal metastasis (LM from malignant solid tumors in cerebrospinal fluid (CSF. We also explored if the Thinprep method could be used in the differential diagnosis of the type of primary tumor cells based on the morphology of tumor cells in CSF samples.The morphological features of tumor cells in fresh CSF samples were analyzed using both methods. The tumor cell detection rates were compared between the two methods.Using the Thinprep method, we found that each type of tumor cells in the CSF samples had specific identifiable morphological features linked to their primary cancer origins, such as adenocarcinomas originated from the lungs, breast, and stomach, and lung squamous cell carcinomas, small cell lung cancer, large-cell neuroendocrine lung cancer, hepatocellular carcinoma, and malignant melanoma. In a retrospective study with 88 LM patients, cancer cells were detected in 80 out of the 88 CSF samples. In the comparative study with 45 LM patients, the initial detection rate of the Thinprep method was significantly higher than that of the Cytospin method (73.3% vs. 57.8%, P<0.01. The cell morphology was better preserved and subcellular structures were clearer using the Thinprep method, compared to the Cytospin method.The Thinprep method is more sensitive and suitable for LM diagnosis in CSF in patients with malignant solid tumors than the Cytospin method. The Thinprep method may facilitate primary tumor detection and help design early treatment regimens for LM patients with tumors of unknown primary origin.

  10. A direct sampling method to an inverse medium scattering problem

    KAUST Repository

    Ito, Kazufumi

    2012-01-10

    In this work we present a novel sampling method for time harmonic inverse medium scattering problems. It provides a simple tool to directly estimate the shape of the unknown scatterers (inhomogeneous media), and it is applicable even when the measured data are only available for one or two incident directions. A mathematical derivation is provided for its validation. Two- and three-dimensional numerical simulations are presented, which show that the method is accurate even with a few sets of scattered field data, computationally efficient, and very robust with respect to noises in the data. © 2012 IOP Publishing Ltd.

  11. Microextraction Methods for Preconcentration of Aluminium in Urine Samples

    Directory of Open Access Journals (Sweden)

    Farzad Farajbakhsh, Mohammad Amjadi, Jamshid Manzoori, Mohammad R. Ardalan, Abolghasem Jouyban

    2016-07-01

    Full Text Available Background: Analysis of aluminium (Al in urine samples is required in management of a number of diseases including patients with renal failure. This work aimed to present dispersive liquid-liquid microextraction (DLLME and ultrasound-assisted emulsification microextraction (USAEME methods for the preconcentration of ultra-trace amount of aluminum in human urine prior to its determination by a graphite furnace atomic absorption spectrometry (GFAAS. Methods: The microextraction methods were based on the complex formation of Al3+ with 8-hydroxyquinoline. The effect of various experimental parameters on the efficiencies of the methods and their optimum values were studied. Results: Under the optimal conditions, the limits of detection for USAEME-GFAAS and DLLME-GFAAS were 0.19 and 0.30 ng mL−1, respectively and corresponding relative standard deviations (RSD, n=5 for the determination of 40 ng mL−1 Al3+ were 5.9% and 4.9%. Conclusion: Both methods could be successfully used to the analysis of ultra trace concentrations of Al in urine samples of dialysis patients.

  12. Testing K. Patrick Method of Psychopathy Diagnosis in Russian Sample

    Directory of Open Access Journals (Sweden)

    Atadzhykova Y.A.,

    2015-12-01

    Full Text Available The article is devoted to the development of a method of diagnosing psychopathy, or antisocial (dissocial personality disorder. Modern researchers mostly use the methods of experiment, expert assessment, clinical interview or different combinations for personality disorders, including psychopathy. However, nowadays there is a growing need in development of a psychopathy diagnosis method which would be less labour-intensive, less expensive and more objective. One of the recently developed models of psychopathy is Trierarchic conceptualization by C. Patrick, it offers a new way to operationalize and diagnose psychopathy. The authors had tested this method in the Russian population, including both common sample as well as criminal offender sample consisting of individuals that have been suspected, accused or convicted of violent crimes. The subject of the current research is psychopathic traits measured by the tested method. We had carried out statistical and content analyzes of the data. Our study allowed to conclude that tested Russian version of the Triarchic Psychopathy Measure is effective enough to be used for research purposes. However, further research is required in order to render this measure valid to practical use.

  13. Vortex-homogenized matrix solid-phase dispersion for the extraction of short chain chlorinated paraffins from indoor dust samples.

    Science.gov (United States)

    Chen, Yu-Hsuan; Chang, Chia-Yu; Ding, Wang-Hsien

    2016-11-11

    A simple and effective method for determining short chain chlorinated paraffins (SCCPs) in indoor dust is presented. The method employed a modified vortex-homogenized matrix solid-phase dispersion (VH-MSPD) prior to its detection by gas chromatography - electron-capture negative-ion mass spectrometry (GC-ECNI-MS) operating in the selected-ion-monitoring (SIM) mode. Under the best extraction conditions, 0.1-g of dust sample was dispersed with 0.1-g of silica gel by using vortex (2min) instead of using a mortar and pestle (3min). After that step, the blend was transferred to a glass column containing 3-g acidic silica gel, 2-g basic silica gel, and 2-g of deactivated silica gel, used as clean-up co-sorbents. Then, target analytes were eluted with 5mL of n-hexane/dichloromethane (2:1, v/v) mixture. The extract was evaporated to dryness under a gentle stream of nitrogen. The residue was then re-dissolved in n-hexane (10μL), and subjected to GC-ECNI-MS analysis. The limits of quantitation (LOQs) ranged from 0.06 to 0.25μg/g for each SCCP congener. Precision was less than 7% for both intra- and inter-day analysis. Trueness was above 89%, which was calculated by mean extraction recovery. The VH-MSPD combined with GC-ECNI-MS was successfully applied to quantitatively detect SCCPs from various indoor dust samples, and the concentrations ranged from 1.2 to 31.2μg/g. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Angoff's delta method revisited: improving DIF detection under small samples.

    Science.gov (United States)

    Magis, David; Facon, Bruno

    2012-05-01

    Most methods for detecting differential item functioning (DIF) are suitable when the sample sizes are sufficiently large to validate the null statistical distributions. There is no guarantee, however, that they will still perform adequately when there are few respondents in the focal group or in both the reference and the focal group. Angoff's delta plot is a potentially useful alternative for small-sample DIF investigation, but it suffers from an improper DIF flagging criterion. The purpose of this paper is to improve this classification rule under mild statistical assumptions. This improvement yields a modified delta plot with an adjusted DIF flagging criterion for small samples. A simulation study was conducted to compare the modified delta plot with both the classical delta plot approach and the Mantel-Haenszel method. It is concluded that the modified delta plot is consistently less conservative and more powerful than the usual delta plot, and is also less conservative and more powerful than the Mantel-Haenszel method as long as at least one group of respondents is small. ©2011 The British Psychological Society.

  15. Gravimetric water distribution assessment from geoelectrical methods (ERT and EMI) in municipal solid waste landfill.

    Science.gov (United States)

    Dumont, Gaël; Pilawski, Tamara; Dzaomuho-Lenieregue, Phidias; Hiligsmann, Serge; Delvigne, Frank; Thonart, Philippe; Robert, Tanguy; Nguyen, Frédéric; Hermans, Thomas

    2016-09-01

    The gravimetric water content of the waste material is a key parameter in waste biodegradation. Previous studies suggest a correlation between changes in water content and modification of electrical resistivity. This study, based on field work in Mont-Saint-Guibert landfill (Belgium), aimed, on one hand, at characterizing the relationship between gravimetric water content and electrical resistivity and on the other hand, at assessing geoelectrical methods as tools to characterize the gravimetric water distribution in a landfill. Using excavated waste samples obtained after drilling, we investigated the influences of the temperature, the liquid phase conductivity, the compaction and the water content on the electrical resistivity. Our results demonstrate that Archie's law and Campbell's law accurately describe these relationships in municipal solid waste (MSW). Next, we conducted a geophysical survey in situ using two techniques: borehole electromagnetics (EM) and electrical resistivity tomography (ERT). First, in order to validate the use of EM, EM values obtained in situ were compared to electrical resistivity of excavated waste samples from corresponding depths. The petrophysical laws were used to account for the change of environmental parameters (temperature and compaction). A rather good correlation was obtained between direct measurement on waste samples and borehole electromagnetic data. Second, ERT and EM were used to acquire a spatial distribution of the electrical resistivity. Then, using the petrophysical laws, this information was used to estimate the water content distribution. In summary, our results demonstrate that geoelectrical methods represent a pertinent approach to characterize spatial distribution of water content in municipal landfills when properly interpreted using ground truth data. These methods might therefore prove to be valuable tools in waste biodegradation optimization projects. Copyright © 2016 Elsevier Ltd. All rights reserved.

  16. Radiochemistry methods in DOE methods for evaluating environmental and waste management samples

    Energy Technology Data Exchange (ETDEWEB)

    Fadeff, S.K.; Goheen, S.C.

    1994-08-01

    Current standard sources of radiochemistry methods are often inappropriate for use in evaluating US Department of Energy environmental and waste management (DOE/EW) samples. Examples of current sources include EPA, ASTM, Standard Methods for the Examination of Water and Wastewater and HASL-300. Applicability of these methods is limited to specific matrices (usually water), radiation levels (usually environmental levels), and analytes (limited number). Radiochemistry methods in DOE Methods for Evaluating Environmental and Waste Management Samples (DOE Methods) attempt to fill the applicability gap that exists between standard methods and those needed for DOE/EM activities. The Radiochemistry chapter in DOE Methods includes an ``analysis and reporting`` guidance section as well as radiochemistry methods. A basis for identifying the DOE/EM radiochemistry needs is discussed. Within this needs framework, the applicability of standard methods and targeted new methods is identified. Sources of new methods (consolidated methods from DOE laboratories and submissions from individuals) and the methods review process will be discussed. The processes involved in generating consolidated methods add editing individually submitted methods will be compared. DOE Methods is a living document and continues to expand by adding various kinds of methods. Radiochemistry methods are highlighted in this paper. DOE Methods is intended to be a resource for methods applicable to DOE/EM problems. Although it is intended to support DOE, the guidance and methods are not necessarily exclusive to DOE. The document is available at no cost through the Laboratory Management Division of DOE, Office of Technology Development.

  17. Halloysite nanotubes as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction for the determination of bismuth in water samples using high-resolution continuum source graphite-furnace atomic absorption spectrometry

    Science.gov (United States)

    Krawczyk-Coda, Magdalena

    2017-03-01

    In this research, a simple, accurate, and inexpensive preconcentration procedure was developed for the determination of bismuth in water samples, using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS). During the preconcentration step, halloysite nanotubes (HNTs) were used as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction (USA DMSPE). The influence of the pH of the sample solution, amount of HNTs, and extraction time, as well as of the main parameters of HR CS GFAAS, on absorbance was investigated. The limit of detection was 0.005 μg L- 1. The preconcentration factor achieved for bismuth was 32. The relative standard deviation (RSD) was 4%. The accuracy of this method was validated by analyses of NIST SRM 1643e (Trace elements in water) and TMDA-54.5 (A high level fortified sample for trace elements) certified reference materials. The measured bismuth contents in these certified reference materials were in satisfactory agreement with the certified values according to the t-test for a 95% confidence level. The proposed method has been successfully applied to the determination of bismuth in five different real water samples (seawater, lake water, river water, stream water and rain water).

  18. Magnetic Solid-Phase Extraction Based on β-Cyclodextrins/Acrylic Acid Modified Magnetic Gelatin for Determination of Moxidectin in Milk Samples

    Directory of Open Access Journals (Sweden)

    Yinzhu Shang

    2016-01-01

    Full Text Available β-Cyclodextrins/acrylic acid modified magnetic gelatin was prepared and then employed as the magnetic solid-phase extraction (MSPE sorbent for extraction of moxidectin in milk samples. Due to the rigidity of hydrophobic cavity of β-cyclodextrins and carboxyl groups of acrylic acid, magnetic composites are prepared to form a complex with target molecules through various kinds of chemical reactions and then showed excellent extraction performance. This method exhibits the advantages of simplicity of implementation, short extraction time (5 min, low solvent consumption, and high extraction efficiency. A rapid, simple, and effective method for the analysis of moxidectin in milk samples was established by MSPE coupled with liquid chromatography-fluorescence detection. The limit of detection was 0.1 ng·mL−1 and the recoveries from milk samples were in the range of 93.8%–112.5%. The relative standard deviation was not higher than 6.4%. In conclusion, magnetic solid-phase extraction is a simple and robust preconcentration technique that can be coupled to other analytical methods for the quantitative determination of target molecules in complex samples.

  19. High-Solids Enzymatic Saccharification Screening Method for Lignocellulosic Biomass (Poster)

    Energy Technology Data Exchange (ETDEWEB)

    Roche, C. M.; Stickel, J. J.

    2009-05-01

    The ability to screen new biomass pretreatments and advanced enzyme systems at process-relevant conditions is key to developing economically viable lignocellulosic ethanol. While much research is being invested in developing pretreatment technologies and enzyme systems that will more efficiently convert cellulosic biomass to sugars, the current standard reactor vessel, a shake flask, that is used for screening enzymatic saccharification of cellulosic biomass is inadequate at high-solids conditions. Shake flasks do not provide adequate mixing at high solids conditions. In this work, a roller bottle reactor was identified as a small-scale high-solids saccharification reaction vessel, and a method was developed for use in screening both pretreated biomass and enzyme systems at process-relevant conditions. This new method addresses mixing issues observed in high-solids saccharifications. In addition, yield calculations from sugar concentrations on a mass basis were used to account for the two-phase nature of the saccharification slurry, which eliminates discontinuities in comparing high-solids to low-solids saccharifications that occur when using concentrations on a volume basis. The roller bottle reactors out-performed the shake flasks by 5% for an initial insoluble solids loading of 15% and 140% for an initial soluble solids loading of 30%. The reactor system and method was compared at bench and floor scales and determined to be scalable for initial insoluble solids loading in the range of 15% to 30%. Pretreatment and enzyme screening results indicate that mid severity pretreated biomass is more digestible than the low and high severity biomass and GC220 is a superior enzyme to Spezyme CP.

  20. Sediment sampling and processing methods in Hungary, and possible improvements

    Science.gov (United States)

    Tamas, Eniko Anna; Koch, Daniel; Varga, Gyorgy

    2016-04-01

    The importance of the monitoring of sediment processes is unquestionable: sediment balance of regulated rivers suffered substantial alterations in the past century, affecting navigation, energy production, fish habitats and floodplain ecosystems alike; infiltration times to our drinking water wells have shortened, exposing them to an eventual pollution event and making them vulnerable; and sediment-attached contaminants accumulate in floodplains and reservoirs, threatening our healthy environment. The changes in flood characteristics and rating curves of our rivers are regularly being researched and described, involving state-of-the-art measurement methods, modeling tools and traditional statistics. Sediment processes however, are much less known. Unlike the investigation of flow processes, sediment-related research is scarce, which is partly due to the outdated methodology and poor database background in the specific field. Sediment-related data, information and analyses form an important and integral part of Civil engineering in relation to rivers all over the world. In relation to the second largest river of Europe, the Danube, it is widely known in expert community and for long discussed at different expert forums that the sediment balance of the river Danube has changed drastically over the past century. Sediment monitoring on the river Danube started as early as the end of the 19th century, with scattered measurements carried out. Regular sediment sampling was developed in the first half of the 20th century all along the river, with different station density and monitoring frequencies in different countries. After the first few decades of regular sampling, the concept of (mainly industrial) development changed along the river and data needs changed as well, furthermore the complicated and inexact methods of sampling bed load on the alluvial reach of the river were not developed further. Frequency of suspended sediment sampling is very low along the river

  1. Application of the cluster variation method to interstitial solid solutions

    NARCIS (Netherlands)

    Pekelharing, M.I.

    2008-01-01

    A thermodynamic model for interstitial alloys, based on the Cluster Variation Method (CVM), has been developed, capable of incorporating short range ordering (SRO), long range ordering (LRO), and the mutual interaction between the host and the interstitial sublattices. The obtained cluster-based

  2. Solid phase extraction method for determination of mitragynine in ...

    African Journals Online (AJOL)

    phase high performance liquid chromatography (RP-HPLC) to determine mitragynine (MG) in rat and human urine, and to investigate the influence of caffeine (CF) on urinary excretion of MG in rats. Methods: A two-dimensional wash-elute ...

  3. A Multiconstrained Ascent Guidance Method for Solid Rocket-Powered Launch Vehicles

    Directory of Open Access Journals (Sweden)

    Si-Yuan Chen

    2016-01-01

    Full Text Available This study proposes a multiconstrained ascent guidance method for a solid rocket-powered launch vehicle, which uses a hypersonic glide vehicle (HGV as payload and shuts off by fuel exhaustion. First, pseudospectral method is used to analyze the two-stage launch vehicle ascent trajectory with different rocket ignition modes. Then, constraints, such as terminal height, velocity, flight path angle, and angle of attack, are converted into the constraints within height-time profile according to the second-stage rocket flight characteristics. The closed-loop guidance method is inferred by different spline curves given the different terminal constraints. Afterwards, a thrust bias energy management strategy is proposed to waste the excess energy of the solid rocket. Finally, the proposed method is verified through nominal and dispersion simulations. The simulation results show excellent applicability and robustness of this method, which can provide a valuable reference for the ascent guidance of solid rocket-powered launch vehicles.

  4. Investigation of Di-ethylhexyl Phthalate Migration by Applying Magnetic Solid Phase Extraction Method Followed by GC-FID Determination

    Directory of Open Access Journals (Sweden)

    Mohammad Faraji

    2016-10-01

    Full Text Available Background and Objectives: The addition of plasticizers (mainly phthalates and adipates makes plastic flexible and popular for packaging, storing and preserving food, water, and so on. The most widely used plasticizer in food contact applications is di-ethylhexyl phthalate (DEHP though being suspected to have carcinogenic and estrogenic properties. The aim of this study is application of magnetic solid phase extraction as new absorbent for determination of DEHP in water samples by gas chromatography (GC. Materials and Methods: Important factors in extraction, separation and determination processes were optimized using the one-variable-at-a-time method. For optimization, all tests were performed two times. Figures of merit of the proposed method were evaluated. The amount of DEHP in some water samples was determined using the proposed method. Results: The results showed that the obtained chromatogram of extract was free of significant interference. The preservatives’ recoveries ranged from 91.6% to 102.2%. Limit of detection and limit of quantitation were 0.1 mg kg-1 and 0.3 µg L-1, respectively. Concentration of DEHP in the studied samples was in the range of N.D-2.3 µg L-1. Conclusions: The acceptable performance and reliability of the proposed method were demonstrated. Temperature and time were fount as the most effective parameters in migration of DEHP. Keywords: Di-ethylhexyl phthalate, Magnetic solid phase extraction, Migration, Gas chromatography

  5. The effect of B{sub 2}O{sub 3} flux on growth NLBCO superconductor by solid state reaction and wet-mixing methods

    Energy Technology Data Exchange (ETDEWEB)

    Suharta, W. G., E-mail: wgsuharta@gmail.com; Wendri, N.; Ratini, N.; Suarbawa, K. N. [Departement of Physics Faculty of Mathematics and Natural Science Udayana University Bali Indonesia (Indonesia)

    2016-03-11

    The synthesis of B{sub 2}O{sub 3} flux substituted NLBCO superconductor NdBa{sub 1.75}La{sub 0.25}Cu{sub 3}O{sub 7-∂} has been done using solid state reaction and wet-mixing methods in order to obtain homogeneous crystals and single phase. From DTA/TGA characteritations showed the synthesis process by wet-mixing requires a lower temperature than the solid state reaction in growing the superconductor NdBa{sub 1.75}La{sub 0.25}Cu{sub 3}O{sub 7-∂}. Therefore, in this research NdBa{sub 1.75}La{sub 0.25}Cu{sub 3}O{sub 7-∂} sample calcinated at 650°C for wet-mixing method and 820°C for solid state reaction methods. The all samples was sintered at 950°C for ten hours. Crystallinity of the sample was confirmed using X-ray techniques and generally obtained sharp peaks that indicates the sample already well crystallized. Search match analyses for diffraction data gave weight fractions of impurity phase of the solid state reaction method higher than wet-mixing method. In this research showed decreasing the price of the lattice parameter about 1% with the addition of B{sub 2}O{sub 3} flux for the both synthesis process and 2% of wet mixing process for all samples. Characterization using scanning electron microscopy (SEM) showed the distribution of crystal zise for wet-mixing method more homogeneous than solid state reaction method, with he grain size of samples is around 150–250 nm. The results of vibrating sample magnetometer (VSM) showed the paramagnetic properties for all samples.

  6. Determination of 3-alkyl-2-methoxypyrazines in lady beetle-infested wine by solid-phase microextraction headspace sampling.

    Science.gov (United States)

    Galvan, Tederson Luiz; Kells, Stephen; Hutchison, William Dale

    2008-02-13

    This study determined the concentration of 3-alkyl-2-methoxypyrazines in Frontenac and Leon Millot wines made from grapes that were naturally or artificially infested with the multicolored Asian lady beetle, Harmonia axyridis (Pallas) (Coleoptera: Coccinellidae). Headspace sampling with solid-phase microextraction (SPME) and gas chromatography (GC) was used for the quantification of 3-isopropyl-2-methoxypyrazine (IPMP), 3- sec-butyl-2-methoxypyrazine (SBMP), and 3-isobutyl-2-methoxypyrazine (IBMP). The resulting method parameters included linearity (r2 > 0.98), limit of detection (>0.25 ng/L), relative standard deviation (<20%), and recovery (75-125%). IPMP concentrations in wine were not significantly different among the levels of natural or artificial infestations of H. axyridis. SBMP was found only in wine artificially infested with H. axyridis. IBMP was found in wine artificially infested with H. axyridis and in Frontenac wine, but not in Leon Millot. The consequences of these results for future research in the contamination of wine with H. axyridis are discussed.

  7. Method for Sampling Alpha-Helical Protein Backbones

    Energy Technology Data Exchange (ETDEWEB)

    Fain, Boris; Levitt, Michael

    2000-02-22

    We present a novel technique of sampling the configurations of helical proteins. Assuming knowledge of native secondary structure, we employ assembly rules gathered from a database of existing structures to enumerate the geometrically possible 3-D arrangements of the constituent helices. We produce a library of possible folds for 25 helical protein cores. In each case the method finds significant numbers of conformations close to the native structure. In addition we assign coordinates to all atoms for 4 of the 25 proteins. In the context of database driven exhaustive enumeration our method performs extremely well, yielding significant percentages of structures (0.02%--82%) within 6A of the native structure. The method's speed and efficiency make it a valuable contribution towards the goal of predicting protein structure.

  8. Comparison between powder and slices diffraction methods in teeth samples

    Energy Technology Data Exchange (ETDEWEB)

    Colaco, Marcos V.; Barroso, Regina C. [Universidade do Estado do Rio de Janeiro (IF/UERJ), RJ (Brazil). Inst. de Fisica. Dept. de Fisica Aplicada; Porto, Isabel M. [Universidade Estadual de Campinas (FOP/UNICAMP), Piracicaba, SP (Brazil). Fac. de Odontologia. Dept. de Morfologia; Gerlach, Raquel F. [Universidade de Sao Paulo (FORP/USP), Rieirao Preto, SP (Brazil). Fac. de Odontologia. Dept. de Morfologia, Estomatologia e Fisiologia; Costa, Fanny N. [Coordenacao dos Programas de Pos-Graduacao de Engenharia (LIN/COPPE/UFRJ), RJ (Brazil). Lab. de Instrumentacao Nuclear

    2011-07-01

    Propose different methods to obtain crystallographic information about biological materials are important since powder method is a nondestructive method. Slices are an approximation of what would be an in vivo analysis. Effects of samples preparation cause differences in scattering profiles compared with powder method. The main inorganic component of bones and teeth is a calcium phosphate mineral whose structure closely resembles hydroxyapatite (HAp). The hexagonal symmetry, however, seems to work well with the powder diffraction data, and the crystal structure of HAp is usually described in space group P63/m. Were analyzed ten third molar teeth. Five teeth were separated in enamel, detin and circumpulpal detin powder and five in slices. All the scattering profile measurements were carried out at the X-ray diffraction beamline (XRD1) at the National Synchrotron Light Laboratory - LNLS, Campinas, Brazil. The LNLS synchrotron light source is composed of a 1.37 GeV electron storage ring, delivering approximately 4x10{sup -1}0 photons/s at 8 keV. A double-crystal Si(111) pre-monochromator, upstream of the beamline, was used to select a small energy bandwidth at 11 keV . Scattering signatures were obtained at intervals of 0.04 deg for angles from 24 deg to 52 deg. The human enamel experimental crystallite size obtained in this work were 30(3)nm (112 reflection) and 30(3)nm (300 reflection). These values were obtained from measurements of powdered enamel. When comparing the slice obtained 58(8)nm (112 reflection) and 37(7)nm (300 reflection) enamel diffraction patterns with those generated by the powder specimens, a few differences emerge. This work shows differences between powder and slices methods, separating characteristics of sample of the method's influence. (author)

  9. Quantitative lead determination in coating paint on children's outwear by LA-ICP-MS: a practical calibration strategy for solid samples.

    Science.gov (United States)

    Mercan, Selda; Ellez, Sevinç Zeynep; Türkmen, Zeynep; Yayla, Murat; Cengiz, Salih

    2015-01-01

    Lead is a hazardous compound that affects the central nervous system in people, particularly children, and may cause some reversible and irreversible diseases. Legal regulations try to prevent the exposure from products especially produced for children such as coating paints, jewelry, toys, bed linen, textile, etc. The aim of this study was to determine the lead levels of coating paints on children׳s outwear selling in district bazaar by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and to specify the percent of non-complying samples. Here we described the solid matrix calibration method and confirmed the results with the microwave-assisted acid digestion method. Both comparative methods were validated by analysis of the certified reference materials (NIST SRM-612 glass matrix, NIST SRM-2582 powdered paint and ERM-EC681k) and bias% for accuracy and RSD% for precision were calculated lower than 6.8% and 7.3%, respectively. The recovery ranges of laser ablation and microwave-assisted acid digestion method for Pb were found to be between 88.2-98.1% and 95.3-101.3%, respectively. The limits of detection values were determined as 0.162 mg kg(-1) for direct sampling in the ablation chamber and 0.002 ng mL(-1) for aqueous solutions. Correlation result of 16 samples (r=0.99) examined in both methods was satisfactory. In coating paint samples, 14.65% of 198 (n=29) did not comply with the 90 mg kg(-1) lead limit according to regulation. Validated quantitative laser ablation method may be preferred to quickly and reliably determine the Pb levels in other solid samples as well as coating paints. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Sampling and measurement methods for diesel exhaust aerosol

    Energy Technology Data Exchange (ETDEWEB)

    Ristimaeki, J.

    2006-07-01

    Awareness of adverse health effects of urban aerosols has increased general interest in aerosol sources. As diesel engines are one significant urban anthropogenic particle source, diesel aerosols have been under intense research during the last decades. This thesis discusses the measurement issues related to the diesel exhaust particles, focusing on the effective density measurement with Elpi-Sumps and Tda-Elpi methods and presents some additional performance issues not discussed in the papers. As the emergence of volatile nanoparticles in the diesel exhaust is sensitive to prevailing circumstances there is a need to properly control the dilution parameters in laboratory measurements in order to obtain repeatable and reproducible results. In addition to the dilution parameters, the effect of ambient temperature on the light duty vehicle exhaust particulate emission was studied. It was found that turbo charged diesel engines were relatively insensitive to changes in ambient temperature whereas particle emissions from naturally aspirated gasoline vehicles were significantly increased at low temperatures. The measurement of effective density and mass of aerosol particles with Dma and impactor was studied and applied to characterisation of diesel exhaust particles. The Tda-Elpi method was used for determination of the volatile mass of diesel exhaust particles as a function of particle size. Based on the measurement results, condensation was suggested to be the main phenomena driving volatile mass transfer to the exhaust particles. Identification of the process and the separation of volatile and solid mass may become important as some health effect studies suggest the volatile fraction to be a key component causing the biological effects of diesel exhaust particles. (orig.)

  11. Hand held sample tube manipulator, system and method

    Science.gov (United States)

    Kenny, Donald V [Liberty Township, OH; Smith, Deborah L [Liberty Township, OH; Severance, Richard A [late of Columbus, OH

    2001-01-01

    A manipulator apparatus, system and method for measuring analytes present in sample tubes. The manipulator apparatus includes a housing having a central bore with an inlet end and outlet end; a plunger mechanism with at least a portion thereof slideably disposed for reciprocal movement within the central bore, the plunger mechanism having a tubular gas channel with an inlet end and an outlet end, the gas channel inlet end disposed in the same direction as said inlet end of the central bore, wherein the inlet end of said plunger mechanism is adapted for movement so as to expel a sample tube inserted in the bore at the outlet end of the housing, the inlet end of the plunger mechanism is adapted for connection to gas supply; a first seal is disposed in the housing for sealing between the central bore and the plunger mechanism; a second seal is disposed at the outlet end of the housing for sealing between the central bore and a sample tube; a holder mounted on the housing for holding the sample tube; and a biasing mechanism for returning the plunger mechanism to a starting position.

  12. Applicability of solid-phase microextraction combined with gas chromatography atomic emission detection (GC-MIP AED) for the determination of butyltin compounds in sediment samples

    Energy Technology Data Exchange (ETDEWEB)

    Carpinteiro, J.; Rodriguez, I.; Cela, R. [Universidad de Santiago de Compostela, Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Santiago de Compostela 15782 (Spain)

    2004-11-01

    The performance of solid-phase microextraction (SPME) applied to the determination of butyltin compounds in sediment samples is systematically evaluated. Matrix effects and influence of blank signals on the detection limits of the method are studied in detail. The interval of linear response is also evaluated in order to assess the applicability of the method to sediments polluted with butyltin compounds over a large range of concentrations. Advantages and drawbacks of including an SPME step, instead of the classic liquid-liquid extraction of the derivatized analytes, in the determination of butyltin compounds in sediment samples are considered in terms of achieved detection limits and experimental effort. Analytes were extracted from the samples by sonication using glacial acetic acid. An aliquot of the centrifuged extract was placed on a vial where compounds were ethylated and concentrated on a PDMS fiber using the headspace mode. Determinations were carried out using GC-MIP AED. (orig.)

  13. Sample Size for Assessing Agreement between Two Methods of Measurement by Bland-Altman Method.

    Science.gov (United States)

    Lu, Meng-Jie; Zhong, Wei-Hua; Liu, Yu-Xiu; Miao, Hua-Zhang; Li, Yong-Chang; Ji, Mu-Huo

    2016-11-01

    The Bland-Altman method has been widely used for assessing agreement between two methods of measurement. However, it remains unsolved about sample size estimation. We propose a new method of sample size estimation for Bland-Altman agreement assessment. According to the Bland-Altman method, the conclusion on agreement is made based on the width of the confidence interval for LOAs (limits of agreement) in comparison to predefined clinical agreement limit. Under the theory of statistical inference, the formulae of sample size estimation are derived, which depended on the pre-determined level of α, β, the mean and the standard deviation of differences between two measurements, and the predefined limits. With this new method, the sample sizes are calculated under different parameter settings which occur frequently in method comparison studies, and Monte-Carlo simulation is used to obtain the corresponding powers. The results of Monte-Carlo simulation showed that the achieved powers could coincide with the pre-determined level of powers, thus validating the correctness of the method. The method of sample size estimation can be applied in the Bland-Altman method to assess agreement between two methods of measurement.

  14. Development of an Analytical Method Based on Temperature Controlled Solid-Liquid Extraction Using an Ionic Liquid as Solid Solvent

    Directory of Open Access Journals (Sweden)

    Zhongwei Pan

    2015-12-01

    Full Text Available At the present paper, an analytical method based on temperature controlled solid-liquid extraction (TC-SLE utilizing a synthesized ionic liquid, (N-butylpyridinium hexafluorophosphate, [BPy]PF6, as solid solvent and phenanthroline (PT as an extractant was developed to determine micro levels of Fe2+ in tea by PT spectrophotometry. TC-SLE was carried out in two continuous steps: Fe2+ can be completely extracted by PT-[BPy]PF6 or back-extracted at 80 °C and the two phases were separated automatically by cooling to room temperature. Fe2+, after back-extraction, needs 2 mol/L HNO3 as stripping agent and the whole process was determined by PT spectrophotometry at room temperature. The extracted species was neutral Fe(PTmCl2 (m = 1 according to slope analysis in the Fe2+-[BPy]PF6-PT TC-SLE system. The calibration curve was Y = 0.20856X − 0.000775 (correlation coefficient = 0.99991. The linear calibration range was 0.10–4.50 μg/mL and the limit of detection for Fe2+ is 7.0 × 10−2 μg/mL. In this method, the contents of Fe2+ in Tieguanyin tea were determined with RSDs (n = 5 3.05% and recoveries in range of 90.6%–108.6%.

  15. A direct sampling method for inverse electromagnetic medium scattering

    KAUST Repository

    Ito, Kazufumi

    2013-09-01

    In this paper, we study the inverse electromagnetic medium scattering problem of estimating the support and shape of medium scatterers from scattered electric/magnetic near-field data. We shall develop a novel direct sampling method based on an analysis of electromagnetic scattering and the behavior of the fundamental solution. It is applicable to a few incident fields and needs only to compute inner products of the measured scattered field with the fundamental solutions located at sampling points. Hence, it is strictly direct, computationally very efficient and highly robust to the presence of data noise. Two- and three-dimensional numerical experiments indicate that it can provide reliable support estimates for multiple scatterers in the case of both exact and highly noisy data. © 2013 IOP Publishing Ltd.

  16. Matrix solid-phase dispersion with chitosan-zinc oxide nanoparticles combined with flotation-assisted dispersive liquid-liquid microextraction for the determination of 13 n-alkanes in soil samples.

    Science.gov (United States)

    Khajeh, Mostafa; Yan, Hongyuan; Arefnejad, Esmat; Bohlooli, Mousa

    2014-11-01

    In this study, chitosan-zinc oxide nanoparticles were used as a sorbent of miniaturized matrix solid-phase dispersion combined with flotation-assisted dispersive liquid-liquid microextraction for the simultaneous determination of 13 n-alkanes such as C8 H18 and C20 H42 in soil samples. The solid samples were directly blended with the chitosan nanoparticles in the solid-phase dispersion method. The eluent of solid-phase dispersion was applied as the dispersive solvent for the following flotation-assisted dispersive liquid-liquid microextraction for further purification and enrichment of the target compounds prior to gas chromatography with flame ionization detection. Under the optimum conditions, good linearity with correlation coefficients in the range 0.9991 alkanes in complicated soil samples with acceptable recoveries. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Solid-state potentiometric biosensors for pH quantification in biological samples

    NARCIS (Netherlands)

    Ivan, M.G.; Wiegersma, S.; Sweelssen, J.; Saalmink, M.; Boersma, A.

    2011-01-01

    This paper reports on manufacturing and characterization of an all-solid-state potentiometric sensor aimed at monitoring pH in dialysate or blood plasma for patients who undergo dialysis. The sensing polymer-based membrane, coated on top of the Au working electrodes, contains a polymer matrix -

  18. Method optimization for fecal sample collection and fecal DNA extraction.

    Science.gov (United States)

    Mathay, Conny; Hamot, Gael; Henry, Estelle; Georges, Laura; Bellora, Camille; Lebrun, Laura; de Witt, Brian; Ammerlaan, Wim; Buschart, Anna; Wilmes, Paul; Betsou, Fay

    2015-04-01

    This is the third in a series of publications presenting formal method validation for biospecimen processing in the context of accreditation in laboratories and biobanks. We report here optimization of a stool processing protocol validated for fitness-for-purpose in terms of downstream DNA-based analyses. Stool collection was initially optimized in terms of sample input quantity and supernatant volume using canine stool. Three DNA extraction methods (PerkinElmer MSM I®, Norgen Biotek All-In-One®, MoBio PowerMag®) and six collection container types were evaluated with human stool in terms of DNA quantity and quality, DNA yield, and its reproducibility by spectrophotometry, spectrofluorometry, and quantitative PCR, DNA purity, SPUD assay, and 16S rRNA gene sequence-based taxonomic signatures. The optimal MSM I protocol involves a 0.2 g stool sample and 1000 μL supernatant. The MSM I extraction was superior in terms of DNA quantity and quality when compared to the other two methods tested. Optimal results were obtained with plain Sarstedt tubes (without stabilizer, requiring immediate freezing and storage at -20°C or -80°C) and Genotek tubes (with stabilizer and RT storage) in terms of DNA yields (total, human, bacterial, and double-stranded) according to spectrophotometry and spectrofluorometry, with low yield variability and good DNA purity. No inhibitors were identified at 25 ng/μL. The protocol was reproducible in terms of DNA yield among different stool aliquots. We validated a stool collection method suitable for downstream DNA metagenomic analysis. DNA extraction with the MSM I method using Genotek tubes was considered optimal, with simple logistics in terms of collection and shipment and offers the possibility of automation. Laboratories and biobanks should ensure protocol conditions are systematically recorded in the scope of accreditation.

  19. Empirical comparison of neutron activation sample analysis methods

    Science.gov (United States)

    Gillenwalters, Elizabeth

    The U.S. Geological Survey (USGS) operates a research reactor used mainly for neutron activation of samples, which are then shipped to industrial customers. Accurate nuclide identification and activity determination are crucial to remain in compliance with Code of Federal Regulations guidelines. This facility utilized a Canberra high purity germanium detector (HPGe) coupled with Canberra Genie(TM) 2000 (G2K) software for gamma spectroscopy. This study analyzed the current method of nuclide identification and activity determination of neutron activated materials utilized by the USGS reactor staff and made recommendations to improve the method. Additionally, analysis of attenuators, effect of detector dead time on nuclide identification, and validity of activity determination assumptions were investigated. The current method of activity determination utilized the G2K software to obtain ratio of activity per nuclide identified. This determination was performed without the use of geometrically appropriate efficiency calibration curves. The ratio of activity per nuclide was used in conjunction with an overall exposure rate in mR/h obtained via a Fluke Biomedical hand-held ion chamber. The overall exposure rate was divided into individual nuclide amounts based on the G2K nuclide ratios. A gamma energy of 1 MeV and a gamma yield of 100% was assumed for all samples. Utilizing the gamma assumption and nuclide ratios, a calculation was performed to determine total sample activity in muCi (microCuries). An alternative method was proposed, which would eliminate the use of exposure rate and rely solely on the G2K software capabilities. The G2K software was energy and efficiency calibrated with efficiency curves developed for multiple geometries. The USGS reactor staff were trained to load appropriate calibration data into the G2K software prior to sample analysis. Comparison of the current method and proposed method demonstrated that the activity value calculated with the 1 Me

  20. Tea bag filter paper as a novel protective membrane for micro-solid phase extraction of butachlor in aqueous samples.

    Science.gov (United States)

    Pelden, Tshering; Thammaknet, Chongdee; Thavarungkul, Panote; Kanatharana, Proespichaya

    2014-01-01

    An innovative, cost-effective, simple, and environmental friendly tea bag filter paper protected micro-solid phase extraction (μ-SPE) technique was developed for the first time with the aim to miniaturize and minimize the use of organic solvents for the extraction and determination of butachlor in aqueous samples. The μ-SPE device was produced by packing 3.0 mg of an easily synthesized new sorbent, hydroxyl-functionalized polypyrrole (OH-PPY), inside a small tea bag filter paper sachet (1.0 cm × 0.5 cm) that served as a protective envelope. Both the extraction and desorption procedures were facilitated by sonication. Due to the high porosity and the fast water absorption of the tea bag filter paper, the analyte could easily diffuse through and enhance the interaction with the sorbent. Under the optimized conditions for the GC-ECD and the μ-SPE, the limit of detection (S/N ≥ 3) was 2.0 μg L(-1) while the limit of quantitation (S/N ≥ 10) was 10.0 μg L(-1). The recoveries of the butachlor spiked at 0.050, 0.10, and 0.50 μg mL(-1) ranged from 77.9 ± 3.0 to 112.5 ± 2.9%. The proposed method was successfully applied for the determination of butachlor in water samples from paddy cultivation sites. The levels found were from non-detectable to 24.71 ± 0.37 μg L(-1).

  1. [Near-infrared spectra combining with CARS and SPA algorithms to screen the variables and samples for quantitatively determining the soluble solids content in strawberry].

    Science.gov (United States)

    Li, Jiang-bo; Guo, Zhi-ming; Huang, Wen-qian; Zhang, Bao-hua; Zhao, Chun-jiang

    2015-02-01

    In using spectroscopy to quantitatively or qualitatively analyze the quality of fruit, how to obtain a simple and effective correction model is very critical for the application and maintenance of the developed model. Strawberry as the research object, this research mainly focused on selecting the key variables and characteristic samples for quantitatively determining the soluble solids content. Competitive adaptive reweighted sampling (CARS) algorithm was firstly proposed to select the spectra variables. Then, Samples of correction set were selected by successive projections algorithm (SPA), and 98 characteristic samples were obtained. Next, based on the selected variables and characteristic samples, the second variable selection was performed by using SPA method. 25 key variables were obtained. In order to verify the performance of the proposed CARS algorithm, variable selection algorithms including Monte Carlo-uninformative variable elimination (MC-UVE) and SPA were used as the comparison algorithms. Results showed that CARS algorithm could eliminate uninformative variables and remove the collinearity information at the same time. Similarly, in order to assess the performance of the proposed SPA algorithm for selecting the characteristic samples, SPA algorithm was compared with classical Kennard-Stone algorithm Results showed that SPA algorithm could be used for selection of the characteristic samples in the calibration set. Finally, PLS and MLR model for quantitatively predicting the SSC (soluble solids content) in the strawberry were proposed based on the variables/samples subset (25/98), respectively. Results show that models built by using the 0.59% and 65.33% information of original variables and samples could obtain better performance than using the ones obtained by using all information of the original variables and samples. MLR model was the best with R(pre)2 = 0.9097, RMSEP=0.3484 and RPD = 3.3278.

  2. Generalized Jones matrix method for homogeneous biaxial samples.

    Science.gov (United States)

    Ortega-Quijano, Noé; Fade, Julien; Alouini, Mehdi

    2015-08-10

    The generalized Jones matrix (GJM) is a recently introduced tool to describe linear transformations of three-dimensional light fields. Based on this framework, a specific method for obtaining the GJM of uniaxial anisotropic media was recently presented. However, the GJM of biaxial media had not been tackled so far, as the previous method made use of a simplified rotation matrix that lacks a degree of freedom in the three-dimensional rotation, thus being not suitable for calculating the GJM of biaxial media. In this work we propose a general method to derive the GJM of arbitrarily-oriented homogeneous biaxial media. It is based on the differential generalized Jones matrix (dGJM), which is the three-dimensional counterpart of the conventional differential Jones matrix. We show that the dGJM provides a simple and elegant way to describe uniaxial and biaxial media, with the capacity to model multiple simultaneous optical effects. The practical usefulness of this method is illustrated by the GJM modeling of the polarimetric properties of a negative uniaxial KDP crystal and a biaxial KTP crystal for any three-dimensional sample orientation. The results show that this method constitutes an advantageous and straightforward way to model biaxial media, which show a growing relevance for many interesting applications.

  3. Evaluation of the 5 and 8 pH point titration methods for monitoring anaerobic digesters treating solid waste.

    Science.gov (United States)

    Vannecke, T P W; Lampens, D R A; Ekama, G A; Volcke, E I P

    2015-01-01

    Simple titration methods certainly deserve consideration for on-site routine monitoring of volatile fatty acid (VFA) concentration and alkalinity during anaerobic digestion (AD), because of their simplicity, speed and cost-effectiveness. In this study, the 5 and 8 pH point titration methods for measuring the VFA concentration and carbonate system alkalinity (H2CO3*-alkalinity) were assessed and compared. For this purpose, synthetic solutions with known H2CO3*-alkalinity and VFA concentration as well as samples from anaerobic digesters treating three different kind of solid wastes were analysed. The results of these two related titration methods were verified with photometric and high-pressure liquid chromatography measurements. It was shown that photometric measurements lead to overestimations of the VFA concentration in the case of coloured samples. In contrast, the 5 pH point titration method provides an accurate estimation of the VFA concentration, clearly corresponding with the true value. Concerning the H2CO3*-alkalinity, the most accurate and precise estimations, showing very similar results for repeated measurements, were obtained using the 8 pH point titration. Overall, it was concluded that the 5 pH point titration method is the preferred method for the practical monitoring of AD of solid wastes due to its robustness, cost efficiency and user-friendliness.

  4. Liquid Metering Centrifuge Sticks (LMCS): A Centrifugal Approach to Metering Known Sample Volumes for Colorimetric Solid Phase Extraction (C-SPE)

    Science.gov (United States)

    Gazda, Daniel B.; Schultz, John R.; Clarke, Mark S.

    2007-01-01

    Phase separation is one of the most significant obstacles encountered during the development of analytical methods for water quality monitoring in spacecraft environments. Removing air bubbles from water samples prior to analysis is a routine task on earth; however, in the absence of gravity, this routine task becomes extremely difficult. This paper details the development and initial ground testing of liquid metering centrifuge sticks (LMCS), devices designed to collect and meter a known volume of bubble-free water in microgravity. The LMCS uses centrifugal force to eliminate entrapped air and reproducibly meter liquid sample volumes for analysis with Colorimetric Solid Phase Extraction (C-SPE). C-SPE is a sorption-spectrophotometric platform that is being developed as a potential spacecraft water quality monitoring system. C-SPE utilizes solid phase extraction membranes impregnated with analyte-specific colorimetric reagents to concentrate and complex target analytes in spacecraft water samples. The mass of analyte extracted from the water sample is determined using diffuse reflectance (DR) data collected from the membrane surface and an analyte-specific calibration curve. The analyte concentration can then be calculated from the mass of extracted analyte and the volume of the sample analyzed. Previous flight experiments conducted in microgravity conditions aboard the NASA KC-135 aircraft demonstrated that the inability to collect and meter a known volume of water using a syringe was a limiting factor in the accuracy of C-SPE measurements. Herein, results obtained from ground based C-SPE experiments using ionic silver as a test analyte and either the LMCS or syringes for sample metering are compared to evaluate the performance of the LMCS. These results indicate very good agreement between the two sample metering methods and clearly illustrate the potential of utilizing centrifugal forces to achieve phase separation and metering of water samples in microgravity.

  5. Facile preparation of a polydopamine-based monolith for multiple monolithic fiber solid-phase microextraction of triazine herbicides in environmental water samples.

    Science.gov (United States)

    Zhang, Zirui; Mei, Meng; Huang, Yanmei; Huang, Xiaojia; Huang, Hanyue; Ding, Yuxin

    2017-02-01

    A new multiple monolithic fiber solid-phase microextraction using a polydopamine-based monolith as the extraction medium is proposed. The monolith was synthesized by facile in situ copolymerization of N-methacryldopamine and dual cross-linkers (divinylbenzene/ethylenedimethacrylate) in the presence of N,N-dimethylformamide. The effect of the contents of N-methacryldopamine and porogen in the polymerization mixture on the extraction performance was investigated thoroughly. A series of characterization studies was performed to validate the structure and properties of the monolith. The prepared multiple monolithic fibers were used for the extraction of triazine herbicides in environmental water samples. After the optimization of the extraction parameters, a convenient, sensitive, cost-effective, and environmentally friendly method for the determination of trace triazine herbicides in water samples was developed by coupling multiple monolithic fibers solid-phase microextraction with high-performance liquid chromatography and diode array detection. The results indicated that the limits of detection and quantification for the target compounds were 0.031-0.14 and 0.10-0.45 μg/L, respectively. Good precision and reproducibility were obtained with the relative standard deviations below 10%. The developed method was applied to the analysis of the triazine herbicides in different water samples (lake, river, and farmland waters). The recoveries of the method were in the range between 79.6 and 117%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Method for Synthesizing Metal Nanowires in Anodic Alumina Membranes Using Solid State Reduction

    Science.gov (United States)

    Martinez-Inesta, Maria M (Inventor); Feliciano, Jennie (Inventor); Quinones-Fontalvo, Leonel (Inventor)

    2016-01-01

    The invention proposes a novel method for the fabrication of regular arrays of MNWs using solid-state reduction (SSR). Using this method copper (Cu), silver (Ag), and palladium (Pd) nanowire (NWs) arrays were synthesized using anodic alumina membranes (AAMs) as templates. Depending on the metal loading used the NWs reached different diameters.

  7. An alternative preparation method for ion exchanged catalysts: Solid state redox reaction

    DEFF Research Database (Denmark)

    Schneider, E.; Hagen, A.; Grunwaldt, J.-D.

    2004-01-01

    infrared Fourier transform spectroscopy (DRIFTS). The evolution of hydrogen was detected at temperatures above 620 K. The source of hydrogen was the solid state redox reaction of the metal with protons of the support. The samples exhibit catalytic activity in ethane aromatization indicating that zinc...

  8. Methods of Human Body Odor Sampling: The Effect of Freezing

    National Research Council Canada - National Science Library

    Lenochova, Pavlina; Roberts, S. Craig; Havlicek, Jan

    Body odor sampling is an essential tool in human chemical ecology research. However, methodologies of individual studies vary widely in terms of sampling material, length of sampling, and sample processing...

  9. Comparison of Spot and Time Weighted Averaging (TWA Sampling with SPME-GC/MS Methods for Trihalomethane (THM Analysis

    Directory of Open Access Journals (Sweden)

    Don-Roger Parkinson

    2016-02-01

    Full Text Available Water samples were collected and analyzed for conductivity, pH, temperature and trihalomethanes (THMs during the fall of 2014 at two monitored municipal drinking water source ponds. Both spot (or grab and time weighted average (TWA sampling methods were assessed over the same two day sampling time period. For spot sampling, replicate samples were taken at each site and analyzed within 12 h of sampling by both Headspace (HS- and direct (DI- solid phase microextraction (SPME sampling/extraction methods followed by Gas Chromatography/Mass Spectrometry (GC/MS. For TWA, a two day passive on-site TWA sampling was carried out at the same sampling points in the ponds. All SPME sampling methods undertaken used a 65-µm PDMS/DVB SPME fiber, which was found optimal for THM sampling. Sampling conditions were optimized in the laboratory using calibration standards of chloroform, bromoform, bromodichloromethane, dibromochloromethane, 1,2-dibromoethane and 1,2-dichloroethane, prepared in aqueous solutions from analytical grade samples. Calibration curves for all methods with R2 values ranging from 0.985–0.998 (N = 5 over the quantitation linear range of 3–800 ppb were achieved. The different sampling methods were compared for quantification of the water samples, and results showed that DI- and TWA- sampling methods gave better data and analytical metrics. Addition of 10% wt./vol. of (NH42SO4 salt to the sampling vial was found to aid extraction of THMs by increasing GC peaks areas by about 10%, which resulted in lower detection limits for all techniques studied. However, for on-site TWA analysis of THMs in natural waters, the calibration standard(s ionic strength conditions, must be carefully matched to natural water conditions to properly quantitate THM concentrations. The data obtained from the TWA method may better reflect actual natural water conditions.

  10. A new generalized Kohn-Sham method for fundamental band-gaps in solids.

    Science.gov (United States)

    Eisenberg, Helen R; Baer, Roi

    2009-06-14

    We developed a method for calculating the ground-state properties and fundamental band-gaps of solids, using a generalized Kohn-Sham approach combining a local density approximation (LDA) functional with a long-range explicit exchange orbital functional. We found that when the range parameter is selected according to the formula gamma=A/(epsiloninfinity-epsilon) where epsiloninfinity is the optical dielectric constant of the solid and epsilon=0.84 and A=0.216 a0(-1), predictions of the fundamental band-gap close to the experimental values are obtained for a variety of solids of different types. For most solids the range parameter gamma is small (i.e. explicit exchange is needed only at long distances) so the predicted values for lattice constants and bulk moduli are similar to those based on conventional LDA calculations. Preliminary calculations on silicon give a general band structure in good agreement with experiment.

  11. Dispersive micro-solid phase extraction based on self-assembling, ionic liquid-coated magnetic particles for the determination of clofentezine and chlorfenapyr in environmental water samples.

    Science.gov (United States)

    Peng, Bing; Zhang, Jiaheng; Lu, Runhua; Zhang, Sanbing; Zhou, Wenfeng; Gao, Haixiang

    2013-11-21

    Two ionic liquid-coated-Fe3O4 magnetic particles (IL-Fe3O4 MPs) were developed for use in two types of dispersive micro-solid phase extraction (D-μ-SPE) for the high-performance liquid chromatographic analysis of clofentezine and chlorfenapyr in environmental water samples. Self-assembling IL-Fe3O4 MPs were used in D-μ-SPE as adsorbents. Two D-μ-SPE extraction methods, namely, direct dispersive micro-solid phase extraction (d-D-μ-SPE) and in situ solvent formation-based dispersive micro-solid phase extraction (ISF-D-μ-SPE), were proposed, using [C8MIM][PF6] to extract analytes through two pathways. Lower IL doses were required in the extraction process compared with those in other IL-based methods. Fe3O4 MPs can also be recycled and reused after extraction and are thus environmentally friendly. These newly developed methods were demonstrated to be feasible for use in the quantitation of clofentezine and chlorfenapyr at trace levels, with lower limit of detection values ranging from 0.4 to 0.5 ng mL(-1) for d-D-μ-SPE and 0.4 ng mL(-1) for ISF-D-μ-SPE. Finally, relative standard deviations of less than 6.0% were obtained.

  12. Verification of spectrophotometric method for nitrate analysis in water samples

    Science.gov (United States)

    Kurniawati, Puji; Gusrianti, Reny; Dwisiwi, Bledug Bernanti; Purbaningtias, Tri Esti; Wiyantoko, Bayu

    2017-12-01

    The aim of this research was to verify the spectrophotometric method to analyze nitrate in water samples using APHA 2012 Section 4500 NO3-B method. The verification parameters used were: linearity, method detection limit, level of quantitation, level of linearity, accuracy and precision. Linearity was obtained by using 0 to 50 mg/L nitrate standard solution and the correlation coefficient of standard calibration linear regression equation was 0.9981. The method detection limit (MDL) was defined as 0,1294 mg/L and limit of quantitation (LOQ) was 0,4117 mg/L. The result of a level of linearity (LOL) was 50 mg/L and nitrate concentration 10 to 50 mg/L was linear with a level of confidence was 99%. The accuracy was determined through recovery value was 109.1907%. The precision value was observed using % relative standard deviation (%RSD) from repeatability and its result was 1.0886%. The tested performance criteria showed that the methodology was verified under the laboratory conditions.

  13. Methods to maximise recovery of environmental DNA from water samples.

    Directory of Open Access Journals (Sweden)

    Rheyda Hinlo

    Full Text Available The environmental DNA (eDNA method is a detection technique that is rapidly gaining credibility as a sensitive tool useful in the surveillance and monitoring of invasive and threatened species. Because eDNA analysis often deals with small quantities of short and degraded DNA fragments, methods that maximize eDNA recovery are required to increase detectability. In this study, we performed experiments at different stages of the eDNA analysis to show which combinations of methods give the best recovery rate for eDNA. Using Oriental weatherloach (Misgurnus anguillicaudatus as a study species, we show that various combinations of DNA capture, preservation and extraction methods can significantly affect DNA yield. Filtration using cellulose nitrate filter paper preserved in ethanol or stored in a -20°C freezer and extracted with the Qiagen DNeasy kit outperformed other combinations in terms of cost and efficiency of DNA recovery. Our results support the recommendation to filter water samples within 24hours but if this is not possible, our results suggest that refrigeration may be a better option than freezing for short-term storage (i.e., 3-5 days. This information is useful in designing eDNA detection of low-density invasive or threatened species, where small variations in DNA recovery can signify the difference between detection success or failure.

  14. Methods to maximise recovery of environmental DNA from water samples.

    Science.gov (United States)

    Hinlo, Rheyda; Gleeson, Dianne; Lintermans, Mark; Furlan, Elise

    2017-01-01

    The environmental DNA (eDNA) method is a detection technique that is rapidly gaining credibility as a sensitive tool useful in the surveillance and monitoring of invasive and threatened species. Because eDNA analysis often deals with small quantities of short and degraded DNA fragments, methods that maximize eDNA recovery are required to increase detectability. In this study, we performed experiments at different stages of the eDNA analysis to show which combinations of methods give the best recovery rate for eDNA. Using Oriental weatherloach (Misgurnus anguillicaudatus) as a study species, we show that various combinations of DNA capture, preservation and extraction methods can significantly affect DNA yield. Filtration using cellulose nitrate filter paper preserved in ethanol or stored in a -20°C freezer and extracted with the Qiagen DNeasy kit outperformed other combinations in terms of cost and efficiency of DNA recovery. Our results support the recommendation to filter water samples within 24hours but if this is not possible, our results suggest that refrigeration may be a better option than freezing for short-term storage (i.e., 3-5 days). This information is useful in designing eDNA detection of low-density invasive or threatened species, where small variations in DNA recovery can signify the difference between detection success or failure.

  15. The curvHDR method for gating flow cytometry samples

    Directory of Open Access Journals (Sweden)

    Wand Matthew P

    2010-01-01

    Full Text Available Abstract Background High-throughput flow cytometry experiments produce hundreds of large multivariate samples of cellular characteristics. These samples require specialized processing to obtain clinically meaningful measurements. A major component of this processing is a form of cell subsetting known as gating. Manual gating is time-consuming and subjective. Good automatic and semi-automatic gating algorithms are very beneficial to high-throughput flow cytometry. Results We develop a statistical procedure, named curvHDR, for automatic and semi-automatic gating. The method combines the notions of significant high negative curvature regions and highest density regions and has the ability to adapt well to human-perceived gates. The underlying principles apply to dimension of arbitrary size, although we focus on dimensions up to three. Accompanying software, compatible with contemporary flow cytometry infor-matics, is developed. Conclusion The method is seen to adapt well to nuances in the data and, to a reasonable extent, match human perception of useful gates. It offers big savings in human labour when processing high-throughput flow cytometry data whilst retaining a good degree of efficacy.

  16. Field evaluation of broiler gait score using different sampling methods

    Directory of Open Access Journals (Sweden)

    AFS Cordeiro

    2009-09-01

    Full Text Available Brazil is today the world's largest broiler meat exporter; however, in order to keep this position, it must comply with welfare regulations while maintaining low production costs. Locomotion problems restrain bird movements, limiting their access to drinking and feeding equipment, and therefore their survival and productivity. The objective of this study was to evaluate locomotion deficiency in broiler chickens reared under stressful temperature conditions using three different sampling methods of birds from three different ages. The experiment consisted in determining the gait score of 28, 35, 42 and 49-day-old broilers using three different known gait scoring methods: M1, birds were randomly selected, enclosed in a circle, and then stimulated to walk out of the circle; M2, ten birds were randomly selected and gait scored; and M3, birds were randomly selected, enclosed in a circle, and then observed while walking away from the circle without stimulus to walking. Environmental temperature, relative humidity, and light intensity inside the poultry houses were recorded. No evidence of interaction between scoring method and age was found however, both method and age influenced gait score. Gait score was found to be lower at 28 days of age. The evaluation using the ten randomly selected birds within the house was the method that presented the less reliable results. Gait score results when birds were stimulated to walk were lower than when they were not simulated, independently of age. The gait scores obtained with the three tested methods and ages were higher than those considered acceptable. The highest frequency of normal gait score (0 represented 50% of the flock. These results may be related to heat stress during rearing. Average gait score incresead with average ambient temperature, relative humidity, and light intensity. The evaluation of gait score to detect locomotion problems of broilers under rearing conditions seems subjective and

  17. Assessing the failure of continuum formula for solid-solid drag force using discrete element method in large size ratios

    Science.gov (United States)

    Jalali, Payman; Hyppänen, Timo

    2017-06-01

    In loose or moderately-dense particle mixtures, the contact forces between particles due to successive collisions create average volumetric solid-solid drag force between different granular phases (of different particle sizes). The derivation of the mathematical formula for this drag force is based on the homogeneity of mixture within the calculational control volume. This assumption especially fails when the size ratio of particles grows to a large value of 10 or greater. The size-driven inhomogeneity is responsible to the deviation of intergranular force from the continuum formula. In this paper, we have implemented discrete element method (DEM) simulations to obtain the volumetric mean force exchanged between the granular phases with the size ratios greater than 10. First, the force is calculated directly from DEM averaged over a proper time window. Second, the continuum formula is applied to calculate the drag forces using the DEM quantities. We have shown the two volumetric forces are in good agreement as long as the homogeneity condition is maintained. However, the relative motion of larger particles in a cloud of finer particles imposes the inhomogeneous distribution of finer particles around the larger ones. We have presented correction factors to the volumetric force from continuum formula.

  18. Determination of zinc in environmental samples by solid phase spectrophotometry: optimization and validation study

    OpenAIRE

    Molina, Mar??a Francisca; Nechar, Mounir; Bosque-Sendra, Juan M.

    1998-01-01

    A simple and specific solid-phase spectrophotometric (SPS) determination of zinc in ??g dm-3 level has been developed based on the reaction of Zn(II) with 4-(2-pyridylazo)resorcinol (PAR) in the presence of potassium iodide; the product was then fixed on an anionic exchanger. The absorbance of the gel, packed in a 1 mm cell, is measured directly. PAR and KI concentrations were optimized simultaneously using response surface methodology (RSM) from sequential experimental Doehlert designs. The ...

  19. PFAS methods and guidance for sampling and analyzing water and other environmental media (Technical Brief)

    Science.gov (United States)

    EPA's methods for analyzing PFAS in environmental media are in various stages of development. This fact sheet summarizes EPA's analytical methods development for groundwater, surface water, wastewater, and solids, including soils, sediments, and biosolids

  20. PFAS Sampling Studies and Methods Development for Water and Other Environmental Media (Technical Brief)

    Science.gov (United States)

    EPA's methods for analyzing PFAS in environmental media are in various stages of development. This fact sheet summarizes EPA's analytical methods development for groundwater, surface water, wastewater, and solids, including soils, sediments, and biosolids

  1. Simultaneous spectrophotometric determination of trace copper, nickel, and cobalt ions in water samples using solid phase extraction coupled with partial least squares approaches

    Science.gov (United States)

    Guo, Yugao; Zhao, He; Han, Yelin; Liu, Xia; Guan, Shan; Zhang, Qingyin; Bian, Xihui

    2017-02-01

    A simultaneous spectrophotometric determination method for trace heavy metal ions based on solid-phase extraction coupled with partial least squares approaches was developed. In the proposed method, trace metal ions in aqueous samples were adsorbed by cation exchange fibers and desorbed by acidic solution from the fibers. After the ion preconcentration process, the enriched solution was detected by ultraviolet and visible spectrophotometer (UV-Vis). Then, the concentration of heavy metal ions were quantified by analyzing ultraviolet and visible spectrum with the help of partial least squares (PLS) approaches. Under the optimal conditions of operation time, flow rate and detection parameters, the overlapped absorption peaks of mixed ions were obtained. The experimental data showed that the concentration, which can be calculated through chemometrics method, of each metal ion increased significantly. The heavy metal ions can be enriched more than 80-fold. The limits of detection (LOD) for the target analytes of copper ions (Cu2 +), cobalt ions (Co2 +) and nickel ions (Ni2 +) mixture was 0.10 μg L- 1, 0.15 μg L- 1 and 0.13 μg L- 1, respectively. The relative standard deviations (RSD) were less than 5%. The performance of the solid-phase extraction can enrich the ions efficiently and the combined method of spectrophotometric detection and PLS can evaluate the ions concentration accurately. The work proposed here is an interesting and promising attempt for the trace ions determination in water samples and will have much more applied field.

  2. Rapid Quantification of the Toxic Alga Prymnesium parvum in Natural Samples by Use of a Specific Monoclonal Antibody and Solid-Phase Cytometry

    Science.gov (United States)

    West, N. J.; Bacchieri, R.; Hansen, G.; Tomas, C.; Lebaron, P.; Moreau, H.

    2006-01-01

    The increasing incidence of harmful algal blooms around the world and their associated health and economic effects require the development of methods to rapidly and accurately detect and enumerate the target species. Here we describe use of a solid-phase cytometer to detect and enumerate the toxic alga Prymnesium parvum in natural samples, using a specific monoclonal antibody and indirect immunofluorescence. The immunoglobulin G antibody 16E4 exhibited narrow specificity in that it recognized several P. parvum strains and a Prymnesium nemamethecum strain but it did not cross-react with P. parvum strains from Scandinavia or any other algal strains, including species of the closely related genus Chrysochromulina. Prymnesium sp. cells labeled with 16E4 were readily detected by the solid-phase cytometer because of the large fluorescence signal and the signal/noise ratio. Immunofluorescence detection and enumeration of cultured P. parvum cells preserved with different fixatives showed that the highest cell counts were obtained when cells were fixed with either glutaraldehyde or formaldehyde plus the cell protectant Pluronic F-68, whereas the use of formaldehyde alone resulted in significantly lower counts. Immunofluorescence labeling and analysis with the solid-phase cytometer of fixed natural samples from a bloom of P. parvum occurring in Lake Colorado in Texas gave cell counts that were close to those obtained by the traditional method of counting using light microscopy. These results show that a solid-phase cytometer can be used to rapidly enumerate natural P. parvum cells and that it could be used to detect other toxic algae, with an appropriate antibody or DNA probe. PMID:16391128

  3. Clustering Methods with Qualitative Data: A Mixed Methods Approach for Prevention Research with Small Samples

    Science.gov (United States)

    Henry, David; Dymnicki, Allison B.; Mohatt, Nathaniel; Allen, James; Kelly, James G.

    2016-01-01

    Qualitative methods potentially add depth to prevention research, but can produce large amounts of complex data even with small samples. Studies conducted with culturally distinct samples often produce voluminous qualitative data, but may lack sufficient sample sizes for sophisticated quantitative analysis. Currently lacking in mixed methods research are methods allowing for more fully integrating qualitative and quantitative analysis techniques. Cluster analysis can be applied to coded qualitative data to clarify the findings of prevention studies by aiding efforts to reveal such things as the motives of participants for their actions and the reasons behind counterintuitive findings. By clustering groups of participants with similar profiles of codes in a quantitative analysis, cluster analysis can serve as a key component in mixed methods research. This article reports two studies. In the first study, we conduct simulations to test the accuracy of cluster assignment using three different clustering methods with binary data as produced when coding qualitative interviews. Results indicated that hierarchical clustering, K-Means clustering, and latent class analysis produced similar levels of accuracy with binary data, and that the accuracy of these methods did not decrease with samples as small as 50. Whereas the first study explores the feasibility of using common clustering methods with binary data, the second study provides a “real-world” example using data from a qualitative study of community leadership connected with a drug abuse prevention project. We discuss the implications of this approach for conducting prevention research, especially with small samples and culturally distinct communities. PMID:25946969

  4. Clustering Methods with Qualitative Data: a Mixed-Methods Approach for Prevention Research with Small Samples.

    Science.gov (United States)

    Henry, David; Dymnicki, Allison B; Mohatt, Nathaniel; Allen, James; Kelly, James G

    2015-10-01

    Qualitative methods potentially add depth to prevention research but can produce large amounts of complex data even with small samples. Studies conducted with culturally distinct samples often produce voluminous qualitative data but may lack sufficient sample sizes for sophisticated quantitative analysis. Currently lacking in mixed-methods research are methods allowing for more fully integrating qualitative and quantitative analysis techniques. Cluster analysis can be applied to coded qualitative data to clarify the findings of prevention studies by aiding efforts to reveal such things as the motives of participants for their actions and the reasons behind counterintuitive findings. By clustering groups of participants with similar profiles of codes in a quantitative analysis, cluster analysis can serve as a key component in mixed-methods research. This article reports two studies. In the first study, we conduct simulations to test the accuracy of cluster assignment using three different clustering methods with binary data as produced when coding qualitative interviews. Results indicated that hierarchical clustering, K-means clustering, and latent class analysis produced similar levels of accuracy with binary data and that the accuracy of these methods did not decrease with samples as small as 50. Whereas the first study explores the feasibility of using common clustering methods with binary data, the second study provides a "real-world" example using data from a qualitative study of community leadership connected with a drug abuse prevention project. We discuss the implications of this approach for conducting prevention research, especially with small samples and culturally distinct communities.

  5. Fiber-based solid phase microextraction using fused silica lined bottles to collect, store, and stabilize a multianalyte headspace gas sample for offline analyses.

    Science.gov (United States)

    Harvey, Chris A; Carter, J Chance; Ertel, John R; Alviso, Cindy T; Chinn, Sarah C; Maxwell, Robert S

    2015-07-03

    We have developed a solid phase microextraction (SPME) sampling method using fused silica lined bottles (400 ml) to collect, store, and stabilize a headspace subsample from the source for subsequent offline, repetitive analyses of the gas using fiber-based SPME. The method enables long-term stability for repeated offline analysis of the organic species collected from the source headspace and retains all the advantages of fiber SPME sampling (e.g. rapid extraction, solvent free, simple and inexpensive) while providing additional advantages. Typically, the analytes collected on the SPME fiber must be desorbed and analyzed immediately to mitigate analyte loss or contamination. The new SPME sampling method, conducted offline using carboxen/polydimethylsiloxane (carboxen/PDMS - 85 μm) coated fibers, has been shown to be identical to in situ SPME sampling of a headspace acquired from an 80 component organic matrix with reproducibility demonstrated to be less than %RSD=7.0% for replicate samples measured over a 30-day period. In addition, repetitive samplings from one headspace aliquot are possible using one or more fibers and fiber types as well as quantitative options such as internal standard addition as demonstrated in a feasibility study using a benzene/toluene/xylene (BTX; 1 ppmv) certified gas standard, in which the SPME measurement precision (%RSD) was improved by a factor of 1.5-1.9 compared to the use of an external standard. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Methods for isolating, identifying, and quantifying anthocyanin metabolites in clinical samples.

    Science.gov (United States)

    de Ferrars, Rachel M; Czank, Charles; Saha, Shikha; Needs, Paul W; Zhang, Qingzhi; Raheem, K Saki; Botting, Nigel P; Kroon, Paul A; Kay, Colin D

    2014-10-21

    The metabolic fate of anthocyanins until recently was relatively unknown, primarily as a result of their instability at physiological pH and a lack of published methods for isolating and identifying their metabolites from biological samples. The aim of the present work was to establish methods for the extraction and quantification of anthocyanin metabolites present in urine, serum, and fecal samples. 35 commercial and 10 synthetic analytes, including both known and predicted human and microbial metabolites of anthocyanins, were obtained as reference standards. HPLC and MS/MS conditions were optimized for organic modifier, ionic modifier, mobile phase gradient, flow rate, column type, MS source, and compound dependent parameters. The impact of sorbent, solvent, acid, preservative, elution, and evaporation on solid phase extraction (SPE) efficiency was also explored. The HPLC-MS/MS method validation demonstrated acceptable linearity (R(2), 0.997 ± 0.002) and sensitivity (limits of detection (LODs): urine, 100 ± 375 nM; serum, 104 ± 358 nM; feces 138 ± 344 nM), and the final SPE methods provided recoveries of 88.3 ± 17.8% for urine, 86.5 ± 11.1% for serum, and 80.6 ± 20.9% for feces. The final methods were applied to clinical samples derived from an anthocyanin intervention study, where 36 of the 45 modeled metabolites were detected within urine, plasma, or fecal samples. The described methods provide suitable versatility for the identification and quantification of an extensive series of anthocyanin metabolites for use in future clinical studies exploring absorption, distribution, metabolism, and elimination.

  7. Pre-equilibrium solid-phase microextraction of free analyte in complex samples: correction for mass transfer variation from protein binding and matrix tortuosity.

    Science.gov (United States)

    Zhang, Xu; Oakes, Ken D; Hoque, Md Ehsanul; Luong, Di; Metcalfe, Chris D; Pawliszyn, Janusz; Servos, Mark R

    2011-05-01

    The accurate measurement of free analyte concentrations within complex sample matrixes by pre-equilibrium solid-phase microextraction (SPME) has proven challenging due to variations in mass uptake kinetics. For the first time, the effects of the sample binding matrix and tortuosity on the kinetics of analyte extraction (from the sample to the SPME fiber) are demonstrated to be quantitatively symmetrical with those of the desorption of preloaded deuterated standards (from the fiber to the sample matrix). Consequently, kinetic calibration methods can be employed to correct for variation in SPME sampling kinetics, facilitating the application of pre-equilibrium SPME within complex sample systems. This approach was applied ex vivo to measure pharmaceuticals in fish muscle tissues, with results consistent with those obtained from equilibrium SPME and microdialysis. The developed method has the inherent advantages of being more accurate, precise, and reproducible, thus providing the framework for applications where rapid measurement of free analyte concentrations (within complicated sample matrixes such as biological tissues, sediment, and surface water) are required.

  8. Simulation of Droplet Impacting on Elastic Solid with the SPH Method

    Directory of Open Access Journals (Sweden)

    Xiao-Jing Ma

    2015-01-01

    Full Text Available The phenomenon of droplet impacting on solid surfaces widely exists in both nature and engineering systems. However, one concern is that the microdeformation of solid surface is difficult to be observed and measured during the process of impacting. Since the microdeformation can directly affect the stability of the whole system, especially for the high-rate rotating components, it is necessary to study this phenomenon. Aiming at this problem, a new numerical simulation algorithm based on the Smoothed Particle Hydrodynamics (SPH method is brought forward to solve fluid-solid coupling and complex free surface problems in the paper. In order to test and analyze the feasibility and effectiveness of the improved SPH method, the process of a droplet impacting on an elastic plate was simulated. The numerical results show that the improved SPH method is able to present more detailed information about the microdeformation of solid surface. The influence of the elastic modulus of solid on the impacting process was also discussed.

  9. Preparation and evaluation of a novel molecularly imprinted polymer coating for selective extraction of indomethacin from biological samples by electrochemically controlled in-tube solid phase microextraction

    Energy Technology Data Exchange (ETDEWEB)

    Asiabi, Hamid [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Yamini, Yadollah, E-mail: yyamini@modares.ac.ir [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Seidi, Shahram; Ghahramanifard, Fazel [Department of Analytical Chemistry, Faculty of Chemistry, K.N. Toosi University of Technology, Tehran (Iran, Islamic Republic of)

    2016-03-24

    In the present work, an automated on-line electrochemically controlled in-tube solid-phase microextraction (EC-in-tube SPME) coupled with HPLC-UV was developed for the selective extraction and preconcentration of indomethacin as a model analyte in biological samples. Applying an electrical potential can improve the extraction efficiency and provide more convenient manipulation of different properties of the extraction system including selectivity, clean-up, rate, and efficiency. For more enhancement of the selectivity and applicability of this method, a novel molecularly imprinted polymer coated tube was prepared and applied for extraction of indomethacin. For this purpose, nanostructured copolymer coating consisting of polypyrrole doped with ethylene glycol dimethacrylate was prepared on the inner surface of a stainless-steel tube by electrochemical synthesis. The characteristics and application of the tubes were investigated. Electron microscopy provided a cross linked porous surface and the average thickness of the MIP coating was 45 μm. Compared with the non-imprinted polymer coated tubes, the special selectivity for indomethacin was discovered with the molecularly imprinted coated tube. Moreover, stable and reproducible responses were obtained without being considerably influenced by interferences commonly existing in biological samples. Under the optimal conditions, the limits of detection were in the range of 0.07–2.0 μg L{sup −1} in different matrices. This method showed good linearity for indomethacin in the range of 0.1–200 μg L{sup −1}, with coefficients of determination better than 0.996. The inter- and intra-assay precisions (RSD%, n = 3) were respectively in the range of 3.5–8.4% and 2.3–7.6% at three concentration levels of 7, 70 and 150 μg L{sup −1}. The results showed that the proposed method can be successfully applied for selective analysis of indomethacin in biological samples. - Graphical abstract: An automated on

  10. Optimization of solid-phase-extraction cleanup and validation of quantitative determination of eugenol in fish samples by gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Li, Jincheng; Zhang, Jing; Liu, Yang

    2015-08-01

    This paper describes a rapid and sensitive method for the determination of eugenol in fish samples, based on solid-phase extraction (SPE) and gas chromatography-tandem mass spectrometry (GC-MS-MS). Samples were extracted with acetonitrile, and then cleanup was performed using C18 solid-phase extraction (SPE). The determination of eugenol was achieved using an electron-ionization source (EI) in multiple-reaction-monitoring (MRM) mode. Under optimized conditions, the average recoveries of eugenol were in the range 94.85-103.61 % and the relative standard deviation (RSD) was lower than 12.0 %. The limit of detection (LOD) was 2.5 μg kg(-1) and the limit of quantification (LOQ) was 5.0 μg kg(-1). This method was applied to an exposure study of eugenol residue in carp muscle tissues. The results revealed that eugenol was nearly totally eliminated within 96 h. Graphical Abstract Flow diagram for sample pretreatment.

  11. Development of a new method for hydrogen isotope analysis of trace hydrocarbons in natural gas samples

    Directory of Open Access Journals (Sweden)

    Xibin Wang

    2016-12-01

    Full Text Available A new method had been developed for the analysis of hydrogen isotopic composition of trace hydrocarbons in natural gas samples by using solid phase microextraction (SPME combined with gas chromatography-isotope ratio mass spectrometry (GC/IRMS. In this study, the SPME technique had been initially introduced to achieve the enrichment of trace content of hydrocarbons with low abundance and coupled to GC/IRMS for hydrogen isotopic analysis. The main parameters, including the equilibration time, extraction temperature, and the fiber type, were systematically optimized. The results not only demonstrated that high extraction yield was true but also shows that the hydrogen isotopic fractionation was not observed during the extraction process, when the SPME device fitted with polydimethylsiloxane/divinylbenzene/carbon molecular sieve (PDMS/DVB/CAR fiber. The applications of SPME-GC/IRMS method were evaluated by using natural gas samples collected from different sedimentary basins; the standard deviation (SD was better than 4‰ for reproducible measurements; and also, the hydrogen isotope values from C1 to C9 can be obtained with satisfying repeatability. The SPME-GC/IRMS method fitted with PDMS/DVB/CAR fiber is well suited for the preconcentration of trace hydrocarbons, and provides a reliable hydrogen isotopic analysis for trace hydrocarbons in natural gas samples.

  12. Development of a sampling and analysis method for 4-vinyl-1-cyclohexene in air.

    Science.gov (United States)

    Kongtip, Pornpimol; Tangprakorn, Bantoon; Yoosook, Witaya; Chantanakul, Suttinun

    2008-01-01

    The purpose of this research was to develop an applicable sampling and analytical method to determine airborne 4-vinyl-1-cyclohexene concentrations which are usually found in the atmosphere of polybutadiene factories. A solid sorbent tube, containing two sections (100 mg in the front and 50 mg in the back) of activated coconut-shell charcoal was chosen for sampling 4-vinyl-1-cyclohexene vapor. The 4-vinyl-1-cyclohexene in the charcoal samples was desorbed with carbon disulfide and analyzed by gas chromatography equipped with a flame ionization detector. The suitable air flow rate, adsorption capacity, sample storage stability, desorption efficiency and reliability of the method for sampling and analysis of 4-vinyl-1-cyclohexene were evaluated. The method was applied to sampling and analysis of 4-vinyl-1-cyclohexene in the rubber industry. The results indicated a suitable air flow rate of 0.3 to 1.5 l/min. The adsorption capacity of 4-vinyl-1-cyclohexene on 100 mg of charcoal was 0.2134 mg. The 4-vinyl-1-cyclohexene adsorbed on the charcoal was stable for 7 d at room temperature or 21 d in a refrigerated condition. The average percent desorption efficiency of 4-vinyl-1-cyclohexene ranged from 90.45% to 97.04% with the loaded amount ranging from 0.412 to 8.250 microg using 1 ml carbon disulfide. The limit of detection of 4-vinyl-1-cyclohexene was 0.044 ng. The average percent recoveries (n=6) of 4-vinyl-1-cyclohexene adsorbed on charcoal ranging from 0.46 to 8.87 microg were 96.78-102.87% with relative standard deviations (RSDs) of 0.34-1.92%, respectively. The concentrations of 4-vinyl-1-cyclohexene ranged from 0.011 to 0.105 mg/m(3) in the working environment of a polybutadiene factory.

  13. Method of remotely characterizing thermal properties of a sample

    Science.gov (United States)

    Heyman, Joseph S. (Inventor); Heath, D. Michele (Inventor); Welch, Christopher (Inventor); Winfree, William P. (Inventor); Miller, William E. (Inventor)

    1992-01-01

    A sample in a wind tunnel is radiated from a thermal energy source outside of the wind tunnel. A thermal imager system, also located outside of the wind tunnel, reads surface radiations from the sample as a function of time. The produced thermal images are characteristic of the heat transferred from the sample to the flow across the sample. In turn, the measured rates of heat loss of the sample are characteristic of the flow and the sample.

  14. Passive sampling methods for contaminated sediments: risk assessment and management.

    Science.gov (United States)

    Greenberg, Marc S; Chapman, Peter M; Allan, Ian J; Anderson, Kim A; Apitz, Sabine E; Beegan, Chris; Bridges, Todd S; Brown, Steve S; Cargill, John G; McCulloch, Megan C; Menzie, Charles A; Shine, James P; Parkerton, Thomas F

    2014-04-01

    This paper details how activity-based passive sampling methods (PSMs), which provide information on bioavailability in terms of freely dissolved contaminant concentrations (Cfree ), can be used to better inform risk management decision making at multiple points in the process of assessing and managing contaminated sediment sites. PSMs can increase certainty in site investigation and management, because Cfree is a better predictor of bioavailability than total bulk sediment concentration (Ctotal ) for 4 key endpoints included in conceptual site models (benthic organism toxicity, bioaccumulation, sediment flux, and water column exposures). The use of passive sampling devices (PSDs) presents challenges with respect to representative sampling for estimating average concentrations and other metrics relevant for exposure and risk assessment. These challenges can be addressed by designing studies that account for sources of variation associated with PSMs and considering appropriate spatial scales to meet study objectives. Possible applications of PSMs include: quantifying spatial and temporal trends in bioavailable contaminants, identifying and evaluating contaminant source contributions, calibrating site-specific models, and, improving weight-of-evidence based decision frameworks. PSM data can be used to assist in delineating sediment management zones based on likelihood of exposure effects, monitor remedy effectiveness, and, evaluate risk reduction after sediment treatment, disposal, or beneficial reuse after management actions. Examples are provided illustrating why PSMs and freely dissolved contaminant concentrations (Cfree ) should be incorporated into contaminated sediment investigations and study designs to better focus on and understand contaminant bioavailability, more accurately estimate exposure to sediment-associated contaminants, and better inform risk management decisions. Research and communication needs for encouraging broader use are discussed. © 2014

  15. Passive sampling methods for contaminated sediments: Risk assessment and management

    Science.gov (United States)

    Greenberg, Marc S; Chapman, Peter M; Allan, Ian J; Anderson, Kim A; Apitz, Sabine E; Beegan, Chris; Bridges, Todd S; Brown, Steve S; Cargill, John G; McCulloch, Megan C; Menzie, Charles A; Shine, James P; Parkerton, Thomas F

    2014-01-01

    This paper details how activity-based passive sampling methods (PSMs), which provide information on bioavailability in terms of freely dissolved contaminant concentrations (Cfree), can be used to better inform risk management decision making at multiple points in the process of assessing and managing contaminated sediment sites. PSMs can increase certainty in site investigation and management, because Cfree is a better predictor of bioavailability than total bulk sediment concentration (Ctotal) for 4 key endpoints included in conceptual site models (benthic organism toxicity, bioaccumulation, sediment flux, and water column exposures). The use of passive sampling devices (PSDs) presents challenges with respect to representative sampling for estimating average concentrations and other metrics relevant for exposure and risk assessment. These challenges can be addressed by designing studies that account for sources of variation associated with PSMs and considering appropriate spatial scales to meet study objectives. Possible applications of PSMs include: quantifying spatial and temporal trends in bioavailable contaminants, identifying and evaluating contaminant source contributions, calibrating site-specific models, and, improving weight-of-evidence based decision frameworks. PSM data can be used to assist in delineating sediment management zones based on likelihood of exposure effects, monitor remedy effectiveness, and, evaluate risk reduction after sediment treatment, disposal, or beneficial reuse after management actions. Examples are provided illustrating why PSMs and freely dissolved contaminant concentrations (Cfree) should be incorporated into contaminated sediment investigations and study designs to better focus on and understand contaminant bioavailability, more accurately estimate exposure to sediment-associated contaminants, and better inform risk management decisions. Research and communication needs for encouraging broader use are discussed. Integr

  16. A headspace SPME-GC-ECD method suitable for determination of chlorophenols in water samples.

    Science.gov (United States)

    de Morais, Paulo; Stoichev, Teodor; Basto, M Clara P; Carvalho, Pedro N; Vasconcelos, M Teresa S D

    2011-03-01

    A headspace solid phase microextraction coupled to gas chromatography with electron capture detector (HS-SPME-GC-ECD) method was optimized for the determination of seven chlorophenols (CPs) with different levels of chlorination. This is the first time that HS-SPME-GC-ECD with acetylation of the analytes is used for the simultaneous determination of CPs in water samples. The influence of fibre type, derivatization conditions, salt addition, temperature and time of extraction and temperature of desorption was checked. Possible sources of contamination and analyte losses were considered. The best results were obtained with the polydimethylsiloxane/divinylbenzene fibre, derivatization by acetylation using 100 μL of acetic anhydride and 0.1 g of anhydrous sodium carbonate per 10 mL of sample, salt addition of 100 g L(-1) sodium chloride, extraction at 70 °C for 60 min and desorption in the GC injector at 260 °C for 6 min. The limits of detection (LOD) for monochlorophenols were 12 and 122 ng L(-1) for 2-chlorophenol and 4-chlorophenol, respectively. For polychlorinated CPs, the LODs were lower than 6 ng L(-1), values similar to the existing methods that use SPME with derivatization for CPs determination in water samples. The method is suitable for the determination of CPs in most environmental aqueous samples. Repeatability and reproducibility were less than 16.8% and 11.7%, respectively. The optimized method was successfully applied for the analysis of waters with complex matrices such as river and estuarine water samples.

  17. A solid phase extraction procedure for the simultaneous determination of total inorganic arsenic and trace metals in seawater: Sample preparation for total-reflection X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Staniszewski, B. [Department of Analytical Chemistry, Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan (Poland)], E-mail: bstanisz@amu.edu.pl; Freimann, P. [Bundesamt fuer Seeschifffahrt und Hydrographie, Wuestland 2, 22589 Hamburg (Germany)], E-mail: peter.freimann@bsh.de

    2008-11-15

    In this paper we present a procedure allowing total-reflection X-ray fluorescence spectrometry (TXRF) determinations of arsenic in water samples, especially in seawater samples. The procedure consists of an arsenate reduction step (performed by using a L-cysteine solution) followed by a complexation of As{sup +3} with sodium dibenzyldithiocarbamate and solid phase extraction. The new procedure is a modification of a method developed by Prange and allows a simultaneous determination of As together with V, Fe, Ni, Cu, Zn, Pb, and U in seawater by TXRF. The procedure was tested using the Certified Reference Material CASS-4 and was later applied to regular seawater samples collected from the North Sea. The detection limit for arsenic is 10 ng L{sup -1}.

  18. A solid phase extraction procedure for the simultaneous determination of total inorganic arsenic and trace metals in seawater: Sample preparation for total-reflection X-ray fluorescence

    Science.gov (United States)

    Staniszewski, B.; Freimann, P.

    2008-11-01

    In this paper we present a procedure allowing total-reflection X-ray fluorescence spectrometry (TXRF) determinations of arsenic in water samples, especially in seawater samples. The procedure consists of an arsenate reduction step (performed by using a L-cysteine solution) followed by a complexation of As +3 with sodium dibenzyldithiocarbamate and solid phase extraction. The new procedure is a modification of a method developed by Prange and allows a simultaneous determination of As together with V, Fe, Ni, Cu, Zn, Pb, and U in seawater by TXRF. The procedure was tested using the Certified Reference Material CASS-4 and was later applied to regular seawater samples collected from the North Sea. The detection limit for arsenic is 10 ng L - 1 .

  19. Method for Computing the Anisotropy of the Solid-Liquid Interfacial Free Energy

    Energy Technology Data Exchange (ETDEWEB)

    Hoyt, J. J.; Asta, Mark; Karma, Alain

    2001-06-11

    We present a method to compute accurately the weak anisotropy of the solid-liquid interfacial free energy, a parameter which influences dendritic evolution in materials with atomically rough interfaces. The method is based on monitoring interfacial fluctuations during molecular dynamics simulation and extracting the interfacial stiffness which is an order of magnitude more anisotropic than the interfacial free energy. We present results for pure Ni with interatomic potentials derived from the embedded atom method.

  20. Method for Computing the Anisotropy of the Solid-Liquid Interfacial Free Energy

    Science.gov (United States)

    Hoyt, J. J.; Asta, Mark; Karma, Alain

    2001-06-01

    We present a method to compute accurately the weak anisotropy of the solid-liquid interfacial free energy, a parameter which influences dendritic evolution in materials with atomically rough interfaces. The method is based on monitoring interfacial fluctuations during molecular dynamics simulation and extracting the interfacial stiffness which is an order of magnitude more anisotropic than the interfacial free energy. We present results for pure Ni with interatomic potentials derived from the embedded atom method.

  1. A comparison of methods for representing sparsely sampled random quantities.

    Energy Technology Data Exchange (ETDEWEB)

    Romero, Vicente Jose; Swiler, Laura Painton; Urbina, Angel; Mullins, Joshua

    2013-09-01

    This report discusses the treatment of uncertainties stemming from relatively few samples of random quantities. The importance of this topic extends beyond experimental data uncertainty to situations involving uncertainty in model calibration, validation, and prediction. With very sparse data samples it is not practical to have a goal of accurately estimating the underlying probability density function (PDF). Rather, a pragmatic goal is that the uncertainty representation should be conservative so as to bound a specified percentile range of the actual PDF, say the range between 0.025 and .975 percentiles, with reasonable reliability. A second, opposing objective is that the representation not be overly conservative; that it minimally over-estimate the desired percentile range of the actual PDF. The presence of the two opposing objectives makes the sparse-data uncertainty representation problem interesting and difficult. In this report, five uncertainty representation techniques are characterized for their performance on twenty-one test problems (over thousands of trials for each problem) according to these two opposing objectives and other performance measures. Two of the methods, statistical Tolerance Intervals and a kernel density approach specifically developed for handling sparse data, exhibit significantly better overall performance than the others.

  2. An adaptive sampling and windowing interrogation method in PIV

    Science.gov (United States)

    Theunissen, R.; Scarano, F.; Riethmuller, M. L.

    2007-01-01

    This study proposes a cross-correlation based PIV image interrogation algorithm that adapts the number of interrogation windows and their size to the image properties and to the flow conditions. The proposed methodology releases the constraint of uniform sampling rate (Cartesian mesh) and spatial resolution (uniform window size) commonly adopted in PIV interrogation. Especially in non-optimal experimental conditions where the flow seeding is inhomogeneous, this leads either to loss of robustness (too few particles per window) or measurement precision (too large or coarsely spaced interrogation windows). Two criteria are investigated, namely adaptation to the local signal content in the image and adaptation to local flow conditions. The implementation of the adaptive criteria within a recursive interrogation method is described. The location and size of the interrogation windows are locally adapted to the image signal (i.e., seeding density). Also the local window spacing (commonly set by the overlap factor) is put in relation with the spatial variation of the velocity field. The viability of the method is illustrated over two experimental cases where the limitation of a uniform interrogation approach appears clearly: a shock-wave-boundary layer interaction and an aircraft vortex wake. The examples show that the spatial sampling rate can be adapted to the actual flow features and that the interrogation window size can be arranged so as to follow the spatial distribution of seeding particle images and flow velocity fluctuations. In comparison with the uniform interrogation technique, the spatial resolution is locally enhanced while in poorly seeded regions the level of robustness of the analysis (signal-to-noise ratio) is kept almost constant.

  3. Geothermal water and gas: collected methods for sampling and analysis. Comment issue. [Compilation of methods

    Energy Technology Data Exchange (ETDEWEB)

    Douglas, J.G.; Serne, R.J.; Shannon, D.W.; Woodruff, E.M.

    1976-08-01

    A collection of methods for sampling and analysis of geothermal fluids and gases is presented. Compilations of analytic options for constituents in water and gases are given. Also, a survey of published methods of laboratory water analysis is included. It is stated that no recommendation of the applicability of the methods to geothermal brines should be assumed since the intent of the table is to encourage and solicit comments and discussion leading to recommended analytical procedures for geothermal waters and research. (WHK)

  4. Pre-concentration and determination of zinc in water samples by ligand assisted pseudo stirbar hollow fiber solid/liquid phase microextraction

    Directory of Open Access Journals (Sweden)

    Zarrin Es’haghi

    2017-05-01

    Full Text Available Pre-concentration and determination of Zn (II across a ligand assisted pseudo stirbar hollow fiber solid/liquid phase microextraction method in water samples has been investigated. All detections were carried out by differential pulse anodic stripping voltammetry (DPASV. The method involves microextraction and pre-concentration of Zn (II on the pseudo stir bar hollow fiber. Then desorption has been done using suitable solvent containing suitable ligand as complexing agent. The optimized conditions were obtained. The relationship between the peak current and concentration was linear over the range of 0.05–500 ng mL−1. The limit of detection was 0.015 ng mL−1. Under the optimized conditions, the pre-concentration factor is 5140. The applicability of the developed technique was evaluated by application to spiked, environmental water samples.

  5. Application of NaClO-treated multiwalled carbon nanotubes as solid phase extraction sorbents for preconcentration of trace 2,4-dichlorophenoxyacetic acid in aqueous samples.

    Science.gov (United States)

    Lu, Ping; Deng, Dayi; Ni, Xiaodan

    2012-09-01

    Multiwalled carbon nanotubes functionalized by oxidation of original multiwalled carbon nanotubes with NaClO were prepared and their application as solid phase extraction sorbent for 2,4-dichlorophenoxyacetic acid (2,4-D) was investigated systemically, and a new method was developed for the determination of trace 2,4-D in water samples based on extraction and preconcentration of 2,4-D with solid phase extraction columns packed with NaClO-treated multiwalled carbon nanotubes prior to its determination by HPLC. The optimum experimental parameters for preconcentration of 2,4-D, including the column activating conditions, the amount of the sorbent, pH of the sample, elution composition, and elution volume, were investigated. The results indicated 2,4-D could be quantitatively retained by 100 mg NaClO-treated multiwalled carbon nanotubes at pH 5, and then eluted completely with 10 mL 3:1 (v/v) methanol-ammonium acetate solution (0.3 mol/L). The detection limit of this method for 2,4-D was 0.15 μg/L, and the relative standard deviation was 2.3% for fortified tap water samples and 2.5% for fortified riverine water sample at the 10 μg/L level. The method was validated using fortified tap water and riverine water samples with known amount of 2,4-D at the 0.4, 10, and 30 μg/L levels, respectively. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. A fictitious domain method for fluid/solid coupling applied to the lithosphere/asthenosphere interaction.

    Science.gov (United States)

    Cerpa, Nestor; Hassani, Riad; Gerbault, Muriel

    2014-05-01

    A large variety of geodynamical problems can be viewed as a solid/fluid interaction problem coupling two bodies with different physics. In particular the lithosphere/asthenosphere mechanical interaction in subduction zones belongs to this kind of problem, where the solid lithosphere is embedded in the asthenospheric viscous fluid. In many fields (Industry, Civil Engineering,etc.), in which deformations of solid and fluid are "small", numerical modelers consider the exact discretization of both domains and fit as well as possible the shape of the interface between the two domains, solving the discretized physic problems by the Finite Element Method (FEM). Although, in a context of subduction, the lithosphere is submitted to large deformation, and can evolve into a complex geometry, thus leading to important deformation of the surrounding asthenosphere. To alleviate the precise meshing of complex geometries, numerical modelers have developed non-matching interface methods called Fictitious Domain Methods (FDM). The main idea of these methods is to extend the initial problem to a bigger (and simpler) domain. In our version of FDM, we determine the forces at the immersed solid boundary required to minimize (at the least square sense) the difference between fluid and solid velocities at this interface. This method is first-order accurate and the stability depends on the ratio between the fluid background mesh size and the interface discretization. We present the formulation and provide benchmarks and examples showing the potential of the method : 1) A comparison with an analytical solution of a viscous flow around a rigid body. 2) An experiment of a rigid sphere sinking in a viscous fluid (in two and three dimensional cases). 3) A comparison with an analog subduction experiment. Another presentation aims at describing the geodynamical application of this method to Andean subduction dynamics, studying cyclic slab folding on the 660 km discontinuity, and its relationship

  7. Paper-based solid-phase microextraction for analysis of 8-hydroxy-2'-deoxyguanosine in urine sample by CE-LIF.

    Science.gov (United States)

    Meng, Xiangying; Liu, Qinrui; Ding, Yongsheng

    2017-02-01

    An easy-to-do paper-based solid-phase microextraction (p-SPME) was developed for determination of 8-hydroxy-2'-deoxyguanosine (8-OHdG) in urine sample by CE-LIF. Small piece of filter paper was used as a solid phase to extract 8-OHdG from urine sample. Its primary mechanism is based on the hydrogen-bonding interaction between 8-OHdG and cellulose molecules. The effects of the pH of the sample solution, extraction time, and temperature on the peak area of the analyte were investigated in order to obtain the optimal p-SPME conditions. Comparing with the untreated sample, the p-SPME can significantly reduce the interference to the separation of 8-OHdG by CE-LIF. Meanwhile, the p-SPEM can provide more than three times concentrated effect. The developed method was evaluated according to an FDA guideline for biological analysis. The precisions (RSD%, n = 5) of the peak area and migration time of the analyte at three different concentrations were within 3.02-5.82% and 0.92-1.58%, respectively. The limit of identification of the method is about 5 nM according to the significant difference between two sets of the samples with and without spiking the standard (Student's t-test, p 0.99) based on the standard addition. The recoveries at three different concentrations were within 99.8-103.5%. The results of the real sample analysis are consistent with those reported in our previous paper (Electrophoresis 2014, 35, 1873-1879). © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Usefulness of endoscopic ultrasound-guided sampling using core biopsy needle as a percutaneous biopsy rescue for diagnosis of solid liver mass: Combined histological-cytological analysis.

    Science.gov (United States)

    Lee, Yun Nah; Moon, Jong Ho; Kim, Hee Kyung; Choi, Hyun Jong; Choi, Moon Han; Kim, Dong Choon; Lee, Tae Hee; Lee, Tae Hoon; Cha, Sang-Woo; Kim, Sang Gyune; Kim, Young Seok

    2015-07-01

    Endoscopic ultrasound (EUS)-guided fine needle aspiration (EUS-FNA) is one of the alternative methods for tissue sampling of liver solid mass. However, the diagnostic efficacy using cytology alone was limited. In this study, we evaluate the diagnostic accuracy of EUS-guided fine needle biopsy (EUS-FNB) as a percutaneous biopsy rescue for liver solid mass. The EUS-FNB using core biopsy needle for liver solid mass was performed prospectively for patients who were failure to acquire a tissue or achieve a diagnosis using percutaneous liver biopsy. The primary outcome was the diagnostic accuracy of EUS-FNB for malignancy and specific tumor type. The secondary outcomes were the median numbers of passes required to establish a diagnosis, the proportions of patients in whom immunohistochemical (IHC) stain was possible and obtained adequate specimen, and safety of EUS-FNB. Twenty-one patients (12 women; mean age, 63 years [range, 37-81]) underwent EUS-FNB for solid liver masses. The median number of needle passes was 2.0 (range, 1-5). On-site cytology and cytology with Papanicolaou stain showed malignancy in 16 patients (76.2%) and 17 patients (81.0%), respectively. In histology with HE stain, 19 patients (90.5%) were diagnosed malignancy and optimal to IHC stain. The overall diagnostic accuracy for malignancy and specific tumor type were 90.5% and 85.7%, respectively. No complications were seen. EUS-FNB with core biopsy needle for solid liver mass may be helpful in the management of patients who are unable to diagnose using percutaneous liver biopsy. © 2015 Journal of Gastroenterology and Hepatology Foundation and Wiley Publishing Asia Pty Ltd.

  9. Peptide Synthesis Method and Solid Support for Use in the Method

    DEFF Research Database (Denmark)

    1994-01-01

    or proteins in a parallel and substantially simultaneous fashion. Preferred embodiments of a solid support for performing the synthesis are prepared from thin polyethylene sheet or film which has been grafted with polystyrene chains in a radical-initiated process in which the polyethylene sheet or film...

  10. A solid-state NMR method for solution of zeolite crystal structures.

    Science.gov (United States)

    Brouwer, Darren H; Darton, Richard J; Morris, Russell E; Levitt, Malcolm H

    2005-07-27

    Since zeolites are notoriously difficult to prepare as large single crystals, structure determination usually relies on powder X-ray diffraction (XRD). However, structure solution (i.e., deriving an initial structural model) directly from powder XRD data is often very difficult due to the diffraction phase problem and the high degree of overlap between the individual reflections, particularly for materials with the structural complexity of most zeolites. Here, we report a method for structure determination of zeolite crystal structures that combines powder XRD and nuclear magnetic resonance (NMR) spectroscopy in which the crucial step of structure solution is achieved using solid-state (29)Si double-quantum dipolar recoupling NMR, which probes the distance-dependent dipolar interactions between naturally abundant (29)Si nuclei in the zeolite framework. For two purely siliceous zeolite blind test samples, we demonstrate that the NMR data can be combined with the unit cell parameters and space group to solve structural models that refine successfully against the powder XRD data.

  11. A simple capacitive method to evaluate ethanol fuel samples

    Science.gov (United States)

    Vello, Tatiana P.; de Oliveira, Rafael F.; Silva, Gustavo O.; de Camargo, Davi H. S.; Bufon, Carlos C. B.

    2017-02-01

    Ethanol is a biofuel used worldwide. However, the presence of excessive water either during the distillation process or by fraudulent adulteration is a major concern in the use of ethanol fuel. High water levels may cause engine malfunction, in addition to being considered illegal. Here, we describe the development of a simple, fast and accurate platform based on nanostructured sensors to evaluate ethanol samples. The device fabrication is facile, based on standard microfabrication and thin-film deposition methods. The sensor operation relies on capacitance measurements employing a parallel plate capacitor containing a conformational aluminum oxide (Al2O3) thin layer (15 nm). The sensor operates over the full range water concentration, i.e., from approximately 0% to 100% vol. of water in ethanol, with water traces being detectable down to 0.5% vol. These characteristics make the proposed device unique with respect to other platforms. Finally, the good agreement between the sensor response and analyses performed by gas chromatography of ethanol biofuel endorses the accuracy of the proposed method. Due to the full operation range, the reported sensor has the technological potential for use as a point-of-care analytical tool at gas stations or in the chemical, pharmaceutical, and beverage industries, to mention a few.

  12. Martian Radiative Transfer Modeling Using the Optimal Spectral Sampling Method

    Science.gov (United States)

    Eluszkiewicz, J.; Cady-Pereira, K.; Uymin, G.; Moncet, J.-L.

    2005-01-01

    The large volume of existing and planned infrared observations of Mars have prompted the development of a new martian radiative transfer model that could be used in the retrievals of atmospheric and surface properties. The model is based on the Optimal Spectral Sampling (OSS) method [1]. The method is a fast and accurate monochromatic technique applicable to a wide range of remote sensing platforms (from microwave to UV) and was originally developed for the real-time processing of infrared and microwave data acquired by instruments aboard the satellites forming part of the next-generation global weather satellite system NPOESS (National Polarorbiting Operational Satellite System) [2]. As part of our on-going research related to the radiative properties of the martian polar caps, we have begun the development of a martian OSS model with the goal of using it to perform self-consistent atmospheric corrections necessary to retrieve caps emissivity from the Thermal Emission Spectrometer (TES) spectra. While the caps will provide the initial focus area for applying the new model, it is hoped that the model will be of interest to the wider Mars remote sensing community.

  13. Numerical study of MPS method with large eddy simulation for fluid solid coupling problem

    Science.gov (United States)

    YANG, Chao; ZHANG, Huaixin; YAO, Huilan

    2017-02-01

    The Moving-Particle Semi-implicit method (MPS) is a kind of meshless Lagrangian calculation method. This method uses particles instead of mesh. In the pretreatment it works simply and conveniently and has high computational efficiency. In practical engineering, many of fluid problems are turbulent flows. Large eddy simulation is a major means of studying turbulence. Fluid-structure coupling is an independent branch of mechanics combined with fluid dynamics and solid mechanics, which is the hot and difficult area of research in many fields at present. In this paper, for the numerical simulation of turbulent flow with interaction of fluid-structure, the modified MPS-LES method is applied in two dimensional dam-break problem. It proves that MPS-LES method can be extended on solving the fluid-solid coupled problem.

  14. Facile synthesis of magnetic carbon nitride nanosheets and its application in magnetic solid phase extraction for polycyclic aromatic hydrocarbons in edible oil samples.

    Science.gov (United States)

    Zheng, Hao-Bo; Ding, Jun; Zheng, Shu-Jian; Zhu, Gang-Tian; Yuan, Bi-Feng; Feng, Yu-Qi

    2016-01-01

    In this study, we proposed a method to fabricate magnetic carbon nitride (CN) nanosheets by simple physical blending. Low-cost CN nanosheets prepared by urea possessed a highly π-conjugated structure; therefore the obtained composites were employed as magnetic solid-phase extraction (MSPE) sorbent for extraction of polycyclic aromatic hydrocarbons (PAHs) in edible oil samples. Moreover, sample pre-treatment time could be carried out within 10 min. Thus, a simple and cheap method for the analysis of PAHs in edible oil samples was established by coupling magnetic CN nanosheets-based MSPE with gas chromatography-mass spectrometry (GC/MS) analysis. Limits of quantitation (LOQs) for eight PAHs ranged from 0.4 to 0.9 ng/g. The intra- and inter-day relative standard deviations (RSDs) were less than 15.0%. The recoveries of PAHs for spiked soybean oil samples ranged from 91.0% to 124.1%, with RSDs of less than 10.2%. Taken together, the proposed method offers a simple and cost-effective option for the convenient analysis of PAHs in oil samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. A fixed-mesh method for incompressible flow structure systems with finite solid deformations

    Science.gov (United States)

    Zhao, Hong; Freund, Jonathan B.; Moser, Robert D.

    2008-03-01

    A fixed-mesh algorithm is proposed for simulating flow-structure interactions such as those occurring in biological systems, in which both the fluid and solid are incompressible and the solid deformations are large. Several of the well-known difficulties in simulating such flow-structure interactions are avoided by formulating a single set of equations of motion on a fixed Eulerian mesh. The solid's deformation is tracked to compute elastic stresses by an overlapping Lagrangian mesh. In this way, the flow-structure interaction is formulated as a distributed body force and singular surface force acting on an otherwise purely fluid system. These forces, which depend on the solid elastic stress distribution, are computed on the Lagrangian mesh by a standard finite-element method and then transferred to the fixed Eulerian mesh, where the joint momentum and continuity equations are solved by a finite-difference method. The constitutive model for the solid can be quite general. For the force transfer, standard immersed-boundary and immersed-interface methods can be used and are demonstrated. We have also developed and demonstrated a new projection method that unifies the transfer of the surface and body forces in a way that exactly conserves momentum; the interface is still effectively sharp for this approach. The spatial convergence of the method is observed to be between first- and second-order, as in most immersed-boundary methods for membrane flows. The algorithm is demonstrated by the simulations of an advected elastic disk, a flexible leaflet in an oscillating flow, and a model of a swimming jellyfish.

  16. A novel method for estimating solid fraction of roller-compacted ribbons.

    Science.gov (United States)

    Nkansah, Paul; Wu, Sy-Juen; Sobotka, Stephanie; Yamamoto, Ken; Shao, Zezhi J

    2008-02-01

    A simple method has been developed to estimate solid fraction or relative density of compacts using the weight of ribbons produced during roller compaction. The method provides an alternative to the commonly used dimensional measurement, especially for formulations not amenable to forming quality ribbons. Surface texture of the compaction rolls has been taken into consideration in our mathematical treatment along with correction for ribbon relaxation. Ribbon relaxation occurring upon ribbon exiting the compaction zone is estimated using roll geometry, roll gap, and ribbon thickness. Detailed experimental runs have been carried out to confirm the validity of the proposed theory. The predicted solid fraction was found comparable to that from actual dimensional measurement by caliper. In the case of the microcrystalline cellulose/dicalcium phosphate one:one formulation, the predicted solid fraction had an error sum of squares (SSE) of 2.64E-03 when compared to the dimensional method. When relaxation was included, the SSE decreased by four folds. Similarly, for the microcrystalline cellulose/lactose monohydrate 2:1 formulation, the SSE decreased twelfth folds when relaxation was taken into consideration. These results further confirm the utility of the proposed throughput method for estimating the solid fraction of ribbons.

  17. Effect of solid distribution on elastic properties of open-cell cellular solids using numerical and experimental methods.

    Science.gov (United States)

    Zargarian, A; Esfahanian, M; Kadkhodapour, J; Ziaei-Rad, S

    2014-09-01

    Effect of solid distribution between edges and vertices of three-dimensional cellular solid with an open-cell structure was investigated both numerically and experimentally. Finite element analysis (FEA) with continuum elements and appropriate periodic boundary condition was employed to calculate the elastic properties of cellular solids using tetrakaidecahedral (Kelvin) unit cell. Relative densities between 0.01 and 0.1 and various values of solid fractions were considered. In order to validate the numerical model, three scaffolds with the relative density of 0.08, but different amounts of solid in vertices, were fabricated via 3-D printing technique. Good agreement was observed between numerical simulation and experimental results. Results of numerical simulation showed that, at low relative densities (numerical simulation and considering the relative density and solid fraction in vertices, empirical relations were derived for Young׳s modulus and Poisson׳s ratio. Copyright © 2014 Elsevier Ltd. All rights reserved.

  18. Multielemental speciation analysis of organometallic compounds of mercury, lead and tin in natural water samples by headspace-solid phase microextraction followed by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Centineo, Giuseppe; González, Elisa Blanco; Sanz-Medel, Alfredo

    2004-04-23

    The development of a simple and rapid multielemental speciation method is described with the ultimate goal to simultaneously determine various organometallic compounds of mercury, lead and tin (inorganic mercury, methylmercury, trimethyllead, triethyllead, monobutyl-, dibutyl- and tributyltin) in natural water samples. The analytical method consists on the ethylation with NaBEt4, simultaneous headspace-solid phase microextraction (HS-SPME) of the derivatives and final gas chromatographic-mass spectrometric (GC-MS) analysis. After optimization of important process parameters, like SPME fiber coating, extraction time and extraction temperature, the analytical characteristics were evaluated. Detection limits in the low ng l(-1) level, linearity over three orders of magnitude and repeatability in the range of 3-20% were achieved for all compounds under study. The accuracy of the method in terms of average percentage recovery of the compounds in spiked river water and seawater samples was better than 90%. Finally, application of the proposed method to real natural aqueous samples enabled the simultaneous determination of all the compounds under study in seawater samples obtained from the marina area of Gijón (Asturias, Spain).

  19. Freeze-thaw method improves the detection of volatile compounds in insects using Headspace Solid-Phase Microextraction (HS-SPME)

    Science.gov (United States)

    Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography–mass spectrometry (GC-MS) is commonly used in analyzing insect volatiles. In order to improve the detection of volatiles in insects, a freeze-thaw method was applied to insect samples before the HS-SPME-GC-MS analysis. ...

  20. A novel flow injection chemiluminescence method for automated and miniaturized determination of phenols in smoked food samples.

    Science.gov (United States)

    Vakh, Christina; Evdokimova, Ekaterina; Pochivalov, Aleksei; Moskvin, Leonid; Bulatov, Andrey

    2017-12-15

    An easily performed fully automated and miniaturized flow injection chemiluminescence (CL) method for determination of phenols in smoked food samples has been proposed. This method includes the ultrasound assisted solid-liquid extraction coupled with gas-diffusion separation of phenols from smoked food sample and analytes absorption into a NaOH solution in a specially designed gas-diffusion cell. The flow system was designed to focus on automation and miniaturization with minimal sample and reagent consumption by inexpensive instrumentation. The luminol - N-bromosuccinimide system in an alkaline medium was used for the CL determination of phenols. The limit of detection of the proposed procedure was 3·10 -8 ·molL -1 (0.01mgkg -1 ) in terms of phenol. The presented method demonstrated to be a good tool for easy, rapid and cost-effective point-of-need screening phenols in smoked food samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

  1. Probing methane hydrate nucleation through the forward flux sampling method.

    Science.gov (United States)

    Bi, Yuanfei; Li, Tianshu

    2014-11-26

    Understanding the nucleation of hydrate is the key to developing effective strategies for controlling methane hydrate formation. Here we present a computational study of methane hydrate nucleation, by combining the forward flux sampling (FFS) method and the coarse-grained water model mW. To facilitate the application of FFS in studying the formation of methane hydrate, we developed an effective order parameter λ on the basis of the topological analysis of the tetrahedral network. The order parameter capitalizes the signature of hydrate structure, i.e., polyhedral cages, and is capable of efficiently distinguishing hydrate from ice and liquid water while allowing the formation of different hydrate phases, i.e., sI, sII, and amorphous. Integration of the order parameter λ with FFS allows explicitly computing hydrate nucleation rates and obtaining an ensemble of nucleation trajectories under conditions where spontaneous hydrate nucleation becomes too slow to occur in direct simulation. The convergence of the obtained hydrate nucleation rate was found to depend crucially on the convergence of the spatial distribution for the spontaneously formed hydrate seeds obtained from the initial sampling of FFS. The validity of the approach is also verified by the agreement between the calculated nucleation rate and that inferred from the direct simulation. Analyzing the obtained large ensemble of hydrate nucleation trajectories, we show hydrate formation at 220 K and 500 bar is initiated by the nucleation events occurring in the vicinity of water-methane interface, and facilitated by a gradual transition from amorphous to crystalline structure. The latter provides the direct support to the proposed two-step nucleation mechanism of methane hydrate.

  2. Comparison of two methods of tear sampling for protein quantification by Bradford method

    Directory of Open Access Journals (Sweden)

    Eliana Farias

    2013-02-01

    Full Text Available The aim of this study was to compare two methods of tear sampling for protein quantification. Tear samples were collected from 29 healthy dogs (58 eyes using Schirmer tear test (STT strip and microcapillary tubes. The samples were frozen at -80ºC and analyzed by the Bradford method. Results were analyzed by Student's t test. The average protein concentration and standard deviation from tears collected with microcapillary tube were 4.45mg/mL ±0.35 and 4,52mg/mL ±0.29 for right and left eyes respectively. The average protein concentration and standard deviation from tears collected with Schirmer Tear Test (STT strip were and 54.5mg/mL ±0.63 and 54.15mg/mL ±0.65 to right and left eyes respectively. Statistically significant differences (p<0.001 were found between the methods. In the conditions in which this study was conducted, the average protein concentration obtained with the Bradford test from tear samples obtained by Schirmer Tear Test (STT strip showed values higher than those obtained with microcapillary tube. It is important that concentration of tear protein pattern values should be analyzed according the method used to collect tear samples.

  3. Structured Extended Finite Element Methods of Solids Defined by Implicit Surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Belytschko, T; Mish, K; Moes, N; Parimi, C

    2002-11-17

    A paradigm is developed for generating structured finite element models from solid models by means of implicit surface definitions. The implicit surfaces are defined by radial basis functions. Internal features, such as material interfaces, sliding interfaces and cracks are treated by enrichment techniques developed in the extended finite element method (X-FEM). Methods for integrating the weak form for such models are proposed. These methods simplify the generation of finite element models. Results presented for several examples show that the accuracy of this method is comparable to standard unstructured finite element methods.

  4. Solid 4He and the diffusion Monte Carlo method: A study of their properties

    Science.gov (United States)

    Rugeles, E. J.; Ujevic, Sebastian; Vitiello, S. A.

    2017-10-01

    Properties of helium atoms in the solid phase are investigated using the multiweight diffusion Monte Carlo method. Two different importance function transformations are used in two series of independent calculations. The kinetic energy is estimated for both the solid and liquid phases of 4He. We estimate the melting and freezing densities, among other properties of interest. Our estimates are compared with experimental values. We discuss why walkers biased by two distinctly different guiding functions do not lead to noticeable changes in the reported results. Criticisms concerning the bias introduced into our estimates by population control and system size effects are considered.

  5. 2nd International Conference on Multiscale Computational Methods for Solids and Fluids

    CERN Document Server

    2016-01-01

    This volume contains the best papers presented at the 2nd ECCOMAS International Conference on Multiscale Computations for Solids and Fluids, held June 10-12, 2015. Topics dealt with include multiscale strategy for efficient development of scientific software for large-scale computations, coupled probability-nonlinear-mechanics problems and solution methods, and modern mathematical and computational setting for multi-phase flows and fluid-structure interaction. The papers consist of contributions by six experts who taught short courses prior to the conference, along with several selected articles from other participants dealing with complementary issues, covering both solid mechanics and applied mathematics. .

  6. Mutation Yield of a 34-Gene Solid Tumor Panel in Community-Based Tumor Samples.

    Science.gov (United States)

    Sanders, Heather; Qu, Kevin; Li, Hairong; Ma, Lin; Barlan, Cindy; Zhang, Xi; Prentice, James; Wolfson, David; Crossley, Beryl; Sferruzza, Anthony; Sninsky, John; Ross, David; Grupe, Andrew; Catanese, Joseph; Hantash, Feras; Waldman, Frederic

    2016-06-01

    Several targeted therapies have been approved for treatment of solid tumors. Identification of gene mutations that indicate response to these therapies is rapidly progressing. A 34-gene next-generation sequencing (NGS) panel, developed and validated by us, was evaluated to detect additional mutations in community-based cancer specimens initially sent to our reference laboratory for routine molecular testing. Consecutive de-identified clinical specimens (n = 121) from melanoma cases (n = 31), lung cancer cases (n = 27), colorectal cancer cases (n = 33), and breast cancer cases (n = 30) were profiled by NGS, and the results were compared with routine molecular testing. Upon initial mutation testing, 20 % (24/121) were positive. NGS detected ≥1 additional mutation not identified by routine testing in 74 % of specimens (90/121). Of the specimens with additional mutations, 16 harbored mutations in National Comprehensive Cancer Network guideline genes. These various additional mutations were in gene regions not routinely covered, in genes not routinely tested, and/or present at low allele frequencies. Moreover, NGS yielded no false negatives. Overall, NGS detected mutations in 59 % of the genes (20/34) included in the panel, 75 % of which (15/20) were detected in multiple tumor types. Mutations in TP53 were found in 51 % of tumors tested (62/121). Mutations in at least one other (non-TP53) gene present in the panel were detected in 64 % of cases (77/121). This assay provides improved breadth and sensitivity for profiling clinically relevant genes in these prevalent solid tumor types.

  7. Quantitative analysis of an oligomeric hindered amine light stabilizer in polypropylene by matrix-assisted laser desorption/ionization mass spectrometry using a solid sampling technique.

    Science.gov (United States)

    Taguchi, Yoshihiko; Ishida, Yasuyuki; Matsubara, Hideki; Ohtani, Hajime

    2006-01-01

    A small amount of an oligomeric hindered amine light stabilizer (HALS) (Adekastab LA-68LD) in polypropylene (PP) materials was directly determined by solid sampling matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) using an internal standard method. First the matrix reagent (dithranol), 20 mg, and the empirically selected internal standard, angiotensin I (MW = 1296.5), 5 microg, were premixed in the solid state. The matrix mixture was then co-ground with the PP sample containing the HALS in liquid nitrogen using a freezer mill. The powdered sample mixture was spotted on the sample plate, suspended in ion-exchanged water, dried to adhere on the plate, and subjected to MALDI-MS. Three series of the HALS components accompanied by the oxidized species were clearly observed as their molecular ions (M*+)) along with that of the internal standard in the mass spectra. A fairly good linear relationship (R2 = 0.9991) with a relative standard deviation of ca. 11% was observed between the relative peak intensities of the HALS components and the HALS contents ranging from 0.1-2.5 wt%, which could be used as the calibration line to determine the HALS content in PP composites directly by MALDI-MS. The UV-exposed PP composite samples were evaluated by this method to interpret the photostabilizing action of HALS in the PP materials based on the observed change in the relative abundances of the original and oxidized HALS components as a function of UV-exposure time. Copyright 2006 John Wiley & Sons, Ltd.

  8. Development of a functionalized polymeric ionic liquid monolith for solid-phase microextraction of polar endocrine disrupting chemicals in aqueous samples coupled to high-performance liquid chromatography.

    Science.gov (United States)

    Feng, Juanjuan; Sun, Min; Bu, Yanan; Luo, Chuannan

    2015-09-01

    Ionic liquids (ILs) have been efficiently used as a "designer sorbent" in sample preparation. A novel 1-(3-aminopropyl)-3-(4-vinylbenzyl)imidazolium 4-styrenesulfonate IL monomer was synthesized and copolymerized with 1,6-di(3-vinylimidazolium) hexane bishexafluorophosphate IL as cross-linking agent to prepare a cross-linked polymeric ionic liquids (PILs) monolith. Coupled to high-performance liquid chromatography (HPLC), the PILs monolith was used as a solid-phase microextraction (SPME) sorbent to extract some polar endocrine disrupting chemical (EDCs) such as estrogens, bisphenol A, and phthalate esters in aqueous samples. Preparation and extraction conditions were investigated and optimized to obtain satisfactory extraction efficiency. Limits of detection (LODs) of the proposed method for three steroid estrogens and bisphenol A were 0.25 and 0.2 μg L(-1), respectively, which were lower than or comparable to some other sample preparation methods. Intra- and inter-day repeatability for all the analytes was 2.2-12%. The monolith-to-monolith repeatability was 7.4-15%. The extraction performance of the method for analysis of target estrogens in treated domestic wastewater was investigated and compared with a dispersive liquid-liquid microextraction (DLLME) method. The proposed SPME method provided better sensitivity and higher resistance to matrix interferences.

  9. Polypyrrole nanowire as an excellent solid phase microextraction fiber for bisphenol A analysis in food samples followed by ion mobility spectrometry.

    Science.gov (United States)

    Kamalabadi, Mahdie; Mohammadi, Abdorreza; Alizadeh, Naader

    2016-08-15

    A polypyrrole nanowire coated fiber was prepared and used in head-space solid phase microextraction coupled with ion mobility spectrometry (HS-SPME-IMS) to the analysis of bisphenol A (BPA) in canned food samples, for the first time. This fiber was synthesized by electrochemical oxidation of the monomer in aqueous solution. The fiber characterization by scanning electron microscopy (SEM) revealed that the new fiber exhibited two-dimensional structures with a nanowire morphology. The effects of important extraction parameters on the efficiency of HS-SPME were investigated and optimized. Under the optimum conditions, the linearity of 10-150ngg(-1) and limit of detection (based on S/N=3) of 1ngg(-1) were obtained in BPA analysis. The repeatability (n=5) expressed as the relative standard deviation (RSD%) was 5.8%. At the end, the proposed method was successfully applied to determine BPA in various canned food samples (peas, corns, beans). Relative recoveries were obtained 93-96%. Method validation was conducted by comparing our results with those obtained through HPLC with fluorescence detection (FLD). Compatible results indicate that the proposed method can be successfully used in BPA analysis. This method is simple and cheaper than chromatographic methods, with no need of extra organic solvent consumption and derivatization prior to sample introduction. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Aqueous ammonium nitrate blasting composition containing solid carbonaceous fuel and method of preparing same

    Energy Technology Data Exchange (ETDEWEB)

    Sheeran, H.W.; Oriard, M.H.

    1969-06-17

    A blasting agent utilizes ammonium nitrate fuel and water to form a desired plasticity. The compound is detonatable because it employs fuel which is water stable either chemically or physically or both and remains in intimate association with the ammonium nitrate in the presence of water whether in the solid phase or liquid phase. The total oxygen balance of ammonium nitrate and fuel is adjusted by the formula proportions to be within detonatable limits. The method for making the blasting agent utilizes heat to liquefy a normally solid fuel while mixing with porous prilled ammonium nitrate to effect adsorption and absorption of the fuel by the ammonium nitrate. This effects intimate association in the solid phase and liberates only that portion of fuel into the liquid phase which corresponds to the quantity of ammonium nitrate which is dissolved by the added water. (19 claims)

  11. Method to resolve microphone and sample location errors in the two-microphone duct measurement method

    Science.gov (United States)

    Katz

    2000-11-01

    Utilizing the two-microphone impedance tube method, the normal incidence acoustic absorption and acoustic impedance can be measured for a given sample. This method relies on the measured transfer function between two microphones, and the knowledge of their precise location relative to each other and the sample material. In this article, a method is proposed to accurately determine these locations. A third sensor is added at the end of the tube to simplify the measurement. First, a justification and investigation of the method is presented. Second, reference terminations are measured to evaluate the accuracy of the apparatus. Finally, comparisons are made between the new method and current methods for determining these distances and the variations are discussed. From this, conclusions are drawn with regards to the applicability and need for the new method and under which circumstances it is applicable. Results show that the method provides a reliable determination of both microphone locations, which is not possible using the current techniques. Errors due to inaccurate determinination of these parameters between methods were on the order of 3% for R and 12% for Re Z.

  12. Design of indirect solid-phase immunosorbent methods for detecting arenavirus antigens and antibodies

    Energy Technology Data Exchange (ETDEWEB)

    Ivanov, A.P.; Rezapkin, G.V.; Dzagurova, T.K.; Tkachenko, E.A.

    1984-05-01

    Specifications have been elaborated for formulating indirect solid-phase enzyme-linked immunosorbent assay (ELISA) and radioimmunoassay (SPRIA) methods that employ anti-human and anti-mice G class immunoglobulin (IgG), conjugated with horseradish peroxidase and /sup 125/I for detecting the arenaviruses Junin, Machupo, Tacaribe, Amalpari, Tamiami, Lassa, and LCM (lymphocytic choriomeningitis). These methods make it possible to identify with a high degree of sensitivity arenavirus antigens and antibodies in various kinds of material.

  13. an assessment of methods for sampling carabid beetles

    African Journals Online (AJOL)

    Mgina

    Moist leaf litter was scooped onto white clothing (1 square metre beating sheet) and carabid beetles caught using a “pootah” (aspirator) or a pair of forceps. Resting beetles were sampled by manual searching under logs, stones and tree barks. Sampling effort was measured by time, each "sample" containing carabid.

  14. Interatomic force microscope and sample observing method therefor

    OpenAIRE

    YAMANAKA, K; Kolosov, Oleg; Ogiso, H; Sato, H.; Koda, T

    1994-01-01

    PURPOSE:To provide a measuring technology for interatomic microscope in which the irregular sample can be separated well from the frictional force. SOLUTION :An oscillating force applied laterally relatively between a sample 8 and a probe 4 Is provided. The sample 8 tilted laterally to excite bending orthogonal oscillation. The phase and the amplitude of the oscillation of the cantilever are detected.

  15. 19 CFR 151.70 - Method of sampling by Customs.

    Science.gov (United States)

    2010-04-01

    ... THE TREASURY (CONTINUED) EXAMINATION, SAMPLING, AND TESTING OF MERCHANDISE Wool and Hair § 151.70... feasible to obtain a representative general sample of the wool or hair in a sampling unit or to test such a... clean yield if such a test is requested in accordance with the provisions of § 151.71(c), or if a second...

  16. Synthesis and Evaluation of a Molecularly Imprinted Polymer for Selective Solid-Phase Extraction of Irinotecan from Human Serum Samples

    Directory of Open Access Journals (Sweden)

    Isabelle Lefebvre-Tournier

    2012-02-01

    Full Text Available A molecularly imprinted polymer (MIP was synthesized by non-covalent imprinting polymerization using irinotecan as template. Methacrylic acid and 4-vinylpyridine were selected as functional monomers. An optimized procedure coupled to LC-PDA analysis was developed for the selective solid-phase extraction of irinotecan from various organic media. A specific capacity of 0.65 µmol•g−1 for the MIP was determined. The high specificity of this MIP was demonstrated by studying the retention behaviour of two related compounds, camptothecin and SN-38. This support was applied for the extraction of irinotecan from human serum samples.

  17. Validity and reliability of the Experience-Sampling Method.

    Science.gov (United States)

    Csikszentmihalyi, M; Larson, R

    1987-09-01

    To understand the dynamics of mental health, it is essential to develop measures for the frequency and the patterning of mental processes in every-day-life situations. The Experience-Sampling Method (ESM) is an attempt to provide a valid instrument to describe variations in self-reports of mental processes. It can be used to obtain empirical data on the following types of variables: a) frequency and patterning of daily activity, social interaction, and changes in location; b) frequency, intensity, and patterning of psychological states, i.e., emotional, cognitive, and conative dimensions of experience; c) frequency and patterning of thoughts, including quality and intensity of thought disturbance. The article reviews practical and methodological issues of the ESM and presents evidence for its short- and long-term reliability when used as an instrument for assessing the variables outlined above. It also presents evidence for validity by showing correlation between ESM measures on the one hand and physiological measures, one-time psychological tests, and behavioral indices on the other. A number of studies with normal and clinical populations that have used the ESM are reviewed to demonstrate the range of issues to which the technique can be usefully applied.

  18. Direct solid sample analysis with graphite furnace atomic absorption spectrometry—a fast and reliable screening procedure for the determination of inorganic arsenic in fish and seafood.

    Science.gov (United States)

    Zmozinski, Ariane V; Llorente-Mirandes, Toni; Damin, Isabel C F; López-Sánchez, José F; Vale, Maria Goreti R; Welz, Bernhard; Silva, Márcia M

    2015-03-01

    Direct solid sample analysis with graphite furnace atomic absorption spectrometry (SS-GF AAS) was investigated initially with the intention of developing a method for the determination of total As in fish and other seafood. A mixture of 0.1% Pd+0.06% Mg+0.06% Triton X-100 was used as the chemical modifier, added in solution over the solid samples, making possible the use of pyrolysis and atomization temperatures of 1200 °C and 2400 °C, respectively. The sample mass had to be limited to 0.25 mg, as the integrated absorbance did not increase further with increasing sample mass. Nevertheless, the recovery of As from several certified reference materials was of the order of 50% lower than the certified value. Strong molecular absorption due to the phosphorus monoxide molecule (PO) was observed with high-resolution continuum source AAS (HR CS AAS), which, however, did not cause any spectral interference. A microwave-assisted digestion with HNO3/H2O2 was also investigated to solve the problem; however, the results obtained for several certified reference materials were statistically not different from those found with direct SS-GF AAS. Accurate values were obtained using inductively coupled plasma mass spectrometry (ICP-MS) to analyze the digested samples, which suggested that organic As compounds are responsible for the low recoveries. HPLC-ICP-MS was used to determine the arsenobetaine (AB) concentration. Accurate results that were not different from the certified values were obtained when the AB concentration was added to the As concentration found by SS-GF AAS for most certified reference materials (CRM) and samples, suggesting that SS-GF AAS could be used as a fast screening procedure for inorganic As determination in fish and seafood. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Heating and temperature gradients of lipid bilayer samples induced by RF irradiation in MAS solid-state NMR experiments.

    Science.gov (United States)

    Wang, Jing; Zhang, Zhengfeng; Zhao, Weijing; Wang, Liying; Yang, Jun

    2016-05-09

    The MAS solid-state NMR has been a powerful technique for studying membrane proteins within the native-like lipid bilayer environment. In general, RF irradiation in MAS NMR experiments can heat and potentially destroy expensive membrane protein samples. However, under practical MAS NMR experimental conditions, detailed characterization of RF heating effect of lipid bilayer samples is still lacking. Herein, using (1) H chemical shift of water for temperature calibration, we systematically study the dependence of RF heating on hydration levels and salt concentrations of three lipids in MAS NMR experiments. Under practical (1) H decoupling conditions used in biological MAS NMR experiments, three lipids show different dependence of RF heating on hydration levels as well as salt concentrations, which are closely associated with the properties of lipids. The maximum temperature elevation of about 10 °C is similar for the three lipids containing 200% hydration, which is much lower than that in static solid-state NMR experiments. The RF heating due to salt is observed to be less than that due to hydration, with a maximum temperature elevation of less than 4 °C in the hydrated samples containing 120 mmol l(-1) of salt. Upon RF irradiation, the temperature gradient across the sample is observed to be greatly increased up to 20 °C, as demonstrated by the remarkable broadening of (1) H signal of water. Based on detailed characterization of RF heating effect, we demonstrate that RF heating and temperature gradient can be significantly reduced by decreasing the hydration levels of lipid bilayer samples from 200% to 30%. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  20. One-step synthesis of magnetic graphene oxide nanocomposite and its application in magnetic solid phase extraction of heavy metal ions from biological samples.

    Science.gov (United States)

    Sun, Jieping; Liang, Qionglin; Han, Qiang; Zhang, Xiaoqiong; Ding, Mingyu

    2015-01-01

    A novel magnetic graphene oxide nanocomposite was synthesized by one-step coprecipitation method and characterized by transmission electron microscopy, X-ray photoelectron spectroscopy and vibrating sample magnetometer. The nanocomposite beard many intriguing properties, including chemical stability, high adsorption capacity, and superparamagnetic. These properties evoked great interest and desire of its exploration in magnetic solid-phase extraction of heavy metal ions from complex samples. Several parameters effecting the analytical performance, such as the sample pH, amounts of adsorbent, sample volumes, elution volumes, and coexisting ions, had been investigated in detail. The adsorbed metal ions were easy eluted by controlling the pH condition and the materials could be reused more than 20 times. Under the optimized conditions, the limits of detection were 0.016, 0.046, 0.395, 0.038, 0.157 μg L(-1) for Co(2+), Ni(2+), Cu(2+), Cd(2+), and Pb(2+), respectively. The intra-day relative standard deviations (n=5) were in the range of 1.8-5.5% at 10 μg L(-1). The proposed method was successfully applied to biological sample analysis and got excellent recoveries in the range of 81-113% even the matrix was complex. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. An Invariant-Preserving ALE Method for Solids under Extreme Conditions

    Energy Technology Data Exchange (ETDEWEB)

    Sambasivan, Shiv Kumar [Los Alamos National Laboratory; Christon, Mark A [Los Alamos National Laboratory

    2012-07-17

    We are proposing a fundamentally new approach to ALE methods for solids undergoing large deformation due to extreme loading conditions. Our approach is based on a physically-motivated and mathematically rigorous construction of the underlying Lagrangian method, vector/tensor reconstruction, remapping, and interface reconstruction. It is transformational because it deviates dramatically from traditionally accepted ALE methods and provides the following set of unique attributes: (1) a three-dimensional, finite volume, cell-centered ALE framework with advanced hypo-/hyper-elasto-plastic constitutive theories for solids; (2) a new physically and mathematically consistent reconstruction method for vector/tensor fields; (3) advanced invariant-preserving remapping algorithm for vector/tensor quantities; (4) moment-of-fluid (MoF) interface reconstruction technique for multi-material problems with solids undergoing large deformations. This work brings together many new concepts, that in combination with emergent cell-centered Lagrangian hydrodynamics methods will produce a cutting-edge ALE capability and define a new state-of-the-art. Many ideas in this work are new, completely unexplored, and hence high risk. The proposed research and the resulting algorithms will be of immediate use in Eulerian, Lagrangian and ALE codes under the ASC program at the lab. In addition, the research on invariant preserving reconstruction/remap of tensor quantities is of direct interest to ongoing CASL and climate modeling efforts at LANL. The application space impacted by this work includes Inertial Confinement Fusion (ICF), Z-pinch, munition-target interactions, geological impact dynamics, shock processing of powders and shaped charges. The ALE framework will also provide a suitable test-bed for rapid development and assessment of hypo-/hyper-elasto-plastic constitutive theories. Today, there are no invariant-preserving ALE algorithms for treating solids with large deformations. Therefore

  2. Monolithic molecularly imprinted solid-phase extraction for the selective determination of trace cytokinins in plant samples with liquid chromatography-electrospray tandem mass spectrometry.

    Science.gov (United States)

    Du, Fuyou; Ruan, Guihua; Liang, Shenghua; Xie, Fuwei; Liu, Huwei

    2012-08-01

    Cytokinins (CTKs) are a class of growth-regulating hormones involved in various physiological and developmental processes. More novel analytical methods for the accurate identification and quantitative determination of trace CTKs in plants have been desired to better elucidate the roles of CTKs. In this work, a novel method based on monolithic molecularly imprinted solid-phase extraction followed by liquid chromatography-electrospray tandem mass spectrometry (mMI-SPE-LC-MS/MS) was developed for accurate determination of four CTKs in plant samples. The molecularly imprinted polymer monolith was prepared by using kinetin as the template in syringes and exhibited specific recognition ability for the four CTKs in comparison with that of non-imprinted polymer monolith. Several factors affecting the extraction performance of mMI-SPE, including the pH of loading sample solution, the nature and volume of elution solvent, the flow rate of sample loading, and sample volume, were investigated, respectively. Under the optimized conditions, the proposed mMI-SPE-LC-MS/MS method was successfully applied in the selective extraction and determination of four CTKs in plant tissues, and it offers detection limits (S/N = 3) of 104, 113, 130, and 89 pg/mL and mean recoveries of 85.9%, 79.3%, 73.5%, and 70.1% for kinetin, kinetin glucoside, trans-zeatin, and meta-topolin (mT), respectively, with the corresponding RSDs less than 15%.

  3. Simultaneous quantification of Aroclor mixtures in soil samples by gas chromatography/mass spectrometry with solid phase microextraction using partial least-squares regression.

    Science.gov (United States)

    Zhang, Mengliang; Harrington, Peter de B

    2015-01-01

    Multivariate partial least-squares (PLS) method was applied to the quantification of two complex polychlorinated biphenyls (PCBs) commercial mixtures, Aroclor 1254 and 1260, in a soil matrix. PCBs in soil samples were extracted by headspace solid phase microextraction (SPME) and determined by gas chromatography/mass spectrometry (GC/MS). Decachlorinated biphenyl (deca-CB) was used as internal standard. After the baseline correction was applied, four data representations including extracted ion chromatograms (EIC) for Aroclor 1254, EIC for Aroclor 1260, EIC for both Aroclors and two-way data sets were constructed for PLS-1 and PLS-2 calibrations and evaluated with respect to quantitative prediction accuracy. The PLS model was optimized with respect to the number of latent variables using cross validation of the calibration data set. The validation of the method was performed with certified soil samples and real field soil samples and the predicted concentrations for both Aroclors using EIC data sets agreed with the certified values. The linear range of the method was from 10μgkg(-1) to 1000μgkg(-1) for both Aroclor 1254 and 1260 in soil matrices and the detection limit was 4μgkg(-1) for Aroclor 1254 and 6μgkg(-1) for Aroclor 1260. This holistic approach for the determination of mixtures of complex samples has broad application to environmental forensics and modeling. Copyright © 2014 Elsevier Ltd. All rights reserved.

  4. Determination of Iodate in Food, Environmental, and Biological Samples after Solid-Phase Extraction with Ni-Al-Zr Ternary Layered Double Hydroxide as a Nanosorbent

    Directory of Open Access Journals (Sweden)

    Hossein Abdolmohammad-Zadeh

    2012-01-01

    Full Text Available Nanostructured nickel-aluminum-zirconium ternary layered double hydroxide was successfully applied as a solid-phase extraction sorbent for the separation and pre-concentration of trace levels of iodate in food, environmental and biological samples. An indirect method was used for monitoring of the extracted iodate ions. The method is based on the reaction of the iodate with iodide in acidic solution to produce iodine, which can be spectrophotometrically monitored at 352 nm. The absorbance is directly proportional to the concentration of iodate in the sample. The effect of several parameters such as pH, sample flow rate, amount of nanosorbent, elution conditions, sample volume, and coexisting ions on the recovery was investigated. In the optimum experimental conditions, the limit of detection (3s and enrichment factor were 0.12 μg mL−1 and 20, respectively. The calibration graph using the preconcentration system was linear in the range of 0.2–2.8 μg mL−1 with a correlation coefficient of 0.998. In order to validate the presented method, a certified reference material, NIST SRM 1549, was also analyzed.

  5. Surfactant-enhanced spectrofluorimetric determination of total aflatoxins from wheat samples after magnetic solid-phase extraction using modified Fe3O4 nanoparticles

    Science.gov (United States)

    Manafi, Mohammad Hanif; Allahyari, Mehdi; Pourghazi, Kamyar; Amoli-Diva, Mitra; Taherimaslak, Zohreh

    2015-07-01

    The extraction and preconcentration of total aflatoxins (including aflatoxin B1, B2, G1, and G2) using magnetic nanoparticles based solid phase extraction (MSPE) followed by surfactant-enhanced spectrofluorimetric detection was proposed. Ethylene glycol bis-mercaptoacetate modified silica coated Fe3O4 nanoparticles as an efficient antibody-free adsorbent was successfully applied to extract aflatoxins from wheat samples. High surface area and strong magnetization properties of magnetic nanoparticles were utilized to achieve high enrichment factor (97), and satisfactory recoveries (92-105%) using only 100 mg of the adsorbent. Furthermore, the fast separation time (less than 10 min) avoids many time-consuming cartridge loading or column-passing procedures accompany with the conventional SPE. In determination step, signal enhancement was performed by formation of Triton X-100 micelles around the analytes in 15% (v/v) acetonitrile-water which dramatically increase the sensitivity of the method. Main factors affecting the extraction efficiency and signal enhancement of the analytes including pH of sample solution, desorption conditions, extraction time, sample volume, adsorbent amount, surfactant concentration and volume and time of micelle formation were evaluated and optimized. Under the optimum conditions, wide linear range of 0.1-50 ng mL-1 with low detection limit of 0.03 ng mL-1 were obtained. The developed method was successfully applied to the extraction and preconcentration of aflatoxins in three commercially available wheat samples and the results were compared with the official AOAC method.

  6. Exploration of structure and function in biomolecules through solid-state NMR and computational methods

    Science.gov (United States)

    Heider, Elizabeth M.

    Solid-State Nuclear Magnetic Resonance (SSNMR) spectroscopy and quantum mechanical calculations are powerful analysis tools. Leveraged independently, each method yields important nuclear and molecular information. Used in concert, SSNMR and computational techniques provide complementary data about the structure of solids. These methods are particularly useful in characterizing the structures of microcrystalline organic compounds and revealing mechanisms of biological activity. Such applications may possess special relevance in analysis of pharmaceutical products; 90% of all pharmaceuticals are marketed as solids and bioactivity is strongly linked with molecular conformation. Accordingly, this dissertation employs both SSNMR and quantum mechanical computation to study three bioactive molecules: citrinin, two forms of Atrasentan (Abt-627), and paclitaxel (Taxol RTM). First, a computational study is utilized to determine the mechanism for unusual antioxidant activity in citrinin. Here, molecular geometries and bond dissociation enthalpies (BDE) of the citrinin O--H groups are calculated from first principles (ab initio). The total molecular Hamiltonian is determined by approximating the individual contributors to energy including electronic energy and contributions from modes of molecular vibration. This study of citrinin clearly identifies specific reaction sites in the active form, establishing the central role of intramolecular hydrogen bonding in this activity. Notably, it is discovered that citrinin itself is not the active species. Instead, a pair of hydrated Michael addition products of citrinin act as radical scavengers via O--H bond dissociation. Next, two separate compounds of the anticancer drug Abt-627 (form I and form II) are examined via SSNMR. The three principal values of the 13C diagonalized chemical shift tensor are acquired through the high resolution 2D experiment, FIREMAT. Isotropic chemical shift assignments are made utilizing both dipolar

  7. Sub-microanalysis of solid samples with near-field enhanced atomic emission spectroscopy

    Science.gov (United States)

    Wang, Xiaohua; Liang, Zhisen; Meng, Yifan; Wang, Tongtong; Hang, Wei; Huang, Benli

    2018-03-01

    A novel approach, which we have chosen to name it as near-field enhanced atomic emission spectroscopy (NFE-AES), was proposed by introducing a scanning tunnelling microscope (STM) system into a laser-induced breakdown spectrometry (LIBS). The near-field enhancement of a laser-illuminated tip was utilized to improve the lateral resolution tremendously. Using the hybrid arrangement, pure metal tablets were analyzed to verify the performance of NFE-AES both in atmosphere and in vacuum. Due to localized surface plasmon resonance (LSPR), the incident electromagnetic field is enhanced and confined at the apex of tip, resulting in sub-micron scale ablation and elemental emission signal. We discovered that the signal-to-noise ratio (SNR) and the spectral resolution obtained in vacuum condition are better than those acquired in atmospheric condition. The quantitative capability of NFE-AES was demonstrated by analyzing Al and Pb in Cu matrix, respectively. Submicron-sized ablation craters were achieved by performing NFE-AES on a Si wafer with an Al film, and the spectroscopic information from a crater of 650 nm diameter was successfully obtained. Due to its advantage of high lateral resolution, NFE-AES imaging of micro-patterned Al lines on an integrated circuit of a SIM card was demonstrated with a sub-micron lateral resolution. These results reveal the potential of the NFE-AES technique in sub-microanalysis of solids, opening an opportunity to map chemical composition at sub-micron scale.

  8. Stirring-controlled solidified floating solid-liquid drop microextraction as a new solid phase-enhanced liquid-phase microextraction method by exploiting magnetic carbon nanotube-nickel hybrid.

    Science.gov (United States)

    Ghazaghi, Mehri; Mousavi, Hassan Zavvar; Shirkhanloo, Hamid; Rashidi, Alimorad

    2017-01-25

    A specific technique is introduced to overcome limitations of classical solidification of floating organic drop microextraction, such as tedious and time-consuming centrifuge step and using disperser solvent, by facile and efficient participation of solid and liquid phases. In this proposed method of stirring-controlled sol