Hollow fiber liquid phase microextraction combined with graphite furnace atomic absorption spectrometry for the determination of methylmercury in human hair and sludge samples

Energy Technology Data Exchange (ETDEWEB)

Jiang Hongmei [Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin [Department of Chemistry, Wuhan University, Wuhan 430072 (China)], E-mail: binhu@whu.edu.cn; Chen Beibei; Zu Wanqing [Department of Chemistry, Wuhan University, Wuhan 430072 (China)

2008-07-15

Two methods, based on hollow fiber liquid-liquid-liquid (three phase) microextraction (HF-LLLME) and hollow fiber liquid phase (two phase) microextraction (HF-LPME), have been developed and critically compared for the determination of methylmercury content in human hair and sludge by graphite furnace atomic absorption spectrometry (GFAAS). In HF-LPME, methylmercury was extracted into the organic phase (toluene) prior to its determination by GFAAS, while inorganic mercury remained as a free species in the sample solution. In HF-LLLME, methylmercury was first extracted into the organic phase (toluene) and then into the acceptor phase (4% thiourea in 1 mol L{sup -1} HCl) prior to its determination by GFAAS, while inorganic mercury remained in the sample solution. The total mercury was determined by inductively coupled plasma-mass spectrometry (ICP-MS), and the levels of inorganic mercury in both HF-LLLME and HF-LPME were obtained by subtracting methylmercury from total mercury. The factors affecting the microextraction of methylmercury, including organic solvent, extraction time, stirring rate and ionic strength, were investigated and the optimal extraction conditions were established for both HF-LLLPME and HF-LPME. With a consumption of 3.0 mL of the sample solution, the enrichment factors were 204 and 55 for HF-LLLPME and HF-LPME, respectively. The limits of detection (LODs) for methylmercury were 0.1 {mu}g L{sup -1} and 0.4 {mu}g L{sup -1} (as Hg) with precisions (RSDs (%), c = 5 {mu}g L{sup -1} (as Hg), n = 5) of 13% and 11% for HF-LLLPME-GFAAS and HF-LPME-GFAAS, respectively. For ICP-MS determination of total mercury, a limit of detection of 39 ng L{sup -} {sup 1} was obtained. Finally, HF-LLLME-GFAAS was applied to the determination of methylmercury content in human hair and sludge, and the recoveries for the spiked samples were in the range of 99-113%. In order to validate the method, HF-LLLME-GFAAS was also applied to the analysis of a certified reference

Magnetic solid-phase extraction combined with graphite furnace atomic absorption spectrometry for speciation of Cr(III) and Cr(VI) in environmental waters.

Science.gov (United States)

Jiang, Hong-mei; Yang, Ting; Wang, Yan-hong; Lian, Hong-zhen; Hu, Xin

2013-11-15

A new approach of magnetic solid phase extraction (MSPE) coupled with graphite furnace atomic absorption spectrometry (GFAAS) has been developed for the speciation of Cr(III) and Cr(VI) using zincon-immobilized silica-coated magnetic Fe3O4 nanoparticles (Zincon-Si-MNPs) as the MSPE absorbent. Cr(III) was quantitatively reserved on the absorbent at pH 9.1 while total Cr was reserved at pH 6.5. The absorbed Cr species were eluted by using 2 mol/L HCl and detected by GFAAS. The concentration of Cr(VI) could be calculated by subtracting Cr(III) from total Cr. All the parameters affecting the separation and extraction efficiency of Cr species such as pH, extraction time, concentration and volume of eluent, sample volume and influence of co-existing ions were systematically examined and the optimized conditions were established accordingly. The detection limit (LOD) of the method was 0.016 and 0.011 ng mL(-1) for Cr(III) and Cr(VI), respectively, with the enrichment factor of 100 and 150. The precisions of this method (Relative standard deviation, RSD, n=7) for Cr(III) and Cr(VI) at 0.1 ng mL(-1) were 6.0% and 6.2%, respectively. In order to validate the proposed method, a certified reference material of environmental water was analyzed, and the result of Cr speciation was in good agreement with the certified value. This MSPE-GFAAS method has been successfully applied for the speciation of Cr(III) and Cr(VI) in lake and tap waters with the recoveries of 88-109% for the spiked samples. Moreover, the MSPE separation mechanism of Cr(III) and Cr(VI) based on their adsorption-desorption on Zincon-Si-MNPs has been explained through various spectroscopic characterization. © 2013 Elsevier B.V. All rights reserved.

Laser solid sampling for a solid-state-detector ICP emission spectrometer

International Nuclear Information System (INIS)

Noelte, J.; Moenke-Blankenburg, L.; Schumann, T.

1994-01-01

Solid sampling with laser vaporization has been coupled to an ICP emission spectrometer with an Echelle optical system and a solid-state-detector for the analysis of steel and soil samples. Pulsation of the vaporized material flow was compensated by real-time background correction and internal standardization, resulting in good accuracy and precision. (orig.)

Atomization of Cd in U+Zr matrix after chemical separation using GF-AAS

International Nuclear Information System (INIS)

Thulasidas, S.K.; Gupta, Santosh Kumar; Natarajan, V.

2014-01-01

Studies on the direct atomization of Cd in U+Zr matrix were carried out and the effect of matrix composition and matrix concentration on the analyte absorbance were investigated. Development of a method using graphite furnace atomic absorption spectrometry (GF-AAS) for determination of Cd is required for FBR fuel (U+20%Zr) materials. It was reported that the absorbance signal for Cd is reduced with matrix, 50% at 20 mg/mL of U and 10 mg/mL of Zr matrix as compared to matrix free solution. To use the method for U+Zr mixed oxide samples, effect of varying composition of Zr in U+Zr mixed matrix was studied. The results indicated that Cd absorbance signal remained unaffected in the range 0-40% Zr in (U+Zr) mixed matrix with 20 mg/mL total matrix. Based on these studies, an analytical method was developed for the direct determination of Cd with 20% Zr in 20 mg/mL of U+Zr solution with optimized experimental parameters. The range of analysis was found to be 0.005-0.1 g/mL for Cd with 20 mg/mL matrix; this leads to detection limits of 0.25 ppm. To meet the specification limits at 0.1 ppm level for Cd, it was necessary to separate the matrix from the sample using solvent extraction method. It was reported that with 30%TBP+70%CCl 4 in 7M HNO 3 , a selective simultaneous extraction of U and Zr into the organic phase can be achieved. In the present studies, same extraction procedure was used with 100 mg U+Zr sample. The effect of U+Zr in raffinate on Cd was also estimated. To validate the method, the extracted aqueous samples were also analyzed by ICP-AES SPECTRO ARCOS SOP technique independently and the results were compared. It was seen that Cd estimation was not affected in the presence of 10-50 μg/mL U+Zr by ICP-AES as well

Determination of arsenic in ambient water at sub-part-per-trillion levels by hydride generation Pd coated platform collection and GFAAS detection.

Science.gov (United States)

Liang, L; Lazoff, S; Chan, C; Horvat, M; Woods, J S

1998-11-01

A method for trace determination of total arsenic in ambient waters is described. Arsenic is separated on-line from a large volume water sample by hydride generation and purging, pre-collected on a Pd coated pyrolytic platform cuvette using a simple and inexpensive system, and finally detected by GFAAS. Instrument parameters, hydride generation, transportation, and collection were optimized. The analytical behavior for major species including As(3+), As(5+), monomethyl As (MMA), and dimethyl As (DMA) were investigated individually. Problems arising from use of the system were discussed and eliminated. The necessity of sample digestion and an efficient digestion method were studied. Sample digestion for water with low organic content such as tap water and clean ground water and some clean surface water can be omitted. The method detection limit (MDL) is 0.3 ng l(-1) for a 25 ml water sample. Recoveries close to 100% with R.S.D.rain, sewage effluent, and saline water from different origins in the US, China, and Canada were collected and analyzed using ultra clean sampling and analysis techniques. The background levels of As in most water analyzed were established for the first time, and found to be far above the EPA's health effect criteria, 18 ng l(-1).

Study of the Analytical Conditions for the Determination of Cadmium in Coal Fly Ashes by GFAAS with evaluation of several matrix modifiers

International Nuclear Information System (INIS)

Rucandio, M.I.; Petit, M.D.

1998-01-01

A new method for the determination of cadmium in coal fly ash samples by Graphite Furnace Atomic Absorption Spectrometry (GFAAS) has been developed. Analytical conditions and different instrumental parameters have been optimized. In a first step, several types of matrix modifiers have been tested and a mixture of 2% NH 4 H 2 PO 4 with 0.4%Mg(NO 3 ) 2 in 0.5N HNO 3 has been selected, since it provides the highest sensitivity. In a second step, an optimization of several conditions, using the selected modifier, has been carried out, such as ashing and atomization temperatures, heating rate, etc. The influence of the use of a L' vov platform on the analytical and background signals has been studied, showing a significative decrease on the background signal, being the net absorbance similar to those obtained in absence of the platform. Using the optimal conditions, the direct method with standard samples provides cadmium concentration consistent with those obtained using the standard addition method. (Author) 18 refs

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.

Applications of liquid-phase microextraction in the sample preparation of environmental solid samples.

Science.gov (United States)

Prosen, Helena

2014-05-23

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.

Comparison of different sample preparation methods for platinum determination in cultured cells by graphite furnace atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Man Xiao

2017-01-01

Full Text Available Background Platinum-based agents are widely used in chemotherapy against solid tumors and insufficient intracellular drug accumulation is one of the leading causes of platinum resistance which is associated with poor survival of tumor patients. Thus, the detection of intracellular platinum is pivotal for studies aiming to overcome platinum resistance. In the present study, we aimed to establish a reliable graphite furnace atomic absorption spectrometry (GFAAS-based assay to quantify the intracellular platinum content for cultured cells. Methods Several most commonly applied cell preparation methods, including 0.2% HNO3, 0.2% Triton X-100, concentrated nitric acid, RIPA combined with concentrated nitric acid and hydroxide, followed by GFAAS for platinum detection were compared in ovarian, cervical and liver cancer cell lines to obtain the optimal one, and parameters regarding linearity, accuracy, precision and sensitivity were evaluated. Influence of other metals on platinum detection and the storage conditions of samples were also determined. Results The treatment of cells with 0.2% HNO3 was superior to other approaches with fewer platinum loss and better repeatability. The recovery rate and precision of this method were 97.3%–103.0% and 1.4%–3.8%, respectively. The average recoveries in the presence of other metals were 95.1%–103.1%. The detection limit was 13.23 ug/L. The recovery rate of platinum remained acceptable even in cell samples stored in −20 °C or −80 °C for two months. Discussion After comparison, we found that 0.2% HNO3 was optimal for intracellular platinum quantification based on GFAAS, which presented values compatible with that of inductively-coupled plasma mass-spectrometry (ICP-MS, and this is partially attributed to the simplicity of this method. Moreover, the assay was proved to be accurate, sensitive, cost-effective and suitable for the research of platinum-based antitumor therapy.

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

OpenAIRE

Helena Prosen

2014-01-01

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...

Determination of palladium, platinum and rhodium in used automobile catalysts and active pharmaceutical ingredients using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sample analysis

Energy Technology Data Exchange (ETDEWEB)

Resano, Martín, E-mail: mresano@unizar.es [Department of Analytical Chemistry, Aragón Institute of Engineering Research (I3A), University of Zaragoza, Pedro Cerbuna 12, 50009 Zaragoza (Spain); Flórez, María del Rosario [Department of Analytical Chemistry, Aragón Institute of Engineering Research (I3A), University of Zaragoza, Pedro Cerbuna 12, 50009 Zaragoza (Spain); Queralt, Ignasi [Institute of Earth Sciences Jaume Almera ICTJA-CSIC, Sole Sabarís s/n, 08028 Barcelona (Spain); Marguí, Eva [Department of Chemistry, Faculty of Sciences, Universitat de Girona, Campus Montilivi s/n, 17071 Girona (Spain)

2015-03-01

This work investigates the potential of high-resolution continuum source graphite furnace atomic absorption spectrometry for the direct determination of Pd, Pt and Rh in two samples of very different nature. While analysis of active pharmaceutical ingredients is straightforward and it is feasible to minimize matrix effects, to the point that calibration can be carried out against aqueous standard solutions, the analysis of used automobile catalysts is more challenging requiring the addition of a chemical modifier (NH{sub 4}F·HF) to help in releasing the analytes, a more vigorous temperature program and the use of a solid standard (CRM ERM®-EB504) for calibration. However, in both cases it was possible to obtain accurate results and precision values typically better than 10% RSD in a fast and simple way, while only two determinations are needed for the three analytes, since Pt and Rh can be simultaneously monitored in both types of samples. Overall, the methods proposed seem suited for the determination of these analytes in such types of samples, offering a greener and faster alternative that circumvents the traditional problems associated with sample digestion, requiring a small amount of sample only (0.05 mg per replicate for catalysts, and a few milligrams for the pharmaceuticals) and providing sufficient sensitivity to easily comply with regulations. The LODs achieved were 6.5 μg g{sup −1} (Pd), 8.3 μg g{sup −1} (Pt) and 9.3 μg g{sup −1} (Rh) for catalysts, which decreased to 0.08 μg g{sup −1} (Pd), 0.15 μg g{sup −1} (Pt) and 0.10 μg g{sup −1} (Rh) for pharmaceuticals. - Highlights: • Solid sampling HR CS GFAAS permits the fast and direct determination of Pd, Pt and Rh. • 2 determinations suffice for the 3 elements (2 of them can be measured simultaneously). • Samples as different as car catalysts and pharmaceuticals can be accurately analyzed. • Aqueous standards (pharmaceuticals) or a solid CRM (catalysts) is used for calibration. �

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.

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

Energy Technology Data Exchange (ETDEWEB)

NONE

2005-04-15

The bias introduced when sampling solid biofuels from stockpiles or containers instead of from moving streams is assessed as well as the number and size of samples required to represent accurately the bulk sample, variations introduced when reducing bulk samples into samples for testing, and the usefulness of sample reduction methods. Details are given of the experimental work carried out in Sweden and Denmark using sawdust, wood chips, wood pellets, forestry residues and straw. The production of a model European Standard for quality assurance of solid biofuels is examined.

Poly(1-vinylimidazole) functionalized magnetic ion imprinted polymer for fast and selective extraction of trace gold in geological, environmental and biological samples followed by graphite furnace atomic absorption spectrometry detection

Science.gov (United States)

Zhao, Bingshan; He, Man; Chen, Beibei; Xu, Hongrun; Hu, Bin

2018-05-01

In this study, poly(1-vinylimidazole) functionalized gold ion imprinted polymer coated magnetic nanoparticles (MNPs@PVIM-Au-IIP) were prepared and characterized. The adsorption behaviors of the prepared MNPs@PVIM-Au-IIP toward gold ions (Au(III)) were studied, it was found that MNPs@PVIM-Au-IIP has good selectivity, high adsorption capacity (185.4 mg g-1) and fast adsorption kinetic for Au(III). Based on it, a new method of ion imprinted magnetic solid phase extraction (II-MSPE) coupled with graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the analysis of trace Au(III) in real samples with complicated matrix. Factors affecting MSPE including sample pH, desorption reagent, elution concentration and volume, elution time, sample volume and adsorption time were optimized. With high enrichment factor of 100-fold, the detection limit of the proposed method is 7.9 ng L-1 for Au(III) with the relative standard deviation of 7.4% (c = 50 ng L-1, n = 7). In order to validate the accuracy of the proposed method, the Certified Reference Material of GBW07293 geological sample (platinpalladium ore) was analyzed, and the determined value was in good agreement with the certified value. The proposed II-MSPE-GFAAS method is simple, fast, selective, sensitive and has been successfully applied in the determination of trace Au in ore, sediment, environmental water and human urine samples with satisfactory results.

Paraffin scintillator for radioassay of solid support samples

International Nuclear Information System (INIS)

Fujii, Haruo; Takiue, Makoto

1989-01-01

A new paraffin scintillator used for solid support sample counting has been proposed, and its composition and various characteristics are described. The solid support sample treated with this scintillator can be easily handled because of rigid sample conditions. This technique provides great advantages such as the elimination of a large volume of scintillator and little radioactive waste material by using an economical polyethylene bag instead of the conventional counting vial. (author)

Novel ion imprinted magnetic mesoporous silica for selective magnetic solid phase extraction of trace Cd followed by graphite furnace atomic absorption spectrometry detection

Energy Technology Data Exchange (ETDEWEB)

Zhao, Bingshan; He, Man; Chen, Beibei; Hu, Bin, E-mail: binhu@whu.edu.cn

2015-05-01

Determination of trace Cd in environmental, biological and food samples is of great significance to toxicological research and environmental pollution monitoring. While the direct determination of Cd in real-world samples is difficult due to its low concentration and the complex matrix. Herein, a novel Cd(II)-ion imprinted magnetic mesoporous silica (Cd(II)-II-MMS) was prepared and was employed as a selective magnetic solid-phase extraction (MSPE) material for extraction of trace Cd in real-world samples followed by graphite furnace atomic absorption spectrometry (GFAAS) detection. Under the optimized conditions, the detection limit of the proposed method was 6.1 ng L{sup −1} for Cd with the relative standard deviation (RSD) of 4.0% (c = 50 ng L{sup −1}, n = 7), and the enrichment factor was 50-fold. To validate the proposed method, Certified Reference Materials of GSBZ 50009–88 environmental water, ZK018-1 lyophilized human urine and NIES10-b rice flour were analyzed and the determined values were in a good agreement with the certified values. The proposed method exhibited a robust anti-interference ability due to the good selectivity of Cd(II)-II-MMS toward Cd(II). It was successfully employed for the determination of trace Cd(II) in environmental water, human urine and rice samples with recoveries of 89.3–116%, demonstrating that the proposed method has good application potential in real world samples with complex matrix. - Highlights: • Novel Cd(II)-II-MMS was prepared by surface imprinting combined with a sol–gel process. • Cd(II)-II-MMS has a high selectivity and adsorption capacity for Cd(II). • A sensitive and selective method of Cd(II)-IIMSPE-GFAAS was developed for trace cadmium analysis. • The method can be applied to determine trace Cd in various samples with complicated matrix.

Novel ion imprinted magnetic mesoporous silica for selective magnetic solid phase extraction of trace Cd followed by graphite furnace atomic absorption spectrometry detection

International Nuclear Information System (INIS)

Zhao, Bingshan; He, Man; Chen, Beibei; Hu, Bin

2015-01-01

Determination of trace Cd in environmental, biological and food samples is of great significance to toxicological research and environmental pollution monitoring. While the direct determination of Cd in real-world samples is difficult due to its low concentration and the complex matrix. Herein, a novel Cd(II)-ion imprinted magnetic mesoporous silica (Cd(II)-II-MMS) was prepared and was employed as a selective magnetic solid-phase extraction (MSPE) material for extraction of trace Cd in real-world samples followed by graphite furnace atomic absorption spectrometry (GFAAS) detection. Under the optimized conditions, the detection limit of the proposed method was 6.1 ng L −1 for Cd with the relative standard deviation (RSD) of 4.0% (c = 50 ng L −1 , n = 7), and the enrichment factor was 50-fold. To validate the proposed method, Certified Reference Materials of GSBZ 50009–88 environmental water, ZK018-1 lyophilized human urine and NIES10-b rice flour were analyzed and the determined values were in a good agreement with the certified values. The proposed method exhibited a robust anti-interference ability due to the good selectivity of Cd(II)-II-MMS toward Cd(II). It was successfully employed for the determination of trace Cd(II) in environmental water, human urine and rice samples with recoveries of 89.3–116%, demonstrating that the proposed method has good application potential in real world samples with complex matrix. - Highlights: • Novel Cd(II)-II-MMS was prepared by surface imprinting combined with a sol–gel process. • Cd(II)-II-MMS has a high selectivity and adsorption capacity for Cd(II). • A sensitive and selective method of Cd(II)-IIMSPE-GFAAS was developed for trace cadmium analysis. • The method can be applied to determine trace Cd in various samples with complicated matrix

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 ...

[Detecting Thallium in Water Samples using Dispersive Liquid Phase Microextraction-Graphite Furnace Atomic Absorption Spectroscopy].

Science.gov (United States)

Zhu, Jing; Li, Yan; Zheng, Bo; Tang, Wei; Chen, Xiao; Zou, Xiao-li

2015-11-01

To develope a method of solvent demulsification dispersive liquid phase microextraction (SD-DLPME) based on ion association reaction coupled with graphite furnace atomic absorption spectroscopy (GFAAS) for detecting thallium in water samples. Methods Thallium ion in water samples was oxidized to Tl(III) with bromine water, which reacted with Cl- to form TlCl4-. The ionic associated compound with trioctylamine was obtained and extracted. DLPME was completed with ethanol as dispersive solvent. The separation of aqueous and organic phase was achieved by injecting into demulsification solvent without centrifugation. The extractant was collected and injected into GFAAS for analysis. With palladium colloid as matrix modifier, a two step drying and ashing temperature programming process was applied for high precision and sensitivity. The linear range was 0.05-2.0 microg/L, with a detection limit of 0.011 microg/L. The relative standard derivation (RSD) for detecting Tl in spiked water sample was 9.9%. The spiked recoveries of water samples ranged from 94.0% to 103.0%. The method is simple, sensitive and suitable for batch analysis of Tl in water samples.

Fast sampling calorimetry with solid argon ionization chambers

International Nuclear Information System (INIS)

Clark, E.; Linn, S.; Piekarz, H.; Wahl, H.; Womersley, J.; Hansen, S.; Hurh, P.; Rivetta, C.; Sanders, R.; Schmitt, R.; Stanek, R.; Stefanik, A.

1992-01-01

A proposal for the fast sampling calorimetry with solid argon as active medium and the preliminary results from the solid argon test cell are presented. The proposed test calorimeter module structure, the signal routing and the mechanical and cryogenic arrangements are also discussed

Spin imaging in solids using synchronously rotating field gradients and samples

International Nuclear Information System (INIS)

Wind, R.A.; Yannoni, C.S.

1983-01-01

A method for spin-imaging in solids using nuclear magnetic resonance (NMR) spectroscopy is described. With this method, the spin density distribution of a two- or three-dimensional object such as a solid can be constructed resulting in an image of the sample. This method lends itself to computer control to map out an image of the object. This spin-imaging method involves the steps of placing a solid sample in the rf coil field and the external magnetic field of an NMR spectrometer. A magnetic field gradient is superimposed across the sample to provide a field gradient which results in a varying DC field that has different values over different parts of the sample. As a result, nuclei in different parts of the sample have different resonant NMR frequencies. The sample is rotated about an axis which makes a particular angle of 54.7 degrees with the static external magnetic field. The magnetic field gradient which has a spatial distribution related to the sample spinning axis is then rotated synchronously with the sample. Data is then collected while performing a solid state NMR line narrowing procedure. The next step is to change the phase relation between the sample rotation and the field gradient rotation. The data is again collected as before while the sample and field gradient are synchronously rotated. The phase relation is changed a number of times and data collected each time. The spin image of the solid sample is then reconstructed from the collected data

Direct determination of Cd and Pb in human urine by GFAAS with deuterium-lamp background correction using different chemical modifiers

International Nuclear Information System (INIS)

Husakova, L.; Baoinova, M.; Sramkova, J.; Cernohorsky, T.

2007-01-01

Several authors have contributed to the elaboration of methodology for direct determination of Cd and Pb in urine by graphite furnace atomic absorption spectrometry (GFAAS). In the proposed approaches, Zeeman background correction systems were predominantly used, without paying much attention to the selection of an appropriate chemical modifier. However, systematic studies on eleven recommended and less commonly used modifiers have resulted in optimization of atomization conditions, so that accurate analysis also with the use of D 2 -lamp background correction became possible. This was confirmed by comparative measurements using both background correction systems. For determination of Cd in urine, NH 4 F has been selected resulting in the lowest limit of detection (LOD): 0.07 μg L -1 . NH 4 F promotes efficient atomization at low temperatures and suppresses chloride interference effect. Pd + Sr (nitrate) has been selected as the most adequate modifier for determination of Pb. Its presence raised the maximum tolerable pyrolysis temperature up to 1200 o C, which resulted in the maximum reduction of the background signal and the lowest LOD of 1.5 mg L -1 for Pb (10 μL aliquots of dispensed urine). Applying the above modifiers to the analysis of standards and samples, direct aqueous calibration for accurate analysis of diluted and acidified urine samples became possible. Accuracy of the analysis was verified by the use of commercially available quality control reference materials. (authors)

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

Graphene oxide-TiO2 composite solid phase extraction combined with graphite furnace atomic absorption spectrometry for the speciation of inorganic selenium in water samples.

Science.gov (United States)

Zhang, Yanan; Chen, Beibei; Wu, Shaowei; He, Man; Hu, Bin

2016-07-01

In this paper, a method of graphene oxide (GO)-TiO2 composite solid phase extraction followed by graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the speciation of inorganic selenium in environmental waters. The adsorption behavior of inorganic Se(IV) and Se(VI) on the GO-TiO2(1:1) composite was investigated. It was found that Se(IV) was quantitatively retained on the GO-TiO2 composites within a wide pH range of 0.5-10, while Se(VI) was quantitatively adsorbed on GO-TiO2(1:1) composite at pH 0.5-2, and no obvious adsorption of Se(VI) within the pH range of 4-10 was found. By selecting pH 6.0, Se(IV) could be easily determined. After reduction of Se(VI), total Se was determined by the proposed method, and Se(VI) was calculated as the difference between the total Se and Se(IV). The factors affecting the separation/preconcentration of Se(IV) and Se(VI) were studied. Under the optimum conditions, the isothermal adsorption of Se(IV) on the GO-TiO2(1:1) composite fitted Langmuir model; a linear range over 0.1-12ngmL(-1) was obtained. The limit of detection (LOD) and precision of the method for Se(IV) was 0.04ngmL(-1) and 9.4% (cSe(IV)=0.5ngmL(-1), n=7), respectively. In order to verify the accuracy of the method, a standard water sample (GSBZ50031-94) was analyzed, and the determined value was in a good agreement to the certified value. The established method was applied to inorganic Se speciation in environmental water samples and the recovery of 87.4-102% was obtained for the spiked samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Cobalt internal standard for Ni to assist the simultaneous determination of Mo and Ni in plant materials by high-resolution continuum source graphite furnace atomic absorption spectrometry employing direct solid sample analysis.

Science.gov (United States)

de Babos, Diego Victor; Bechlin, Marcos André; Barros, Ariane Isis; Ferreira, Edilene Cristina; Gomes Neto, José Anchieta; de Oliveira, Silvana Ruella

2016-05-15

A new method is proposed for the simultaneous determination of Mo and Ni in plant materials by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS), employing direct solid sample analysis (DSS) and internal standardization (IS). Cobalt was used as internal standard to minimize matrix effects during Ni determinations, enabling the use of aqueous standards for calibration. Correlation coefficients for the calibration curves were typically better than 0.9937. The performance of the method was checked by analysis of six plant certified reference materials, and the results for Mo and Ni were in agreement with the certified values (95% confidence level, t-test). Analysis was made of different types of plant materials used as renewable sources of energy, including sugarcane leaves, banana tree fiber, soybean straw, coffee pods, orange bagasse, peanut hulls, and sugarcane bagasse. The concentrations found for Mo and Ni ranged from 0.08 to 0.63 ng mg(-1) and from 0.41 to 6.92 ng mg(-1), respectively. Precision (RSD) varied from 2.1% to 11% for Mo and from 3.7% to 10% for Ni. Limits of quantification of 0.055 and 0.074 ng were obtained for Mo and Ni, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of gold and cobalt dopants in advanced materials based on tin oxide by slurry sampling high-resolution continuum source graphite furnace atomic absorption spectrometry

Science.gov (United States)

Filatova, Daria G.; Eskina, Vasilina V.; Baranovskaya, Vasilisa B.; Vladimirova, Svetlana A.; Gaskov, Alexander M.; Rumyantseva, Marina N.; Karpov, Yuri A.

2018-02-01

A novel approach is developed for the determination of Co and Au dopants in advanced materials based on tin oxide using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS) with direct slurry sampling. Sodium carboxylmethylcellulose (Na-CMC) is an effective stabilizer for diluted suspensions. Use Na-CMC allows to transfer the analytes into graphite furnace completely and reproducibly. The relative standard deviation obtained by HR CS GFAAS was not higher than 4%. Accuracy was proven by means inductively coupled plasma mass spectrometry (ICP-MS) in solutions after decomposition as a comparative technique. To determine Au and Co in the volume of SnO2, the acid decomposition conditions (HCl, HF) of the samples were suggested by means of an autoclave in a microwave oven.

Solid state characterization of commercial crystalline and amorphous atorvastatin calcium samples.

Science.gov (United States)

Shete, Ganesh; Puri, Vibha; Kumar, Lokesh; Bansal, Arvind K

2010-06-01

Atorvastatin calcium (ATC), an anti-lipid BCS class II drug, is marketed in crystalline and amorphous solid forms. The objective of this study was to perform solid state characterization of commercial crystalline and amorphous ATC drug samples available in the Indian market. Six samples each of crystalline and amorphous ATC were characterized using X-ray powder diffractometry (XRPD), differential scanning calorimetry (DSC), thermogravimetric analysis, Karl Fisher titrimetry, microscopy (hot stage microscopy, scanning electron microscopy), contact angle, and intrinsic dissolution rate (IDR). All crystalline ATC samples were found to be stable form I, however one sample possessed polymorphic impurity, evidenced in XRPD and DSC analysis. Amongst the amorphous ATC samples, XRPD demonstrated five samples to be amorphous 'form 27', while, one matched amorphous 'form 23'. Thermal behavior of amorphous ATC samples was compared to amorphous ATC generated by melt quenching in DSC. ATC was found to be an excellent glass former with T(g)/T(m) of 0.95. Residual crystallinity was detected in two of the amorphous samples by complementary use of conventional and modulated DSC techniques. The wettability and IDR of all amorphous samples was found to be higher than the crystalline samples. In conclusion, commercial ATC samples exhibited diverse solid state behavior that can impact the performance and stability of the dosage forms.

Selective extraction of chromium(VI) using a leaching procedure with sodium carbonate from some plant leaves, soil and sediment samples

Energy Technology Data Exchange (ETDEWEB)

Elci, Latif, E-mail: elci@pamukkale.edu.tr [Department of Chemistry, Pamukkale University, 20017 Denizli (Turkey); Divrikli, Umit; Akdogan, Abdullah; Hol, Aysen; Cetin, Ayse [Department of Chemistry, Pamukkale University, 20017 Denizli (Turkey); Soylak, Mustafa [Department of Chemistry, Erciyes University, 38039 Kayseri (Turkey)

2010-01-15

Speciation of chromium in some plant leaves, soil and sediment samples was carried out by selective leaching of Cr(VI) using a sodium carbonate leaching procedure. Total chromium from the samples was extracted using aqua regia and oxidative acid digestion, respectively. The concentrations of chromium species in the extracts were determined using by graphite furnace atomic absorption spectrometry (GFAAS). Uncoated graphite furnace tubes were used as an atomizer. Due to the presence of relatively high amounts of Na{sub 2}CO{sub 3} in the resulting samples, the possible influences of Na{sub 2}CO{sub 3} on the absorbance signals were checked. There is no interference of Na{sub 2}CO{sub 3} on the chromium absorbance up to 0.1 mol L{sup -1} Na{sub 2}CO{sub 3}. A limit of detection (LOD) for determination of Cr(VI) in 0.1 Na{sub 2}CO{sub 3} solution by GFAAS was found to be 0.93 {mu}g L{sup -1}. The procedure was applied to environmental samples. The relative standard deviation, R.S.D. as precision for 10 replicate measurements of 20 {mu} L{sup -1} Cr in processed soil sample was 4.2%.

Selective extraction of chromium(VI) using a leaching procedure with sodium carbonate from some plant leaves, soil and sediment samples.

Science.gov (United States)

Elci, Latif; Divrikli, Umit; Akdogan, Abdullah; Hol, Aysen; Cetin, Ayse; Soylak, Mustafa

2010-01-15

Speciation of chromium in some plant leaves, soil and sediment samples was carried out by selective leaching of Cr(VI) using a sodium carbonate leaching procedure. Total chromium from the samples was extracted using aqua regia and oxidative acid digestion, respectively. The concentrations of chromium species in the extracts were determined using by graphite furnace atomic absorption spectrometry (GFAAS). Uncoated graphite furnace tubes were used as an atomizer. Due to the presence of relatively high amounts of Na(2)CO(3) in the resulting samples, the possible influences of Na(2)CO(3) on the absorbance signals were checked. There is no interference of Na(2)CO(3) on the chromium absorbance up to 0.1 mol L(-1) Na(2)CO(3). A limit of detection (LOD) for determination of Cr(VI) in 0.1 Na(2)CO(3) solution by GFAAS was found to be 0.93 microg L(-1). The procedure was applied to environmental samples. The relative standard deviation, R.S.D. as precision for 10 replicate measurements of 20 microL(-1) Cr in processed soil sample was 4.2%.

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

Solid State Characterization of Commercial Crystalline and Amorphous Atorvastatin Calcium Samples

OpenAIRE

Shete, Ganesh; Puri, Vibha; Kumar, Lokesh; Bansal, Arvind K.

2010-01-01

Atorvastatin calcium (ATC), an anti-lipid BCS class II drug, is marketed in crystalline and amorphous solid forms. The objective of this study was to perform solid state characterization of commercial crystalline and amorphous ATC drug samples available in the Indian market. Six samples each of crystalline and amorphous ATC were characterized using X-ray powder diffractometry (XRPD), differential scanning calorimetry (DSC), thermogravimetric analysis, Karl Fisher titrimetry, microscopy (hot s...

Determination of trace elements in paints by direct sampling graphite furnace atomic absorption spectrometry

International Nuclear Information System (INIS)

Bentlin, Fabrina R.S.; Pozebon, Dirce; Mello, Paola A.; Flores, Erico M.M.

2007-01-01

A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO 3 ) 2 was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 μg g -1 of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES)

An approach for sampling solid heterogeneous waste at the Hanford Site waste receiving and processing and solid waste projects

International Nuclear Information System (INIS)

Sexton, R.A.

1993-03-01

This paper addresses the problem of obtaining meaningful data from samples of solid heterogeneous waste while maintaining sample rates as low as practical. The Waste Receiving and Processing Facility, Module 1, at the Hanford Site in south-central Washington State will process mostly heterogeneous solid wastes. The presence of hazardous materials is documented for some packages and unknown for others. Waste characterization is needed to segregate the waste, meet waste acceptance and shipping requirements, and meet facility permitting requirements. Sampling and analysis are expensive, and no amount of sampling will produce absolute certainty of waste contents. A sampling strategy is proposed that provides acceptable confidence with achievable sampling rates

Determination of diphenylarsinic acid, phenylarsonic acid and inorganic arsenic in drinking water by graphite-furnace atomic-absorption spectrometry after simultaneous separation and preconcentration with solid-phase extraction disks.

Science.gov (United States)

Hagiwara, Kenta; Inui, Tetsuo; Koike, Yuya; Nakamura, Toshihiro

2013-01-01

A simple method of graphite-furnace atomic-absorption spectrometry (GFAAS) after solid-phase extraction (SPE) was developed for the determination of diphenylarsinic acid (DPAA), phenylarsonic acid (PAA), and inorganic arsenic (iAs) in drinking water. This method involves the simultaneous collection of DPAA, PAA, and iAs using three stacked SPE disks, i.e., an Empore SDB-XD disk (the upper layer), an activated carbon disk (the middle layer), and a Cation-SR disk loaded with Zr and Ca (ZrCa-CED; the lower layer). A 200-mL aqueous sample was adjusted to pH 3 with nitric acid and passed through the SPE disks at a flow rate of 15 mL min(-1), to concentrate DPAA on the SDB-XD disk, PAA on the activated carbon disk, and iAs on the ZrCa-CED. The As compounds were eluted from the disks with 10 mL of ethanol containing 0.5 mol L(-1) ammonia solution for DPAA, 20 mL of 1 mol L(-1) ammonia solution for PAA, and 20 mL of 6 mol L(-1) hydrochloric acid for iAs. The eluates of DPAA, PAA, and iAs were diluted to 20, 25, and 25 mL, respectively, with deionized water, and then analyzed by GFAAS. The detection limits of As (three-times the standard deviation (n = 3) of the blank values) were 0.13 and 0.16 μg L(-1) at enrichment factors of 10 and 8, respectively, using a 200-mL water sample. Spike tests with 2 μg (10 μg L(-1)) of DPAA, PAA, and iAs in 200 mL of tap water and bottled drinking water showed good recoveries (96.1-103.8%).

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

International Nuclear Information System (INIS)

Ely, T. M.; LaMothe, M. E.; Lachut, J. S.

2016-01-01

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.

Determination of trace elements in paints by direct sampling graphite furnace atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Bentlin, Fabrina R.S. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil); Pozebon, Dirce [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil)], E-mail: dircepoz@iq.ufrgs.br; Mello, Paola A.; Flores, Erico M.M. [Departamento de Quimica, Universidade Federal de Santa Maria, UFSM, 97105-900 Santa Maria, RS (Brazil)

2007-10-17

A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO{sub 3}){sub 2} was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 {mu}g g{sup -1} of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES)

Determination of bismuth and cadmium after solid-phase extraction with chromosorb-107 in a syringe

International Nuclear Information System (INIS)

Tokman, Nilgun; Akman, Suleyman

2004-01-01

The determination of bismuth and cadmium by graphite furnace atomic absorption spectrometry (GFAAS) after solid-phase extraction (SPE) on Chromosorb-107 filled in a syringe was described. To retain the analytes, the sample solution treated with and without ammonium pyrolidine dithiocarbamate (APDC) was drawn into the syringe filled with Chromosorb-107 and discharged back manually. Bismuth and cadmium were quantitatively sorbed at pH ≥ 6 irrespective of whether the analyte was complexed with APDC prior to passing through the Chromosorb-107. Analyte elements sorbed on the resin were quantitatively eluted with 3.0 M of HNO 3 again drawing and discharging the eluent into the syringe and ejected it back. Optimum flow rates of sample or eluent for sorption and elution processes were 20 ml min -1 for drawing and 20 ml min -1 for discharging in all cases. Bismuth and cadmium were analyzed by graphite furnace atomic absorption spectrometry. The elements could be concentrated by drawing and discharging several portions of sample successively but eluting only one time. The validity of the proposed method was checked with standard reference materials (NIST SRM 1515 Apple-Leaves, CWW-TM-E Waste Water and CRM-SW Sea Water). The analyte elements were quantitatively (>95%) recovered from different matrices irrespective of treated samples with APDC. Detection limits (δ) were 0.8 and 1.2 μg l -1 for Bi and Cd, respectively. The method can be characterized with fastness, simplicity, quantitative recovery and high reproducibility

Solid Phase Characterization Of Heel Samples From Tank 241-C-110

International Nuclear Information System (INIS)

Page, J.S.; Cooke, G.A.; Pestovich, J.A.; Huber, H.J.

2011-01-01

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 μm and a finer fraction of < 710 μm. These two fractions were analyzed separately. The coarser

Fast acquisition of multidimensional NMR spectra of solids and mesophases using alternative sampling methods.

Science.gov (United States)

Lesot, Philippe; Kazimierczuk, Krzysztof; Trébosc, Julien; Amoureux, Jean-Paul; Lafon, Olivier

2015-11-01

Unique information about the atom-level structure and dynamics of solids and mesophases can be obtained by the use of multidimensional nuclear magnetic resonance (NMR) experiments. Nevertheless, the acquisition of these experiments often requires long acquisition times. We review here alternative sampling methods, which have been proposed to circumvent this issue in the case of solids and mesophases. Compared to the spectra of solutions, those of solids and mesophases present some specificities because they usually display lower signal-to-noise ratios, non-Lorentzian line shapes, lower spectral resolutions and wider spectral widths. We highlight herein the advantages and limitations of these alternative sampling methods. A first route to accelerate the acquisition time of multidimensional NMR spectra consists in the use of sparse sampling schemes, such as truncated, radial or random sampling ones. These sparsely sampled datasets are generally processed by reconstruction methods differing from the Discrete Fourier Transform (DFT). A host of non-DFT methods have been applied for solids and mesophases, including the G-matrix Fourier transform, the linear least-square procedures, the covariance transform, the maximum entropy and the compressed sensing. A second class of alternative sampling consists in departing from the Jeener paradigm for multidimensional NMR experiments. These non-Jeener methods include Hadamard spectroscopy as well as spatial or orientational encoding of the evolution frequencies. The increasing number of high field NMR magnets and the development of techniques to enhance NMR sensitivity will contribute to widen the use of these alternative sampling methods for the study of solids and mesophases in the coming years. Copyright © 2015 John Wiley & Sons, Ltd.

Metalloproteomics Approach to Analyze Mercury in Breast Milk and Hair Samples of Lactating Women in Communities of the Amazon Basin, Brazil.

Science.gov (United States)

Cerbino, M R; Vieira, José Cavalcante Souza; Braga, C P; Oliveira, G; Padilha, I F; Silva, T M; Zara, L F; Silva, N J; Padilha, P M

2018-02-01

Mercury is a potentially toxic element that is present in the environment of the Brazilian Amazon and is responsible for adverse health effects in humans. This study sought to assess possible protein biomarkers of mercury exposure in breast milk samples from lactating women in the Madeira and Negro Rivers in the Brazilian Amazon. The mercury content of hair samples of lactating women was determined, and the proteome of breast milk samples was obtained using two-dimensional electrophoresis after protein precipitation with acetone. Mercury measurements of protein spots obtained via protein fractionation were performed by graphite furnace atomic absorption spectrometry (GFAAS), and it was observed that mercury is linked to proteins with molecular masses in the range of 14-26 kDa. The total mercury concentration was also determined by GFAAS in unprocessed milk, lyophilized milk, and protein pellets, with the purpose of determining the mercury mass balance in relation to the concentration of this element in milk and pellets. Approximately 85 to 97% of mercury present in the lyophilized milk from samples of lactating women of the Madeira River is bound in the protein fraction. From lactating women of the Negro River, approximately 49% of the total mercury is bound in the protein fraction, and a difference of 51% is bound in the lipid fraction.

Modified emission-transmission method for determining trace elements in solid samples using the XRF techniques

International Nuclear Information System (INIS)

Poblete, V.; Alvarez, M.; Hermosilla, M.

2000-01-01

This is a study of an analysis of trace elements in medium thick solid samples, by the modified transmission emission method, using the energy dispersion X-ray fluorescence technique (EDXRF). The effects of absorption and reinforcement are the main disadvantages of the EDXRF technique for the quantitative analysis of bigger elements and trace elements in solid samples. The implementation of this method and its application to a variety of samples was carried out using an infinitely thick multi-element white sample that calculates the correction factors by absorbing all the analytes in the sample. The discontinuities in the masic absorption coefficients versus energies association for each element, with medium thick and homogenous samples, are analyzed and corrected. A thorough analysis of the different theoretical and test variables are proven by using real samples, including certified material with known concentration. The simplicity of the calculation method and the results obtained show the method's major precision, with possibilities for the non-destructive routine analysis of different solid samples, using the EDXRF technique (author)

Solid Sampling with a Diode Laser for Portable Ambient Mass Spectrometry.

Science.gov (United States)

Yung, Yeni P; Wickramasinghe, Raveendra; Vaikkinen, Anu; Kauppila, Tiina J; Veryovkin, Igor V; Hanley, Luke

2017-07-18

A hand-held diode laser is implemented for solid sampling in portable ambient mass spectrometry (MS). Specifically, a pseudocontinuous wave battery-powered surgical laser diode is employed for portable laser diode thermal desorption (LDTD) at 940 nm and compared with nanosecond pulsed laser ablation at 2940 nm. Postionization is achieved in both cases using atmospheric pressure photoionization (APPI). The laser ablation atmospheric pressure photoionization (LAAPPI) and LDTD-APPI mass spectra of sage leaves (Salvia officinalis) using a field-deployable quadrupole ion trap MS display many similar ion peaks, as do the mass spectra of membrane grown biofilms of Pseudomonas aeruginosa. These results indicate that LDTD-APPI method should be useful for in-field sampling of plant and microbial communities, for example, by portable ambient MS. The feasibility of many portable MS applications is facilitated by the availability of relatively low cost, portable, battery-powered diode lasers. LDTD could also be coupled with plasma- or electrospray-based ionization for the analysis of a variety of solid samples.

Air sampling with solid phase microextraction

Science.gov (United States)

Martos, Perry Anthony

There is an increasing need for simple yet accurate air sampling methods. The acceptance of new air sampling methods requires compatibility with conventional chromatographic equipment, and the new methods have to be environmentally friendly, simple to use, yet with equal, or better, detection limits, accuracy and precision than standard methods. Solid phase microextraction (SPME) satisfies the conditions for new air sampling methods. Analyte detection limits, accuracy and precision of analysis with SPME are typically better than with any conventional air sampling methods. Yet, air sampling with SPME requires no pumps, solvents, is re-usable, extremely simple to use, is completely compatible with current chromatographic equipment, and requires a small capital investment. The first SPME fiber coating used in this study was poly(dimethylsiloxane) (PDMS), a hydrophobic liquid film, to sample a large range of airborne hydrocarbons such as benzene and octane. Quantification without an external calibration procedure is possible with this coating. Well understood are the physical and chemical properties of this coating, which are quite similar to those of the siloxane stationary phase used in capillary columns. The log of analyte distribution coefficients for PDMS are linearly related to chromatographic retention indices and to the inverse of temperature. Therefore, the actual chromatogram from the analysis of the PDMS air sampler will yield the calibration parameters which are used to quantify unknown airborne analyte concentrations (ppb v to ppm v range). The second fiber coating used in this study was PDMS/divinyl benzene (PDMS/DVB) onto which o-(2,3,4,5,6- pentafluorobenzyl) hydroxylamine (PFBHA) was adsorbed for the on-fiber derivatization of gaseous formaldehyde (ppb v range), with and without external calibration. The oxime formed from the reaction can be detected with conventional gas chromatographic detectors. Typical grab sampling times were as small as 5 seconds

Sample-size effects in fast-neutron gamma-ray production measurements: solid-cylinder samples

International Nuclear Information System (INIS)

Smith, D.L.

1975-09-01

The effects of geometry, absorption and multiple scattering in (n,Xγ) reaction measurements with solid-cylinder samples are investigated. Both analytical and Monte-Carlo methods are employed in the analysis. Geometric effects are shown to be relatively insignificant except in definition of the scattering angles. However, absorption and multiple-scattering effects are quite important; accurate microscopic differential cross sections can be extracted from experimental data only after a careful determination of corrections for these processes. The results of measurements performed using several natural iron samples (covering a wide range of sizes) confirm validity of the correction procedures described herein. It is concluded that these procedures are reliable whenever sufficiently accurate neutron and photon cross section and angular distribution information is available for the analysis. (13 figures, 5 tables) (auth)

Eosinophilia in routine blood samples as a biomarker for solid tumor development

DEFF Research Database (Denmark)

Andersen, Christen Bertel L; Siersma, V.D.; Hasselbalch, H.C.

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...... 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...... that additional preclinical studies are needed in order to shed further light on the role of eosinophils in carcinogenesis, where it is still unknown whether the cells contribute to tumor immune surveillance or neoplastic evolution....

Solid-phase extraction and determination of trace elements in environmental samples using naphthalene adsorbent

International Nuclear Information System (INIS)

Pourreza, N.

2004-01-01

Naphthalene co-precipitated with quaternary ammonium salt such as tetraoctyl ammonium bromide and methyltrioctyl ammonium chloride have been used as adsorbent for solid phase extraction of metal ions such as Hg, Cd and Fe. The metal ions are retained on the adsorbent in a column as their complexes with suitable ligands and eluted by an eluent before instrumental measurements. The optimization of the procedures for solid phase extraction and consequent determination of trace elements and application to environmental samples especially water samples will be discussed. (author)

Metal-organic framework based in-syringe solid-phase extraction for the on-site sampling of polycyclic aromatic hydrocarbons from environmental water samples.

Science.gov (United States)

Zhang, Xiaoqiong; Wang, Peiyi; Han, Qiang; Li, Hengzhen; Wang, Tong; Ding, Mingyu

2018-04-01

In-syringe solid-phase extraction is a promising sample pretreatment method for the on-site sampling of water samples because of its outstanding advantages of portability, simple operation, short extraction time, and low cost. In this work, a novel in-syringe solid-phase extraction device using metal-organic frameworks as the adsorbent was fabricated for the on-site sampling of polycyclic aromatic hydrocarbons from environmental waters. Trace polycyclic aromatic hydrocarbons were effectively extracted through the self-made device followed by gas chromatography with mass spectrometry analysis. Owing to the excellent adsorption performance of metal-organic frameworks, the analytes could be completely adsorbed during one adsorption cycle, thus effectively shortening the extraction time. Moreover, the adsorbed analytes could remain stable on the device for at least 7 days, revealing the potential of the self-made device for on-site sampling of degradable compounds in remote regions. The limit of detection ranged from 0.20 to 1.9 ng/L under the optimum conditions. Satisfactory recoveries varying from 84.4 to 104.5% and relative standard deviations below 9.7% were obtained in real samples analysis. The results of this study promote the application of metal-organic frameworks in sample preparation and demonstrate the great potential of in-syringe solid-phase extraction for the on-site sampling of trace contaminants in environmental waters. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Sampling of solid particles in clouds

International Nuclear Information System (INIS)

Feuillebois, F.; Lasek, A.; Scibilia, M.F.

1986-01-01

This paper is concerned with the sampling of small solid particles from clouds by an airborne apparatus to be mounted on an airplane for meteorological investigations. In the airborne experiment the particles entering the test tube should be as representative as possible of the upstream conditions ahead of the plane, in the real cloud. Due to the inertia of the particles, the proportion of the different sizes of particles entering the test tube depends on the location of the tube mouth. We present a method of calculating the real concentration in particles of different sizes, using the results of measurements executed during the flight of an airplane in a cloud. Two geometries are considered: the nose of the airplane, represented schematically by a hemisphere, and a wing represented by a (2D) Joukowski profile which matches well a NACA 0015 profile on its leading edge

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

Science.gov (United States)

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

2018-04-01

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 toward 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. 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. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Air-assisted Liquid Liquid Microextraction Combined with Graphite Furnace Atomic Absorption Spectrometry for Preconcentration and Determination of Trace Amount of Co(II and Ni(II Ions in Water Samples

Directory of Open Access Journals (Sweden)

Saeed Mohammad Sorouraddin

2017-12-01

Full Text Available A simple, rapid and efficient method has been developed for the extraction, preconcentration and determination of cobalt (II and nickel (II ions in water samples by air-assisted liquid-liquid microextraction (AALLME coupled with graphite furnace atomic absorption spectrometry (GFAAS. In the proposed method, much less volume of an organic solvent was used as the extraction solvent in the absence of disperser solvent. Fine organic droplets were formed by sucking and injecting of the mixture of aqueous sample solution and extraction solvent with a syringe for several times in a conical test tube. After extraction, phase separation was performed by centrifugation and the enriched analytes in the sedimented phase were determined by GFAAS. Several variables that could affect the extraction efficiency were investigated and optimized. Calibration graphs were linear in the range of 6.5-100 ng L-1. Detection limits for Co and Ni were 2.3 ng L-1 and 3 ng L-1, respectively. The accuracy of the developed procedure was checked by analyzing NRCC-SLRS4 Riverine water as a certified reference material. Finally, the proposed method has been successfully applied for the determination of cobalt (II and nickel (II ions in tap, surface and river water samples.

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

Selective sampling and measurement of Cr (VI) in water with polyquaternary ammonium salt as a binding agent in diffusive gradients in thin-films technique.

Science.gov (United States)

Chen, Hong; Zhang, Yang-Yang; Zhong, Ke-Li; Guo, Lian-Wen; Gu, Jia-Li; Bo, Le; Zhang, Meng-Han; Li, Jian-Rong

2014-04-30

A diffusive gradients in thin films (DGT) device with polyquaternary ammonium salt (PQAS) as a novel binding agent (PQAS DGT) combined with graphite furnace atomic absorption spectrometry (GFAAS) was developed for the selective sampling and measurement of Cr (VI) in water. The performance of PQAS DGT was independent of pH 3-12 and ionic strength from 1 × 10(-3) to 1 molL(-1). DGT validation experiments showed that Cr (VI) was measured accurately as well as selectively by PQAS DGT, whereas Cr (III) was not determined quantitatively. Compared with diphenylcarbazide spectrophotometric method (DPC), the measurement of Cr (VI) with PQAS DGT was agreement with that of DPC method in the industrial wastewater. PQAS-DGT device had been successfully deployed in local freshwater. The concentrations of Cr (VI) determined by PQAS DGT coupled with GFAAS in Nuer River, Ling River and North Lake were 0.73 ± 0.09 μg L(-1), 0.50 ± 0.07 μg L(-1) and 0.61 ± 0.07 μg L(-1), respectively. The results indicate that PQAS DGT device can be used for the selective sampling and measurement Cr (VI) in water and its detection limit is lower than that of DPC method. Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of lead in whole blood: Comparison of the LeadCare blood lead testing system with zeeman longitudinal electrothermal atomic absorption spectrometry

International Nuclear Information System (INIS)

Pineau, A.; Viallefont, A.; Fauconneau, B.; Rafael, M.; Guillard, O.

2002-01-01

This study compares the efficiency of blood lead level analysis by graphite furnace atomic absorption spectrometry (GFAAS) and the portable LeadCare Blood lead testing system (LCS). Recoveries of two added lead concentrations of 22 and 42 μg/dL ranged from 102.4 to 105.5% for LCS and from 96.3 to 97.2% for GFAAS. Measurement of a certified sample (Certified Danish Whole Blood) at a blood lead concentration of 26.2 μg/dL gave within- and between-run coefficients of variation which were both approximately 8% by LCS and 2% by GFAAS. Comparison of the tested method (LCS) versus GFAAS from analysis of 76 samples of blood lead collected from workers in different industrial sectors showed imperfect overall correlation (r = 0.95). The LCS is quite suitable for screening purposes, but requires the use of non-frozen blood collected less than 24 h before. Conservative threshold values should be applied when using the LCS for initial screening in the field. (orig.)

Determination of tellurium in coal samples by means of graphite furnace atomic absorption spectrometry after coprecipitation with iron(III) hydroxide

Energy Technology Data Exchange (ETDEWEB)

Oda, S.; Arikawa, Y. [Japan Womens University, Tokyo (Japan)

2005-11-01

A simple and accurate method for the determination of tellurium in coal samples was investigated by the combustion of samples under a high pressure of oxygen and coprecipitation with Fe(OH){sub 3}, followed by a measurement by graphite furnace atomic absorption spectrometry (GF-AAS). About 0.5 g of an accurately weighed ground coal sample and 0.5 g of starch were combusted in an oxygen combustion bomb filled with oxygen to 3 MPa and added with 3 ml of water as an absorbing solution. The formed tellurium trioxide TeOs dissolved in water as TeO{sub 4}{sup 2-}, which was in turn reduced to TeO{sub 3}{sup 2-} by heating. After diluting the above-mentioned solution up to about 50 ml with water, Fe(OH){sub 3} is formed upon adding Fe(NO{sub 3}){sub 3} and sodium hydroxide solutions at pH 8-9 and left standing overnight. After dissolving the precipitate by HCl, the solution was diluted to 10 ml with water and the concentration of tellurium was measured by GF-AAS at a wavelength of 214.3 nm. The standard addition method was employed for the determination of tellurium in real coal samples, because those processes for the formation of tellurium(VI) oxide and coprecipitation with Fe(OH)3 were interfered by matrices. For NIST SRM 1632c, the standard coal sample tellurium content of 0.057 {+-} 0.004 mg kg{sup -1} was in good agreement with the information value of 0.05 mg kg{sup -1} with 7% of RSD in five replicate analyses. The tellurium contents in 20 real coal samples given by Center for Coal Utilization, Japan were also determined. The tellurium contents in these samples were scattered over the narrow range between 0.032 and 0.100 mg kg{sup -1}.

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

Neutron emission from impacted solid LiD samples

International Nuclear Information System (INIS)

Kaushik, T.C.; Shyam, A.; Kulkarni, L.V.; Srinivasan, M.

1993-01-01

Nylon projectiles with 0.1 g to 0.3 g mass, accelerated to velocities of 0.2-1 km/s using a 60 cm long electromagnetic accelerator (railgun), have been impacted upon solid lithium deuteride (LiD) samples of 3 proportional counters. The output from the BF 3 set-up is monitored in several ways to characterize the possible neutron emission from the target. This includes a simple technique of counting the single channel analyser (SCA) output through a dead-time unit to identify bursts of < 100 μs duration. Counting is started after a delay of ∼ 1 ms to avoid the initial interference from the capacitor bank discharge. The signal is also recorded in a storage oscilloscope from the start of projectile acceleration along with a time marker just before the impact. From a number of shots taken with and without the samples, a significant evidence of neutron emission from the LiD samples appears to emerge. The experiments suggest that approximately 100 neutrons might be generated during every such impact in a duration of < 4 ms. (author). 7 refs., 3 figs

Detection of silver nanoparticles in parsley by solid sampling high-resolution-continuum source atomic absorption spectrometry.

Science.gov (United States)

Feichtmeier, Nadine S; Leopold, Kerstin

2014-06-01

In this work, we present a fast and simple approach for detection of silver nanoparticles (AgNPs) in biological material (parsley) by solid sampling high-resolution-continuum source atomic absorption spectrometry (HR-CS AAS). A novel evaluation strategy was developed in order to distinguish AgNPs from ionic silver and for sizing of AgNPs. For this purpose, atomisation delay was introduced as significant indication of AgNPs, whereas atomisation rates allow distinction of 20-, 60-, and 80-nm AgNPs. Atomisation delays were found to be higher for samples containing silver ions than for samples containing silver nanoparticles. A maximum difference in atomisation delay normalised by the sample weight of 6.27 ± 0.96 s mg(-1) was obtained after optimisation of the furnace program of the AAS. For this purpose, a multivariate experimental design was used varying atomisation temperature, atomisation heating rate and pyrolysis temperature. Atomisation rates were calculated as the slope of the first inflection point of the absorbance signals and correlated with the size of the AgNPs in the biological sample. Hence, solid sampling HR-CS AAS was proved to be a promising tool for identifying and distinguishing silver nanoparticles from ionic silver directly in solid biological samples.

Bismuth as a general internal standard for lead in atomic absorption spectrometry

International Nuclear Information System (INIS)

Bechlin, Marcos A.; Fortunato, Felipe M.; Ferreira, Edilene C.; Neto, José A. Gomes; Nóbrega, Joaquim A.; Donati, George L.; Jones, Bradley T.

2014-01-01

Highlights: • Single internal standard is commonly proposed for definite application in AAS. • Internal standard for general use in AAS techniques is original. • Bi showed efficiency as internal standard for Pb determinations by FAAS and GFAAS. • Assorted samples were analyzed and accurate results were found. - Abstract: Bismuth was evaluated as internal standard for Pb determination by line source flame atomic absorption spectrometry (LS FAAS), high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) and line source graphite furnace atomic absorption spectrometry (LS GFAAS). Analysis of samples containing different matrices indicated close relationship between Pb and Bi absorbances. Correlation coefficients of calibration curves built up by plotting A Pb /A Bi versus Pb concentration were higher than 0.9953 (FAAS) and higher than 0.9993 (GFAAS). Recoveries of Pb improved from 52–118% (without IS) to 97–109% (IS, LS FAAS); 74–231% (without IS) to 96–109% (IS, HR-CS FAAS); and 36–125% (without IS) to 96–110% (IS, LS GFAAS). The relative standard deviations (n = 12) were reduced from 0.6–9.2% (without IS) to 0.3–4.3% (IS, LS FAAS); 0.7–7.7% (without IS) to 0.1–4.0% (IS, HR-CS FAAS); and 2.1–13% (without IS) to 0.4–5.9% (IS, LS GFAAS)

Gastric emptying of solids: When should we sample

International Nuclear Information System (INIS)

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

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.

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.

Estimation of plant sampling uncertainty: an example based on chemical analysis of moss samples.

Science.gov (United States)

Dołęgowska, Sabina

2016-11-01

In order to estimate the level of uncertainty arising from sampling, 54 samples (primary and duplicate) of the moss species Pleurozium schreberi (Brid.) Mitt. were collected within three forested areas (Wierna Rzeka, Piaski, Posłowice Range) in the Holy Cross Mountains (south-central Poland). During the fieldwork, each primary sample composed of 8 to 10 increments (subsamples) was taken over an area of 10 m 2 whereas duplicate samples were collected in the same way at a distance of 1-2 m. Subsequently, all samples were triple rinsed with deionized water, dried, milled, and digested (8 mL HNO 3 (1:1) + 1 mL 30 % H 2 O 2 ) in a closed microwave system Multiwave 3000. The prepared solutions were analyzed twice for Cu, Fe, Mn, and Zn using FAAS and GFAAS techniques. All datasets were checked for normality and for normally distributed elements (Cu from Piaski, Zn from Posłowice, Fe, Zn from Wierna Rzeka). The sampling uncertainty was computed with (i) classical ANOVA, (ii) classical RANOVA, (iii) modified RANOVA, and (iv) range statistics. For the remaining elements, the sampling uncertainty was calculated with traditional and/or modified RANOVA (if the amount of outliers did not exceed 10 %) or classical ANOVA after Box-Cox transformation (if the amount of outliers exceeded 10 %). The highest concentrations of all elements were found in moss samples from Piaski, whereas the sampling uncertainty calculated with different statistical methods ranged from 4.1 to 22 %.

Synthesis and application of novel ion-imprinted polymer coated magnetic multi-walled carbon nanotubes for selective solid phase extraction of lead(II) ions

Energy Technology Data Exchange (ETDEWEB)

Fayazi, Maryam, E-mail: maryam.fayazi@yahoo.com [Mineral Industries Research Center, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Young Researchers Society, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Taher, Mohammad Ali [Department of Chemistry, Faculty of Sciences, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Afzali, Daryoush [Department of Environment, Institute of Science and High Technology and Environmental Sciences, Graduate University of Advanced Technology, Kerman (Iran, Islamic Republic of); Mostafavi, Ali [Department of Chemistry, Faculty of Sciences, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Ghanei-Motlagh, Masoud, E-mail: m.ghaneimotlagh@yahoo.com [Young Researchers Society, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Department of Chemistry, Faculty of Sciences, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of)

2016-03-01

In this study, novel magnetic ion-imprinted polymer (MIIP) nanoparticles were utilized for the sensitive and selective detection of Pb(II) ions by graphite furnace atomic absorption spectrometry (GFAAS). The Pb(II)-imprinted polymer was synthesized by using 4-vinylpyridine (4VP) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the cross-linker, 2,3,5,6-tetra(2-pyridyl) pyrazine (TPPZ) as the chelating agent and magnetic multi-walled carbon nanotubes (MMWCNTs) as the carrier. The synthesized MIIP materials were characterized by field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and vibrating sample magnetometer (VSM). Various analytical parameters such as extraction and desorption time, eluent type and concentration, pH and sample volume were systematically examined. The selectivity of MIIP sorbent for Pb(II) ions in the presence of some cations was also evaluated. The limit of detection (LOD, 3S{sub b}) and the relative standard deviation (RSD, n = 8, c = 25 ng L{sup −1}) were found to be 2.4 ng L{sup −1} and 5.6%, respectively. The maximum sorption capacity of the MIIP for Pb(II) was found to be 48.1 mg g{sup −1}. Finally, the proposed analytical procedure was successfully applied to monitoring lead in human hair and water samples with satisfactory results for the spiked samples. - Highlights: • A selective and sensitive method based on MSPE-GFAAS was proposed. • The MIIP nanoparticles were characterized using FE-SEM, XRD, VSM and FT-IR techniques. • The synthesized MIIP material is efficient at extracting lead ions. • The method was applied to determine lead ions in several real samples.

A pyrolysis/gas chromatographic method for the determination of hydrogen in solid samples

Science.gov (United States)

Carr, R. H.; Bustin, R.; Gibson, E. K.

1987-01-01

A method is described for the determination of hydrogen in solid samples. The sample is heated under vacuum after which the evolved gases are separated by gas chromatography with a helium ionization detector. The system is calibrated by injecting known amounts of hydrogen, as determined manometrically. The method, which is rapid and reliable, was checked for a variety of lunar soils; the limit of detection is about 10 ng of hydrogen.

Solid phase microextraction headspace sampling of chemical warfare agent contaminated samples : method development for GC-MS analysis

Energy Technology Data Exchange (ETDEWEB)

Jackson Lepage, C.R.; Hancock, J.R. [Defence Research and Development Canada, Medicine Hat, AB (Canada); Wyatt, H.D.M. [Regina Univ., SK (Canada)

2004-07-01

Defence R and D Canada-Suffield (DRDC-Suffield) is responsible for analyzing samples that are suspected to contain chemical warfare agents, either collected by the Canadian Forces or by first-responders in the event of a terrorist attack in Canada. The analytical techniques used to identify the composition of the samples include gas chromatography-mass spectrometry (GC-MS), liquid chromatography-mass spectrometry (LC-MS), Fourier-transform infrared spectroscopy (FT-IR) and nuclear magnetic resonance spectroscopy. GC-MS and LC-MS generally require solvent extraction and reconcentration, thereby increasing sample handling. The authors examined analytical techniques which reduce or eliminate sample manipulation. In particular, this paper presented a screening method based on solid phase microextraction (SPME) headspace sampling and GC-MS analysis for chemical warfare agents such as mustard, sarin, soman, and cyclohexyl methylphosphonofluoridate in contaminated soil samples. SPME is a method which uses small adsorbent polymer coated silica fibers that trap vaporous or liquid analytes for GC or LC analysis. Collection efficiency can be increased by adjusting sampling time and temperature. This method was tested on two real-world samples, one from excavated chemical munitions and the second from a caustic decontamination mixture. 7 refs., 2 tabs., 3 figs.

Determination of radiocaesium in agriculture-related water samples containing suspended solids using gelling method

International Nuclear Information System (INIS)

Matsunami, Hisaya; Shin, Moono; Takahashi, Yoshihiko; Shinano, Takuro; Kitajima, Shiori; Tsuchiya, Takashi

2015-01-01

After the TEPCO Fukushima Dai-ichi Nuclear Power Plant accident in 2011, the radiocaesium, which flowed into the paddy fields via irrigation water, have been widely investigated. When the concentration of radiocaesium in the water samples containing suspended solids were directly measured using a high purity germanium detector with a 2 L marinelli beaker, the radiocaesium concentration might be overestimated due to the sedimentation of the suspended solids during the measurement time. In fact, the values obtained by the direct method were higher than those obtained by the filtering method and/or the gelling method in most of the agriculture-related water samples. We concluded that the gelling method using sodium polyacrylate can be widely adapted for the analysis of the total radiocaesium in the agriculture-related water samples because of its many advantage such as simple preparation procedure, accurate analysis values, excellent long-term stability of geometry and low operating cost. (author)

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

International Nuclear Information System (INIS)

Ross, G.A.

1998-01-01

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

Investigation of the suspected presence of solid hydrocarbon in bedded salt samples from the Palo Duro Basin, Texas

International Nuclear Information System (INIS)

1985-10-01

This report contains laboratory test results for two bedded salt samples from the Grabbe No. 1 (PD-2) Well of the Palo Duro Basin, Texas. This study was commissioned to determine whether or not solid hydrocarbons exist in bedded salt samples in the Palo Duro Basin. Laboratory investigations include electron microprobe examinations on polished thin sections and optical examinations and chemical tests on insoluble residues of the salt samples. No direct evidence was found that identifiable solid hydrocarbons are present in either sample of the bedded salt core. The total carbon content of the two salt samples was measured yielding 0.016 and 0.022 weight percent carbon. Detailed microscopic analyses showed that the carbon in the samples was associated with calcite, clays, and the epoxy resin used in sample preparation

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

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...

Localisation and identification of radioactive particles in solid samples by means of a nuclear track technique

International Nuclear Information System (INIS)

Boehnke, Antje; Treutler, Hanns-Christian; Freyer, Klaus; Schubert, Michael; Holger Weiss

2005-01-01

This study is aimed to develop a generally applicable methodology of investigation that can be used for the localisation of single alpha-active particles in solid samples, such as industrial dust or natural soils, sediments and rocks by autoradiography using solid-state nuclear track detectors. The developed technique allows the detection of local enrichments of alpha-emitters in any solid material. The results of such an investigation are of interest from technical, biological and environmental points of view. The idea behind the methodology is to locate the position of alpha-active spots in a sample by attaching the track detector to the sample in a defined manner, thoroughly described in the paper. The located alpha-active particles are subsequently analysed by an electron microscope and an electron microprobe. An example of the application of this methodology is also given. An ultra-fine -grained ore-processing residue, which causes serious environmental pollution in the respective mining district and thus limits possible land use and affects quality of life in the area, was examined using the described technique. The investigation revealed considerable amounts of alpha-active particles in this material

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.

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

International Nuclear Information System (INIS)

Virgilio, Alex; Nóbrega, Joaquim A.; Rêgo, Jardes F.; Neto, José A. Gomes

2012-01-01

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 °C and 2400 °C, respectively. Slopes of calibration curves (50–750 pg Cr, R 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 μg g −1 Cr range. The highest RSD (n = 5) was 15.4% for the sample Melissa officinalis containing 13.9 ± 2.1 μg g −1 Cr. The limit of detection was 3.3 ng g −1 Cr. - Highlights: ► Direct solid sampling is first time employed for Cr in plant materials. ► Calibration curves with liquids and solids are coincident. ► Microanalysis of plants for Cr is validated by reference materials. ► The proposed HR-CS GF AAS method is environmental friendly.

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.

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.

Permeability and compression characteristics of municipal solid waste samples

Science.gov (United States)

Durmusoglu, Ertan; Sanchez, Itza M.; Corapcioglu, M. Yavuz

2006-08-01

Four series of laboratory tests were conducted to evaluate the permeability and compression characteristics of municipal solid waste (MSW) samples. While the two series of tests were conducted using a conventional small-scale consolidometer, the two others were conducted in a large-scale consolidometer specially constructed for this study. In each consolidometer, the MSW samples were tested at two different moisture contents, i.e., original moisture content and field capacity. A scale effect between the two consolidometers with different sizes was investigated. The tests were carried out on samples reconsolidated to pressures of 123, 246, and 369 kPa. Time settlement data gathered from each load increment were employed to plot strain versus log-time graphs. The data acquired from the compression tests were used to back calculate primary and secondary compression indices. The consolidometers were later adapted for permeability experiments. The values of indices and the coefficient of compressibility for the MSW samples tested were within a relatively narrow range despite the size of the consolidometer and the different moisture contents of the specimens tested. The values of the coefficient of permeability were within a band of two orders of magnitude (10-6-10-4 m/s). The data presented in this paper agreed very well with the data reported by previous researchers. It was concluded that the scale effect in the compression behavior was significant. However, there was usually no linear relationship between the results obtained in the tests.

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

Study on solid phase extraction and graphite furnace atomic absorption spectrometry for the determination of nickel, silver, cobalt, copper, cadmium and lead with MCI GEL CHP 20Y as sorbent

International Nuclear Information System (INIS)

Yang Guangyu; Fen Weibo; Lei Chun; Xiao Weilie; Sun Handong

2009-01-01

A solid phase extraction and graphite furnace atomic absorption spectrometry (GFAAS) for the determination of nickel, silver, cobalt, copper, cadmium and lead with MCI GEL CHP 20Y as sorbent was studied. Trace amounts of chromium, nickel, silver, cobalt, copper, cadmium and lead were reacted with 2-(2-quinolinil-azo)-4-methyl-1,3-dihydroxidobenzene (QAMDHB) followed by adsorption onto MCI GEL CHP 20Y solid phase extraction column, and 1.0 mol L -1 HNO 3 was used as eluent. The metal ions in 300 mL solution can be concentrated to 1.0 mL, representing an enrichment factor of 300 was achieved. The recoveries of analytes at pH 8.0 with 1.0 g of resin were greater than 95% without interference from alkaline, earth alkaline and some metal ions. When detected with graphite furnace atomic absorption spectrometry, the detection limits in the original samples were 1.4 ng L -1 for Cr(III), 1.0 ng L -1 for Ni(II), 0.85 ng L -1 for Ag(I), 1.2 ng L -1 for Co(II), 1.0 ng L -1 for Cu(II), 1.2 ng L -1 for Cd(II) and 1.3 ng L -1 for Pb(II). The validation of the procedure was performed by the analysis of the certified standard reference materials, and the presented procedure was applied to the determination of analytes in biological, water and soil samples with good results (recoveries range from 89 to 104%, and R.S.D.% lower than 3.2%. The results agreed with the standard value or reference method)

Se Concentrations in Epiphytic Lichens From the Boreal Forest of Forthern Québec

Science.gov (United States)

Marin, L.; Lhomme, J.; Carignan, J.

2004-05-01

The knowledge of Se concentration in environmental samples is important because this element may be both toxic and nutrient for live organisms. This study aims to characterise the Se concentration in lichen samples in order to document the variability of atmospheric fallout. Lichens are of particular interest because their epiphytic character makes them totally dependant of atmospheric nutrients, so that their chemical composition reflects that of atmospheric matter. Lichens hanging on tree branches were sampled in various location of the boreal forest of northern Québec. We developed a separation and pre-concentration technique for Se analysis of low mineral matrix samples by GFAAS. After mineralisation and addition of a Se-free mineral charge to the sample, total Se is reduced to Se IV and fixed onto a thiol cotton. The latter is dissolved and directly analysed by GFAAS. A limit of determination of 0.02 ppm in the solid sample and a precision (relative standard deviation) varying from 3 to 15% was found through the course of this study. Our results are very similar to the certified values of the reference materials analysed, suggesting a good accuracy of the method for organic materials. Some lichen samples were also analysed by INAA and the agreement between results obtained by both techniques is not always perfect. There is, however, no systematic bias between the methods. Some samples agree within analytical uncertainty (about 5%), whereas others differ by more than 20%. The most probable reason why such discrepancies are observed is because these lichen samples were not crushed and homogenised before analysis. Indeed, some duplicate samples analysed by INAA yielded results that differed by more than 20%, while other agreed within 2%. Considering these facts, the overall agreement between GFAAS and INAA is pretty much satisfactory. The Se concentrations measured in lichens vary from 1.2 to 0.3 ppm and decrease from the coast of Hudson Bay towards inland at

Polychlorinated biphenyls (PCB) analysis report for solid sample from 219S tank 101

International Nuclear Information System (INIS)

Diaz, L.A.

1998-01-01

One waste sample that was obtained with solids from tank 101 of 219S via a peristaltic pump equipped with a stainless steel tube and Norprene tubing (Phthalate free) was obtained in a glass jar with teflon lid was analyzed (with duplicate, matrix spike, and matrix spike duplicate) for PCBs as Aroclor mixtures by the Inorganic/Organic Chemistry Group. A soxhlet extraction procedure was used for extraction of the Aroclors from the sample. Analysis was performed using dual column confirmation gas chromatography/electron capture detection (GC/ECD). Results are presented

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of arsenic and selenium in water and sediment by graphite furnace atomic absorption spectrometry

Science.gov (United States)

Jones, Sandra R.; Garbarino, John R.

1999-01-01

Graphite furnace-atomic absorption spectrometry (GF-AAS) is a sensitive, precise, and accurate technique that can be used to determine arsenic and selenium in samples of water and sediment. The GF-AAS method has been developed to replace the hydride generation-atomic absorption spectrometry (HG-AAS) methods because the method detection limits are similar, bias and variability are comparable, and interferences are minimal. Advantages of the GF-AAS method include shorter sample preparation time, increased sample throughput from simultaneous multielement analysis, reduced amount of chemical waste, reduced sample volume requirements, increased linear concentration range, and the use of a more accurate digestion procedure. The linear concentration range for arsenic and selenium is 1 to 50 micrograms per liter in solution; the current method detection limit for arsenic in solution is 0.9 microgram per liter; the method detection limit for selenium in solution is 1 microgram per liter. This report describes results that were obtained using stop-flow and low-flow conditions during atomization. The bias and variability of the simultaneous determination of arsenic and selenium by GF-AAS under both conditions are supported with results from standard reference materials--water and sediment, real water samples, and spike recovery measurements. Arsenic and selenium results for all Standard Reference Water Samples analyzed were within one standard deviation of the most probable values. Long-term spike recoveries at 6.25, 25.0, 37.5 micrograms per liter in reagent-, ground-, and surface-water samples for arsenic averaged 103 plus or minus 2 percent using low-flow conditions and 104 plus or minus 4 percent using stop-flow conditions. Corresponding recoveries for selenium were 98 plus or minus 13 percent using low-flow conditions and 87 plus or minus 24 percent using stop-flow conditions. Spike recoveries at 25 micrograms per liter in 120 water samples ranged from 97 to 99 percent

Effects of sample preparation conditions on biomolecular solid-state NMR lineshapes

Energy Technology Data Exchange (ETDEWEB)

Jakeman, David L.; Mitchell, Dan J.; Shuttleworth, Wendy A.; Evans, Jeremy N.S. [Washington State University, Department of Biochemistry and Biophysics (United States)

1998-10-15

Sample preparation conditions with the 46 kDa enzyme complex of 5-enolpyruvyl-shikimate-3-phosphate (EPSP) synthase, shikimate-3-phosphate (S3P) and glyphosate (GLP) have been examined in an attempt to reduce linewidths in solid-state NMR spectra. The linewidths of {sup 13}P resonances associated with enzyme bound S3P and GLP in the lyophilized ternary complex have been reduced to 150 {+-} 12 Hz and 125 {+-} 7 Hz respectively, by a variety of methods involving additives and freezing techniques.

A general assignment method for oriented sample (OS) solid-state NMR of proteins based on the correlation of resonances through heteronuclear dipolar couplings in samples aligned parallel and perpendicular to the magnetic field.

Science.gov (United States)

Lu, George J; Son, Woo Sung; Opella, Stanley J

2011-04-01

A general method for assigning oriented sample (OS) solid-state NMR spectra of proteins is demonstrated. In principle, this method requires only a single sample of a uniformly ¹⁵N-labeled membrane protein in magnetically aligned bilayers, and a previously assigned isotropic chemical shift spectrum obtained either from solution NMR on micelle or isotropic bicelle samples or from magic angle spinning (MAS) solid-state NMR on unoriented proteoliposomes. The sequential isotropic resonance assignments are transferred to the OS solid-state NMR spectra of aligned samples by correlating signals from the same residue observed in protein-containing bilayers aligned with their normals parallel and perpendicular to the magnetic field. The underlying principle is that the resonances from the same residue have heteronuclear dipolar couplings that differ by exactly a factor of two between parallel and perpendicular alignments. The method is demonstrated on the membrane-bound form of Pf1 coat protein in phospholipid bilayers, whose assignments have been previously made using an earlier generation of methods that relied on the preparation of many selectively labeled (by residue type) samples. The new method provides the correct resonance assignments using only a single uniformly ¹⁵N-labeled sample, two solid-state NMR spectra, and a previously assigned isotropic spectrum. Significantly, this approach is equally applicable to residues in alpha helices, beta sheets, loops, and any other elements of tertiary structure. Moreover, the strategy bridges between OS solid-state NMR of aligned samples and solution NMR or MAS solid-state NMR of unoriented samples. In combination with the development of complementary experimental methods, it provides a step towards unifying these apparently different NMR approaches. Copyright © 2011 Elsevier Inc. All rights reserved.

The influence of pyrolysis and matrix modifiers on determination of Cr and Pb in sediment samples by GFAAS

Directory of Open Access Journals (Sweden)

Risfidian Mohadi

2016-04-01

Full Text Available Abstract: The Influence of pyrolysis and matrix modifiers on determination of Cr and Pb in sediment samples using graphite furnace atomic absorption spectrometry has been investigated. The sediment samples including three certified reference materials (CRMs are reported. Analyses were performed using microwave assisted dissolution. The matrix modifiers Mg(NO32, Pd+Mg(NO32 and NH4H2PO4were shown to be optimazed. The recovery for Cr and Pb in CRMs in the case of sample dissolution was found to be between 81 to 91% for Cr and 94 to 98% for Pb of the certified values, respectively. Keywords: Sediment, Pyrolysis, Matrix modifiers, Cr, Pb Abstrak (Indonesia: Pengaruh pirolisis dan matriks pengubah pada penentuan Cr dan Pb dalam sampel sedimen menggunakan tungku grafit spektroskopi serapan atom telah diteliti. Sampel sedimen termasuk tiga bahan referensi bersertifikat (CRMs dilaporkan dianalisis dengan menggunakan bantuan microwave ekstraktor. Matriks pengubah Mg(NO32, Pd+Mg(NO32 dan NH4H2PO4 telah digunakan dan menghasilkan nilai temu balik untuk Cr dan Pb dalam CRMs ditemukan antara 81-91% untuk Cr dan 94-98 % untuk Pb dari nilai sertifikat masing-masing. Katakunci: Sedimen, Pirolisis, Matrix modifiers, Cr, Pb

Molecularly imprinted solid-phase extraction of glutathione from urine samples

International Nuclear Information System (INIS)

Song, Renyuan; Hu, Xiaoling; Guan, Ping; Li, Ji; Zhao, Na; Wang, Qiaoli

2014-01-01

Molecularly imprinted polymer (MIP) particles for glutathione were synthesized through iniferter-controlled living radical precipitation polymerization (IRPP) under ultraviolet radiation at ambient temperature. Static adsorption, solid-phase extraction, and high-performance liquid chromatography were carried out to evaluate the adsorption properties and selective recognition characteristics of the polymers for glutathione and its structural analogs. The obtained IRPP-MIP particles exhibited a regularly spherical shape, rapid binding kinetics, high imprinting factor, and high selectivity compared with the MIP particles prepared using traditional free-radical precipitation polymerization. The selective separation and enrichment of glutathione from the mixture of glycyl-glycine and glutathione disulfide could be achieved on the IRPP-MIP cartridge. The recoveries of glutathione, glycyl-glycine, and glutathione disulfide were 95.6% ± 3.65%, 29.5% ± 1.26%, and 49.9% ± 1.71%, respectively. The detection limit (S/N = 3) of glutathione was 0.5 mg·L −1 . The relative standard deviations (RSDs) for 10 replicate detections of 50 mg·L −1 of glutathione were 5.76%, and the linear range of the calibration curve was 0.5 mg·L −1 to 200 mg·L −1 under optimized conditions. The proposed approach was successfully applied to determine glutathione in spiked human urine samples with recoveries of 90.24% to 96.20% and RSDs of 0.48% to 5.67%. - Highlights: • Imprinted polymer particles were prepared by IRPP at ambient temperature. • High imprinting factor, high selectivity, and rapid binding kinetics were achieved. • Selective solid-phase extraction of glutathione from human urine samples

SESAR: Addressing the need for unique sample identification in the Solid Earth Sciences

Science.gov (United States)

Lehnert, K. A.; Goldstein, S. L.; Lenhardt, C.; Vinayagamoorthy, S.

2004-12-01

The study of solid earth samples is key to our knowledge of Earth's dynamical systems and evolution. The data generated provide the basis for models and hypotheses in all disciplines of the Geosciences from tectonics to magmatic processes to mantle dynamics to paleoclimate research. Sample-based data are diverse ranging from major and trace element abundances, radiogenic and stable isotope ratios of rocks, minerals, fluid or melt inclusions, to age determinations and descriptions of lithology, texture, mineral or fossil content, stratigraphic context, physical properties. The usefulness of these data is critically dependent on their integration as a coherent data set for each sample. If different data sets for the same sample cannot be combined because the sample cannot be unambiguously recognized, valuable information is lost. The ambiguous naming of samples has been a major problem in the geosciences. Different samples are often given identical names, and there is a tendency for different people analyzing the same sample to rename it in their publications according to local conventions. This situation has generated significant confusion, with samples often losing their "history", making it difficult or impossible to link available data. This has become most evident through the compilation of geochemical data in relational databases such as PetDB, NAVDAT, and GEOROC. While the relational data structure allows linking of disparate data for samples published in different references, linkages cannot be established due to ambiguous sample names. SESAR is a response to this problem of ambiguous naming of samples. SESAR will create a common clearinghouse that provides a centralized registry of sample identifiers, to avoid ambiguity, to systematize sample designation, and ensure that all information associated with a sample would in fact be unique. The project will build a web-based digital registry for solid earth samples that will provide for the first time a way to

Bismuth as a general internal standard for lead in atomic absorption spectrometry.

Science.gov (United States)

Bechlin, Marcos A; Fortunato, Felipe M; Ferreira, Edilene C; Gomes Neto, José A; Nóbrega, Joaquim A; Donati, George L; Jones, Bradley T

2014-06-11

Bismuth was evaluated as internal standard for Pb determination by line source flame atomic absorption spectrometry (LS FAAS), high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) and line source graphite furnace atomic absorption spectrometry (LS GFAAS). Analysis of samples containing different matrices indicated close relationship between Pb and Bi absorbances. Correlation coefficients of calibration curves built up by plotting A(Pb)/A(Bi)versus Pb concentration were higher than 0.9953 (FAAS) and higher than 0.9993 (GFAAS). Recoveries of Pb improved from 52-118% (without IS) to 97-109% (IS, LS FAAS); 74-231% (without IS) to 96-109% (IS, HR-CS FAAS); and 36-125% (without IS) to 96-110% (IS, LS GFAAS). The relative standard deviations (n=12) were reduced from 0.6-9.2% (without IS) to 0.3-4.3% (IS, LS FAAS); 0.7-7.7% (without IS) to 0.1-4.0% (IS, HR-CS FAAS); and 2.1-13% (without IS) to 0.4-5.9% (IS, LS GFAAS). Copyright © 2014 Elsevier B.V. All rights reserved.

On-line determination of manganese in solid seafood samples by flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Yebra, M.C.; Moreno-Cid, A.

2003-01-01

Manganese is extracted on-line from solid seafood samples by a simple continuous ultrasound-assisted extraction system (CUES). This system is connected to an on-line manifold, which permits the flow-injection flame atomic absorption spectrometric determination of manganese. Optimisation of the continuous leaching procedure is performed by an experimental design. The proposed method allows the determination of manganese with a relative standard deviation of 0.9% for a sample containing 23.4 μg g -1 manganese (dry mass). The detection limit is 0.4 μg g -1 (dry mass) for 30 mg of sample and the sample throughput is ca. 60 samples per hour. Accurate results are obtained by measuring TORT-1 certified reference material. The procedure is finally applied to mussel, tuna, sardine and clams samples

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

International Nuclear Information System (INIS)

Edjabou, Maklawe Essonanawe; Jensen, Morten Bang; Götze, Ramona; Pivnenko, Kostyantyn; Petersen, Claus; Scheutz, Charlotte; Astrup, Thomas Fruergaard

2015-01-01

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

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

Solid Phase Microextraction (SPME in Determination of Pesticide Residues in Soil Samples

Directory of Open Access Journals (Sweden)

Rada Đurović

2011-01-01

Full Text Available The basic principles and application possibilities of the methods based on solid phase microextraction (SPME in the analysis of pesticide residues in soil samples are presented in the paper. The most important experimental parameters which affect SPME efficacy inpesticide determination (type and thickness of microextraction fiber, duration of microextraction,temperature at which it is conducted, effect of addition of salts (the effect of efflorescence,temperature and time of desorption, the choice of optimal solvent for pesticide exctraction from the soil and the optimal number of extraction steps, as well as general guidelines for their optimization are also shown. In the end, current applications of SPMEmethods in the analysis of pesticide residues in soil samples are presented.

Sampling of tar from sewage sludge gasification using solid phase adsorption.

Science.gov (United States)

Ortiz González, Isabel; Pérez Pastor, Rosa Ma; Sánchez Hervás, José Ma

2012-06-01

Sewage sludge is a residue from wastewater treatment plants which is considered to be harmful to the environment and all living organisms. Gasification technology is a potential source of renewable energy that converts the sewage sludge into gases that can be used to generate energy or as raw material in chemical synthesis processes. But tar produced during gasification is one of the problems for the implementation of the gasification technology. Tar can condense on pipes and filters and may cause blockage and corrosion in the engines and turbines. Consequently, to minimize tar content in syngas, the ability to quantify tar levels in process streams is essential. The aim of this work was to develop an accurate tar sampling and analysis methodology using solid phase adsorption (SPA) in order to apply it to tar sampling from sewage sludge gasification gases. Four types of commercial SPA cartridges have been tested to determine the most suitable one for the sampling of individual tar compounds in such streams. Afterwards, the capacity, breakthrough volume and sample stability of the Supelclean™ ENVI-Carb/NH(2), which is identified as the most suitable, have been determined. Basically, no significant influences from water, H(2)S or NH(3) were detected. The cartridge was used in sampling real samples, and comparable results were obtained with the present and traditional methods.

Development of a portable mass spectrometric system for determination of isotopic composition of solid uranium samples using fluorine volatilization

Science.gov (United States)

Loge, G.

1994-09-01

Using hardware and materials supplied by LANL, a prototype quadrupole mass spectrometer system designed for portable field analysis of isotopic composition of solid uranium samples was assembled and tested. The system contained the capability for fluorine volatilization of solid uranium samples with gas introduction, which was successfully tested and demonstrated using 100 mg samples of U3O8. Determination of precision and accuracy for measuring isotopic composition was performed using isotopic standards. Use with soil samples containing uranium were also attempted. Silicates in the soil forming SiF4 were found to be a kinetic bottleneck to the formation of UF6. This could be avoided by performing some sort of chemical separation as a pre-treatment step, which was demonstrated using nitric acid.

Solid sampling-graphite furnace atomic absorption spectrometry for the direct determination of boron in plant tissues

International Nuclear Information System (INIS)

Resano, M.; Briceno, J.; Aramendia, M.; Belarra, M.A.

2007-01-01

In this work, the potential of graphite furnace atomic absorption spectrometry for the direct determination of B in plant tissues has been investigated. Three certified reference materials (NIST SRM 1570a spinach leaves, NIST SRM 1573a tomato leaves and BCR CRM 679 white cabbage) were selected for this study, the goal always being to develop a fast procedure that could be robust enough to provide a satisfactory performance for all of them, without any modifications in the conditions applied. The use of a suitable chemical modifier was found to be essential for obtaining a reproducible and sufficiently sensitive signal for boron solutions. In this regard, the performance of the combination of citric acid plus W (added as a permanent modifier) was noteworthy, resulting in well-defined signal profiles, a remarkable analyte stabilization during the pyrolysis step (up to 2100 deg. C) and minimal memory effects. This mixture of modifiers provided a good performance for the direct analysis of solid samples as well, but only if a suitable temperature program, favoring the interaction between the analyte and the modifiers, was used. Thus, such a temperature program, with two pyrolysis steps and the addition of NH 4 NO 3 in order to carry out the in situ sample microdigestion, was optimized. Under these conditions, the peak areas obtained for both solid samples and aqueous standards were comparable. Finally, the analysis of the samples was carried out. In all cases, a good agreement with the certified values was obtained, while R.S.D. values ranged between 6 and 10%. It can be concluded that the method proposed shows significant advantages for the determination of this complicated element in solid samples such as the use of aqueous standards for calibration, a high sample throughput (20 min per sample), a suitable limit of detection (0.3 μg g -1 ) and reduced risk of analyte losses and contamination

Simultaneous Effects of Total Solids Content, Milk Base, Heat Treatment Temperature and Sample Temperature on the Rheological Properties of Plain Stirred Yogurt

Directory of Open Access Journals (Sweden)

Attilio Converti

2006-01-01

Full Text Available Response surface methodology was used to establish a relationship between total solids content, milk base, heat treatment temperature, and sample temperature, and consistency index, flow behaviour index, and apparent viscosity of plain stirred yogurts. Statistical treatments resulted in developments of mathematical models. All samples presented shear thinning fluid behaviour. The increase of the content of total solids (9.3–22.7 % and milk base heat treatment temperature (81.6–98.4 °C resulted in a significant increase in consistency index and a decrease in flow behaviour index. Increase in the sample temperature (1.6–18.4 °C caused a decrease in consistency index and increase in flow behaviour index. Apparent viscosity was directly related to the content of total solids. Rheological properties of yogurt were highly dependent on the content of total solids in milk.

Direct determination of cadmium in foods by solid sampling electrothermal vaporization inductively coupled plasma mass spectrometry using a tungsten coil trap

Science.gov (United States)

Zhang, Ying; Mao, Xuefei; Liu, Jixin; Wang, Min; Qian, Yongzhong; Gao, Chengling; Qi, Yuehan

2016-04-01

In this work, a solid sampling device consisting of a tungsten coil trap, porous carbon vaporizer and on-line ashing furnace of a Ni-Cr coil was interfaced with inductively coupled plasma mass spectrometry (ICP-MS). A modified double gas circuit system was employed that was composed of carrier and supplemental gas lines controlled by separate gas mass flow controllers. For Cd determination in food samples using the assembled solid sampling ICP-MS, the optimal ashing and vaporization conditions, flow rate of the argon-hydrogen (Ar/H2) (v:v = 24:1) carrier gas and supplemental gas, and minimum sampling mass were investigated. Under the optimized conditions, the limit of quantification was 0.5 pg and the relative standard deviation was within a 10.0% error range (n = 10). Furthermore, the mean spiked recoveries for various food samples were 99.4%-105.9% (n = 6). The Cd concentrations measured by the proposed method were all within the certified values of the reference materials or were not significantly different (P > 0.05) from those of the microwave digestion ICP-MS method, demonstrating the good accuracy and precision of the solid sampling ICP-MS method for Cd determination in food samples.

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.

Headspace Solid Phase Microextraction in Pesticide Residues Analysis: 2. Apple Samples

Directory of Open Access Journals (Sweden)

Jelena Milinović

2007-01-01

Full Text Available Headspace solid phase microextraction method (HS/SPME, optimised previously for pesticide water solutions, was applied to trace residues of the pesticides chlorpyrifos, fenthion and bifenthrin in apple samples. One-hour extraction procedure was performed at 60oC extraction temperature. Nonpolar polydimethyl siloxane (PDMS fiber was used. Detection and quantification were carried out by gas chromatography/mass spectrometry (GC/MS. A non-pesticide treated apple sample was fortified with the pesticides over a 0.025-1.25 mg/kg concentration range in order to determine analytical parameters of the method applied. Linearity with regression coefficient (R values higher than 0.99 were obtained over the whole concentration range investigated for chlorpyrifos and fenthion, while linear dependence was observed in the 0.1-1.25 mg/kg range for bifenthrin. Relative recovery values for samples fortified at different levels were in the 56.68-82.91% range. Limit of detection (LOD values were determined as follows: 0.014 mg/kg for chlorpyrifos, 0.021 mg/kg for fenthion and 0.053 mg/kg for bifenthrin. Relative standard deviation (RSD values obtained for multiple analysis of the sample fortified at 0.6 mg/kg level were not higher than 20%.

Liquid-phase microextraction combined with graphite furnace atomic absorption spectrometry: A review

Energy Technology Data Exchange (ETDEWEB)

Calle, Inmaculada de la; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos, E-mail: bendicho@uvigo.es

2016-09-14

An overview of the combination of liquid-phase microextraction (LPME) techniques with graphite furnace atomic absorption spectrometry (GFAAS) is reported herein. The high sensitivity of GFAAS is significantly enhanced by its association with a variety of miniaturized solvent extraction approaches. LPME-GFAAS thus represents a powerful combination for determination of metals, metalloids and organometallic compounds at (ultra)trace level. Different LPME modes used with GFAAS are briefly described, and the experimental parameters that show an impact in those microextraction processes are discussed. Special attention is paid to those parameters affecting GFAAS analysis. Main issues found when coupling LPME and GFAAS, as well as those strategies reported in the literature to solve them, are summarized. Relevant applications published on the topic so far are included. - Highlights: • We review the LPME-GFAAS combination in a comprehensive way. • A brief description of main LPME modes is included. • Effect of experimental parameters in the performance of LPME-GFAAS is discussed. • Main applications for trace element analysis and speciation are reviewed.

Liquid-phase microextraction combined with graphite furnace atomic absorption spectrometry: A review

International Nuclear Information System (INIS)

Calle, Inmaculada de la; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

2016-01-01

An overview of the combination of liquid-phase microextraction (LPME) techniques with graphite furnace atomic absorption spectrometry (GFAAS) is reported herein. The high sensitivity of GFAAS is significantly enhanced by its association with a variety of miniaturized solvent extraction approaches. LPME-GFAAS thus represents a powerful combination for determination of metals, metalloids and organometallic compounds at (ultra)trace level. Different LPME modes used with GFAAS are briefly described, and the experimental parameters that show an impact in those microextraction processes are discussed. Special attention is paid to those parameters affecting GFAAS analysis. Main issues found when coupling LPME and GFAAS, as well as those strategies reported in the literature to solve them, are summarized. Relevant applications published on the topic so far are included. - Highlights: • We review the LPME-GFAAS combination in a comprehensive way. • A brief description of main LPME modes is included. • Effect of experimental parameters in the performance of LPME-GFAAS is discussed. • Main applications for trace element analysis and speciation are reviewed.

Determination of Pu isotopic composition and 241Am by high resolution gamma spectrometry on solid samples

International Nuclear Information System (INIS)

Sarkar, Arnab; Paul, Sumana; Aggarwal, Suresh K.; Tomar, Bhupendra S.

2011-08-01

The present report gives a detailed account of the development of non-destructive assay technique using high resolution gamma-ray spectrometry (HRGS) for determination of plutonium (Pu) isotopic composition and the 241 Am content in solid Pu samples. Energy range 120-420 keV was used in this study. The methodology involves in situ relative efficiency calibration during the measurement process itself, to reduce the errors and increase the reliability of the method. Twenty solid Pu samples of power reactor and research reactor grade were analyzed by this method and the results were compared with those obtained by thermal ionization mass spectrometry. The accuracy of the final results depends strongly upon the accuracy of the available nuclear data (decay constant, gamma abundance etc.). MATLAB based programme was written to perform the analysis. A counting time of 4 hour was chosen for achieving good statistics on the results for samples having 100-200 mg of Pu. The attainable accuracy is found to be 0.5-1% for the fissile isotopes ( 239 Pu + 241 Pu) and 5-10% for 241 Am content. (author)

Inorganic mass spectrometry of solid samples

International Nuclear Information System (INIS)

Adams, F.; Vertes, A.

1990-01-01

In this review some recent developments in the field of inorganic mass spectrometry of solids are described with special emphasis on the actual state of understanding of the ionization processes. It concentrates on the common characteristics of methods such as spark source-, laser-, secondary ion-, inductively coupled plasma- and glow discharge mass spectrometry. (orig.)

Discrete element method (DEM) simulations of stratified sampling during solid dosage form manufacturing.

Science.gov (United States)

Hancock, Bruno C; Ketterhagen, William R

2011-10-14

Discrete element model (DEM) simulations of the discharge of powders from hoppers under gravity were analyzed to provide estimates of dosage form content uniformity during the manufacture of solid dosage forms (tablets and capsules). For a system that exhibits moderate segregation the effects of sample size, number, and location within the batch were determined. The various sampling approaches were compared to current best-practices for sampling described in the Product Quality Research Institute (PQRI) Blend Uniformity Working Group (BUWG) guidelines. Sampling uniformly across the discharge process gave the most accurate results with respect to identifying segregation trends. Sigmoidal sampling (as recommended in the PQRI BUWG guidelines) tended to overestimate potential segregation issues, whereas truncated sampling (common in industrial practice) tended to underestimate them. The size of the sample had a major effect on the absolute potency RSD. The number of sampling locations (10 vs. 20) had very little effect on the trends in the data, and the number of samples analyzed at each location (1 vs. 3 vs. 7) had only a small effect for the sampling conditions examined. The results of this work provide greater understanding of the effect of different sampling approaches on the measured content uniformity of real dosage forms, and can help to guide the choice of appropriate sampling protocols. Copyright © 2011 Elsevier B.V. All rights reserved.

A new method for determining the uranium and thorium distribution in volcanic rock samples using solid state nuclear track detectors

International Nuclear Information System (INIS)

Misdaq, M.A.; Bakhchi, A.; Ktata, A.; Koutit, A.; Lamine, J.; Ait nouh, F.; Oufni, L.

2000-01-01

A method based on using solid state nuclear track detectors (SSNTD) CR- 39 and LR-115 type II and calculating the probabilities for the alpha particles emitted by the uranium and thorium series to reach and be registered on these films was utilized for uranium and thorium contents determination in various geological samples. The distribution of uranium and thorium in different volcanic rocks has been investigated using the track fission method. In this work, the uranium and thorium contents have been determined in different volcanic rock samples by using CR-39 and LR-115 type II solid state nuclear track detectors (SSNTD). The mean critical angles of etching of the solid state nuclear track detectors utilized have been calculated. A petrographical study of the volcanic rock thin layers studied has been conducted. The uranium and thorium distribution inside different rock thin layers has been studied. The mechanism of inclusion of the uranium and thorium nuclei inside the volcanic rock samples studied has been investigated. (author)

Selective sampling and measurement of Cr (VI) in water with polyquaternary ammonium salt as a binding agent in diffusive gradients in thin-films technique

Energy Technology Data Exchange (ETDEWEB)

Chen, Hong, E-mail: redastar@163.com [College of Chemistry, Chemical Engineering and Food Safety, Bohai University (China); Research Institute of Food Science, Bohai University (China); Food Safety Key Lab of Liaoning Province, Jinzhou 121013 (China); Zhang, Yang-Yang; Zhong, Ke-Li; Guo, Lian-Wen [College of Chemistry, Chemical Engineering and Food Safety, Bohai University (China); Research Institute of Food Science, Bohai University (China); Food Safety Key Lab of Liaoning Province, Jinzhou 121013 (China); Gu, Jia-Li [College of Chemistry, Chemical Engineering and Food Safety, Bohai University (China); Bo, Le; Zhang, Meng-Han [College of Chemistry, Chemical Engineering and Food Safety, Bohai University (China); Research Institute of Food Science, Bohai University (China); Food Safety Key Lab of Liaoning Province, Jinzhou 121013 (China); Li, Jian-Rong, E-mail: lijianrong@zjgsu.edu.cn [College of Chemistry, Chemical Engineering and Food Safety, Bohai University (China); Research Institute of Food Science, Bohai University (China); Food Safety Key Lab of Liaoning Province, Jinzhou 121013 (China)

2014-04-01

Graphical abstract: - Highlights: • We develop a new DGT device for in situ sampling Cr (VI) in water. • Polyquaternary ammonium salt (PQAS) was used as binding agent of DGT device. • Cr (VI) can be accumulated in the PQAS binding phase whereas Cr (III) cannot. • The DGT performance was independent of pH 3–12 and ionic strength 1 × 10{sup −3}–1 mol L{sup −1}. - Abstract: A diffusive gradients in thin films (DGT) device with polyquaternary ammonium salt (PQAS) as a novel binding agent (PQAS DGT) combined with graphite furnace atomic absorption spectrometry (GFAAS) was developed for the selective sampling and measurement of Cr (VI) in water. The performance of PQAS DGT was independent of pH 3–12 and ionic strength from 1 × 10{sup −3} to 1 mol L{sup −1}. DGT validation experiments showed that Cr (VI) was measured accurately as well as selectively by PQAS DGT, whereas Cr (III) was not determined quantitatively. Compared with diphenylcarbazide spectrophotometric method (DPC), the measurement of Cr (VI) with PQAS DGT was agreement with that of DPC method in the industrial wastewater. PQAS-DGT device had been successfully deployed in local freshwater. The concentrations of Cr (VI) determined by PQAS DGT coupled with GFAAS in Nuer River, Ling River and North Lake were 0.73 ± 0.09 μg L{sup −1}, 0.50 ± 0.07 μg L{sup −1} and 0.61 ± 0.07 μg L{sup −1}, respectively. The results indicate that PQAS DGT device can be used for the selective sampling and measurement Cr (VI) in water and its detection limit is lower than that of DPC method.

Selective sampling and measurement of Cr (VI) in water with polyquaternary ammonium salt as a binding agent in diffusive gradients in thin-films technique

International Nuclear Information System (INIS)

Chen, Hong; Zhang, Yang-Yang; Zhong, Ke-Li; Guo, Lian-Wen; Gu, Jia-Li; Bo, Le; Zhang, Meng-Han; Li, Jian-Rong

2014-01-01

Graphical abstract: - Highlights: • We develop a new DGT device for in situ sampling Cr (VI) in water. • Polyquaternary ammonium salt (PQAS) was used as binding agent of DGT device. • Cr (VI) can be accumulated in the PQAS binding phase whereas Cr (III) cannot. • The DGT performance was independent of pH 3–12 and ionic strength 1 × 10 −3 –1 mol L −1 . - Abstract: A diffusive gradients in thin films (DGT) device with polyquaternary ammonium salt (PQAS) as a novel binding agent (PQAS DGT) combined with graphite furnace atomic absorption spectrometry (GFAAS) was developed for the selective sampling and measurement of Cr (VI) in water. The performance of PQAS DGT was independent of pH 3–12 and ionic strength from 1 × 10 −3 to 1 mol L −1 . DGT validation experiments showed that Cr (VI) was measured accurately as well as selectively by PQAS DGT, whereas Cr (III) was not determined quantitatively. Compared with diphenylcarbazide spectrophotometric method (DPC), the measurement of Cr (VI) with PQAS DGT was agreement with that of DPC method in the industrial wastewater. PQAS-DGT device had been successfully deployed in local freshwater. The concentrations of Cr (VI) determined by PQAS DGT coupled with GFAAS in Nuer River, Ling River and North Lake were 0.73 ± 0.09 μg L −1 , 0.50 ± 0.07 μg L −1 and 0.61 ± 0.07 μg L −1 , respectively. The results indicate that PQAS DGT device can be used for the selective sampling and measurement Cr (VI) in water and its detection limit is lower than that of DPC method

Separation and preconcentration of platinum-group metals from spent autocatalysts solutions using a hetero-polymeric S, N-containing sorbent and determination by high-resolution continuum source graphite furnace atomic absorption spectrometry.

Science.gov (United States)

Eskina, Vasilina V; Dalnova, Olga A; Filatova, Daria G; Baranovskaya, Vasilisa B; Karpov, Yuri A

2016-10-01

This paper describes the potential of high-resolution continuum source graphite furnace atomic absorption spectrometry for determination of Pt, Pd and Rh after separation and concentration by original in-house developed heterochain polymer S, N-containing sorbent. The methods of sample preparation of spent ceramic-based autocatalysts were considered, two of which were used: autoclave decomposition in mixture of acids HCl:HNO3 (3:1) and high-temperature melting with K2S2O7. Both methods anyway limit the direct determination of analytes by HR CS GFAAS. Using the first method it is an incomplete digestion of spent autocatalysts samples, since the precipitate is Si, and the rhodium metal dissolves with difficulty and partially passes into solution. In contrast to the first method, the second method allow to completely transfer analytes into solution, however, the background signal produced by the chemical composition of the flux, overlaps the analytical zone. It was found, that Pt, Pd and Rh contained in the spent ceramic automotive catalysts could be effectively separated and concentrated by heterochain polymer S, N-containing sorbent, which has high sorption capacity, selectivity and resistant to dilute acids. The chosen HR CS GFAAS analysis conditions enable us to determine Pt, Pd and Rh with good metrological characteristics. The concentrations of Pt, Pd and Rh in two samples of automobile exhaust catalysts were found in range of 0.00015-0.00050; 0.170-0.189; 0.0180-0.0210wt%, respectively. The relative standard deviation obtained by HR CS GFAAS was not more than 5%. Limits of detection by HR CS GFAAS achieved were 6.2·10(-6)wt% for Pt, 1.8·10(-6)wt% for Pd, and 3.4·10(-6)wt% for Rh. Limits of determination achieved by HR CS GFAAS were 1.1·10(-5)wt% for Pt, 6.9·10(-5)wt% for Pd, and 8.3·10(-5)wt% for Rh. To control the accuracy of PGM in sorption concentrates by HR CS GFAAS method, it was appropriate to conduct an inter-method comparative experiment. The

Determination of colloidal and dissolved silver in water samples using colorimetric solid-phase extraction.

Science.gov (United States)

Hill, April A; Lipert, Robert J; Porter, Marc D

2010-03-15

The increase in bacterial resistance to antibiotics has led to resurgence in the use of silver as a biocidal agent in applications ranging from washing machine additives to the drinking water treatment system on the International Space Station (ISS). However, growing concerns about the possible toxicity of colloidal silver to bacteria, aquatic organisms and humans have led to recently issued regulations by the US EPA and FDA regarding the usage of silver. As part of an ongoing project, we have developed a rapid, simple method for determining total silver, both ionic (silver(I)) and colloidal, in 0.1-1mg/L aqueous samples, which spans the ISS potable water target of 0.3-0.5mg/L (total silver) and meets the US EPA limit of 0.1mg/L in drinking water. The method is based on colorimetric solid-phase extraction (C-SPE) and involves the extraction of silver(I) from water samples by passage through a solid-phase membrane impregnated with the colorimetric reagent DMABR (5-[4-(dimethylamino)benzylidene]rhodanine). Silver(I) exhaustively reacts with impregnated DMABR to form a colored compound, which is quantified using a handheld diffuse reflectance spectrophotometer. Total silver is determined by first passing the sample through a cartridge containing Oxone, which exhaustively oxidizes colloidal silver to dissolved silver(I). The method, which takes less than 2 min to complete and requires only approximately 1 mL of sample, has been validated through a series of tests, including a comparison with the ICP-MS analysis of a water sample from ISS that contained both silver(I) and colloidal silver. Potential earth-bound applications are also briefly discussed. Copyright (c) 2009 Elsevier B.V. All rights reserved.

Determination of trace impurities in titanium dioxide by direct solid sampling electrothermal atomic absorption spectrometry

Czech Academy of Sciences Publication Activity Database

Vojtková, Blanka; Dočekal, Bohumil

2005-01-01

Roč. 99, S (2005), s489-s491 ISSN 0009-2770. [Meeting on Chemistry and Life /3./. Brno, 20.09.2005-22.09.2005] Institutional research plan: CEZ:AV0Z40310501 Keywords : solid sampling * electrothermal atomic absorption spectrometry * trace analysis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 0.445, year: 2005

Preconcentration of trace elements from high-purity thorium and uranium on Chelex-100 and determination by graphite furnace atomic absorption spectrometry with Zeeman-effect background correction

International Nuclear Information System (INIS)

Raje, Naina; Kayasth, Satish; Asari, T.P.S.; Gangadharan, S.

1994-01-01

Preconcentration of trace impurities from large-sized samples of uranium metal and thorium oxide using a small column of Chelex-100 followed by their determination using graphite furnace atomic absorption spectrometry (GFAAS) is reported. A 0.5-10-g amount of the sample (uranium metal or thorium oxide) was dissolved, complexed with ammonium carbonate and subjected to the ion-exchange procedure. The retained analytes were eluted with 2-4 M nitric acid and brought to a small volume for a final dilution to 10-25 ml for their determination using GFAAS. The validity of the separation procedure and recoveries at μg kg -1 levels was checked by standard addition; the recoveries were >95%

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

DEFF Research Database (Denmark)

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

2008-01-01

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 a large amount...... of soil sample (up to 5 g), 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 4-step sequential...

Liquid-phase microextraction combined with graphite furnace atomic absorption spectrometry: A review.

Science.gov (United States)

de la Calle, Inmaculada; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

2016-09-14

An overview of the combination of liquid-phase microextraction (LPME) techniques with graphite furnace atomic absorption spectrometry (GFAAS) is reported herein. The high sensitivity of GFAAS is significantly enhanced by its association with a variety of miniaturized solvent extraction approaches. LPME-GFAAS thus represents a powerful combination for determination of metals, metalloids and organometallic compounds at (ultra)trace level. Different LPME modes used with GFAAS are briefly described, and the experimental parameters that show an impact in those microextraction processes are discussed. Special attention is paid to those parameters affecting GFAAS analysis. Main issues found when coupling LPME and GFAAS, as well as those strategies reported in the literature to solve them, are summarized. Relevant applications published on the topic so far are included. Copyright © 2016 Elsevier B.V. All rights reserved.

Mercury speciation in environmental solid samples using thermal release technique with atomic absorption detection

Energy Technology Data Exchange (ETDEWEB)

Shuvaeva, Olga V. [Institute of Inorganic Chemistry, Academician Lavrent' ev Prospect 3, 630090 Novosbirsk (Russian Federation)], E-mail: olga@che.nsk.su; Gustaytis, Maria A.; Anoshin, Gennadii N. [Institute of Geology and Mineralogy, Siberian Branch of Russian Academy of Sciences, Koptyug Prospect 3, 630090 Novosibirsk (Russian Federation)

2008-07-28

A sensitive and very simple method for determination of mercury species in solid samples has been developed involving thermal release analysis in combination with atomic absorption (AAS) detection. The method allows determination of mercury(II) chloride, methylmercury and mercury sulfide at the level of 0.70, 0.35 and 0.20 ng with a reproducibility of the results of 14, 25 and 18%, respectively. The accuracy of the developed assay has been estimated using certified reference materials and by comparison of the results with those of an independent method. The method has been applied for Hg species determination in original samples of lake sediments and plankton.

Automated sample preparation station for studying self-diffusion in porous solids with NMR spectroscopy

Science.gov (United States)

Hedin, Niklas; DeMartin, Gregory J.; Reyes, Sebastián C.

2006-03-01

In studies of gas diffusion in porous solids with nuclear magnetic resonance (NMR) spectroscopy the sample preparation procedure becomes very important. An apparatus is presented here that pretreats the sample ex situ and accurately sets the desired pressure and temperature within the NMR tube prior to its introduction in the spectrometer. The gas manifold that supplies the NMR tube is also connected to a microbalance containing another portion of the same sample, which is kept at the same temperature as the sample in the NMR tube. This arrangement permits the simultaneous measurement of the adsorption loading on the sample, which is required for the interpretation of the NMR diffusion experiments. Furthermore, to ensure a good seal of the NMR tube, a hybrid valve design composed of titanium, a Teflon® seat, and Kalrez® O-rings is utilized. A computer controlled algorithm ensures the accuracy and reproducibility of all the procedures, enabling the NMR diffusion experiments to be performed at well controlled conditions of pressure, temperature, and amount of gas adsorbed on the porous sample.

Development of a portable mass spectrometric system for determination of isotopic composition of solid uranium samples using fluorine volatilization. Final report

International Nuclear Information System (INIS)

Loge, G.

1994-01-01

Using hardware and materials supplied by LANL, a prototype quadrupole mass spectrometer system designed for portable field analysis of isotopic composition of solid uranium samples was assembled and tested. The system contained the capability for fluorine volatilization of solid uranium samples with gas introduction, which was successfully tested and demonstrated using 100 mg samples of U 3 O 8 . Determination of precision and accuracy for measuring isotopic composition was performed using isotopic standards. Use with soil samples containing uranium were also attempted. Silicates in the soil forming SiF 4 were found to be a kinetic bottleneck to the formation of UF 6 . This could be avoided by performing some sort of chemical separation as a pre-treatment step, which was demonstrated using nitric acid

Detection of fission fragments using thick samples in contact with solid state nuclear track detectors

International Nuclear Information System (INIS)

Lima, D.A. de; Martins, J.B.; Tavares, O.A.P.

1987-01-01

Whenever use is made of thick samples in contact with solid state nuclear track detectors for determining fission yields, one of the fundamental problems is the evaluation of the effective number of target nuclei which contributes to the fraction of the number of fission events that will be recorded. The evaluation of the effective number of target nuclei which contributes to recorded events is based on the effective thickness of the sample. A method for evaluating effective thickness of thick samples for binary fission modes, is presented. A cross section equation which takes into account all the necessary corrections due to fragment attenuation effects by a thick target for calculation induced fission yields, was obtained. (Author) [pt

The determination of cadmium, lead and vanadium by high resolution ICP-MS in Antarctic snow samples

Energy Technology Data Exchange (ETDEWEB)

Lanza, F. [Joh. Gutenberg Univ., Mainz (Germany). Inst. fuer Anorganische und Analytische Chemie; Trincherini, P. [European Union Joint Research Centre, Ispra, VA (Italy). Inst. of Environment

2000-02-01

Double focusing ICP-MS was successfully used in this research for the direct determination of the cadmium, lead and vanadium content of a set of Antarctic samples collected during the 11. Italian Expedition to Antarctica. For cadmium and lead measurements the low resolution mode was chosen since it ensured the highest ion sensitivity and it allowed the highest detection limits to be attained; in the case of vanadium the high resolution mode was used to solve the isobaric interference. As far as vanadium and cadmium are concerned by GFAAS coupled with different preconcentration procedures. The vanadium, cadmium and lead content measured in a riverine water reference material (SRLS-3) was found in agreement with the certified values. [Italian] Si e' utilizzato uno spettrometro ICP-MS a doppia focalizzazione per la determinazione diretta di cadmio, piombo e vanadio in una serie di campioni di neve antartica superficiale raccolta durante l'undicesima spedizione italiana in Antartide. Per le determinazioni di cadmio e piombo si e' scelta la procedura a bassa risoluzione, che ha garantito la piu' elevata sensibilita' ed ha permesso di ottenere limiti di determinazione migliori; nel caso del vanadio si e' utilizzata la procedura ad alta risoluzione che ha permesso di risolvere problemi di interferenza isobarica. Per quanto riguarda cadmio e vanadio, i risultati delle determinazioni mediante ICP-MS sono risultati in buon accordo con quelli ottenuti mediante GFAAS accoppiata a diverse procedure di preconcentrazione. Il contenuto di cadmio, piombo e vanadio misurato con le procedure sviluppate in un campione certificato di acqua di fiume (SRLS-3) e' risultato in accordo con i valori certificati.

Reimiep 87. An interlaboratory U-235 enrichment determination by gamma measurement on solid UF6 sample

International Nuclear Information System (INIS)

Aparo, M.; Cresti, P.

1988-01-01

Gamma spectroscopy technique, based on the measurement of U 235 186 KeV flux, is now currently used for the determination of Uranium enrichment in different material of nuclear fuel cycle, namely: Uranium metallic, UO 2 pellets, UF 6 liquid or solid. The present paper describes the use of such a technique and the obtained results in determining the U 235 /U atomic isotopic abundance on a certified UF 6 solid sample. The measurements have been carried out in the frame work of the partecipation to the ''UF 6 Interlaboratory Measurements Evaluation Programme'' organized by CBNM/Geel with the support of the ESARDA (European Safeguards Research and Development Association)

The indicating FTA elute cartridge a solid sample carrier to detect high-risk HPV and high-grade cervical lesions

NARCIS (Netherlands)

Bie, R.P. de; Schmeink, C.E.; Bakkers, J.M.J.E.; Snijders, P.J.L.M.; Quint, W.G.V.; Massuger, L.F.A.G.; Bekkers, R.L.M.; Melchers, W.J.G.

2011-01-01

The clinically validated high-risk human papillomavirus (hrHPV) Hybrid Capture 2 (HC2) and GP5+/6+-PCR assays were analyzed on an Indicating FTA Elute cartridge (FTA cartridge). The FTA cartridge is a solid dry carrier that allows safe transport of cervical samples. FTA cartridge samples were

Calibration of track detectors and measurement of radon exhalation rate from solid samples

International Nuclear Information System (INIS)

Singh, Ajay Kumar; Jojo, P.J.; Prasad, Rajendra; Khan, A.J.; Ramachandran, T.V.

1997-01-01

CR-39 and LR-115 type II track detectors to be used for radon exhalation measurements have been calibrated. The configurations fitted with detectors in Can technique in the open cup mode are cylindrical plastic cup (PC) and conical plastic cup (CPC). The experiment was performed in radon exposure chamber having monodisperse aerosols of 0.2 μm size, to find the relationship between track density and the radon concentration. The calibration factors for PC and CPC type dosimeters with LR-115 type II detector were found to be 0.056 and 0.083 tracks cm -2 d -1 (Bqm -3 ) -1 respectively, while with CR-39 detector the values were 0.149 and 0.150 tracks cm -2 d -1 (Bq m -3 ) -1 . Employing the Can technique, measurements of exhalation rates from solid samples used as construction materials, are undertaken. Radon exhalation rate is found to be minimum in cement samples while in fly ash it is not enhanced as compared to coal samples. (author)

Development of mixed-waste analysis capability for graphite furnace atomic absorption spectrophotometry

International Nuclear Information System (INIS)

Bass, D.A.; TenKate, L.B.; Wroblewski, A.

1995-03-01

Graphite furnace atomic absorption spectrophotometer (GFAAS) are typically configured with ventilation to capture potentially toxic and corrosive gases emitted from the vaporization of sample aliquots. When radioactive elements are present, additional concerns (such as meeting safety guidelines and ALARA principles) must be addressed. This report describes a modification to a GFAAS that provides additional containment of vaporized sample aliquots. The modification was found to increase containment by a factor of 80, given expected operating conditions. The use of the modification allows more mixed-waste samples to be analyzed, permits higher levels of radioactive samples to be analyzed, or exposes the analyst to less airborne radioactivity. The containment apparatus was attached to a Perkin-Elmer Zeeman 5000 spectrophotometer for analysis of mixed-waste samples; however, it could also be used on other systems and in other applications where greater containment of vaporized material is desired

Application of direct solid sample analysis for the determination of chlorine in biological materials using electrothermal vaporization inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Santos de Gois, Jefferson; Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); Welz, Bernhard [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); INCT de Energia e Ambiente do CNPq (Brazil); Borges, Daniel L.G., E-mail: daniel.borges@ufsc.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); INCT de Energia e Ambiente do CNPq (Brazil)

2015-03-01

This work describes a methodology developed to carry out Cl determination in biological materials using electrothermal vaporization inductively coupled plasma mass spectrometry and direct solid sample analysis. The solid samples were directly weighed into graphite ‘cups’ and inserted into the graphite furnace. The RF power and the carrier gas flow rate were optimized at 1300 W and 0.7 L min{sup −1}, respectively. Calibration could be carried out using aqueous standard solutions with pre-dried modifiers (Pd + Nd or Pd + Ca) or using solid certified reference materials with the same pre-dried modifiers or without the use of modifiers. The limit of quantification was determined as 5 μg g{sup −1} under optimized conditions and the Cl concentration was determined in five certified reference materials with certified concentrations for Cl, in addition to three certified reference materials, for which certified values for Cl were unavailable; in the latter case, the results were compared with those obtained using high-resolution continuum source molecular absorption spectrometry. Good agreement at a 95% statistical confidence level was achieved between determined and certified or reference values. - Highlights: • Direct determination of chlorine in solid biological materials is described for the first time using ICP-MS. • Calibration against aqueous standards is feasible. • The method is accurate and sensitive, regardless of the composition of the solid sample.

Comparison of the solid-phase extraction efficiency of a bounded and an included cyclodextrin-silica microporous composite for polycyclic aromatic hydrocarbons determination in water samples.

Science.gov (United States)

Mauri-Aucejo, Adela; Amorós, Pedro; Moragues, Alaina; Guillem, Carmen; Belenguer-Sapiña, Carolina

2016-08-15

Solid-phase extraction is one of the most important techniques for sample purification and concentration. A wide variety of solid phases have been used for sample preparation over time. In this work, the efficiency of a new kind of solid-phase extraction adsorbent, which is a microporous material made from modified cyclodextrin bounded to a silica network, is evaluated through an analytical method which combines solid-phase extraction with high-performance liquid chromatography to determine polycyclic aromatic hydrocarbons in water samples. Several parameters that affected the analytes recovery, such as the amount of solid phase, the nature and volume of the eluent or the sample volume and concentration influence have been evaluated. The experimental results indicate that the material possesses adsorption ability to the tested polycyclic aromatic hydrocarbons. Under the optimum conditions, the quantification limits of the method were in the range of 0.09-2.4μgL(-1) and fine linear correlations between peak height and concentration were found around 1.3-70μgL(-1). The method has good repeatability and reproducibility, with coefficients of variation under 8%. Due to the concentration results, this material may represent an alternative for trace analysis of polycyclic aromatic hydrocarbons in water trough solid-phase extraction. Copyright © 2016 Elsevier B.V. All rights reserved.

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

DEFF Research Database (Denmark)

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

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......Accummulation of metal ions in different compartments of the biosphere and their possible mobilization under changing environmental conditions induce a pertubation of the ecosystem and may cause adverse health effects. Nowadays, it is widely recognized that the information on total content...... the ecotoxicological significance of metal ions in solid environmental samples. The background of end-over-end fractionation for releasing metal species bound to particular soil phases is initially discussed, its relevant features and limitations being thoroughly described. However, taking into account that naturally...

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.

EPA Method 3135.2I: Cyanide, Total and Amenable in Aqueous and Solid Samples Automated Colorimetric With Manual Digestion

Science.gov (United States)

This method describes procedures for preparation and analysis of solid, water and wipe samples for detection and measurement of cyanide amendable to chlorination using acid digestion and spectrophotometry.

Solvent-assisted dispersive solid-phase extraction: A sample preparation method for trace detection of diazinon in urine and environmental water samples.

Science.gov (United States)

Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

2016-09-02

In this research, a sample preparation method termed solvent-assisted dispersive solid-phase extraction (SA-DSPE) was applied. The used sample preparation method was based on the dispersion of the sorbent into the aqueous sample to maximize the interaction surface. In this approach, the dispersion of the sorbent at a very low milligram level was received 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 diazinon, the cloudy solution was centrifuged and diazinon in the sediment phase dissolved in ethanol and determined by gas chromatography-flame ionization detector. Under the optimized conditions (pH of solution=7.0, Sorbent: benzophenone, 2%, Disperser solvent: ethanol, 500μL, Centrifuge: centrifuged at 4000rpm for 3min), the method detection limit for diazinon was 0.2, 0.3, 0.3 and 0.3μgL(-1) for distilled water, lake water, waste water and urine sample, respectively. Furthermore, the pre-concentration factor was 363.8, 356.1, 360.7 and 353.38 in distilled water, waste water, lake water and urine sample, respectively. SA-DSPE was successfully used for trace monitoring of diazinon in urine, lake and waste water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of cobalt in biological samples by line-source and high-resolution continuum source graphite furnace atomic absorption spectrometry using solid sampling or alkaline treatment

International Nuclear Information System (INIS)

Ribeiro, Anderson Schwingel; Vieira, Mariana Antunes; Furtado da Silva, Alessandra; Borges, Daniel L. Gallindo; Welz, Bernhard; Heitmann, Uwe; Curtius, Adilson Jose

2005-01-01

Two procedures for the determination of Co in biological samples by graphite furnace atomic absorption spectrometry (GF AAS) were compared: solid sampling (SS) and alkaline treatment with tetramethylammonium hydroxide (TMAH) using two different instruments for the investigation: a conventional line-source (LS) atomic absorption spectrometer and a prototype high-resolution continuum source atomic absorption spectrometer. For the direct introduction of the solid samples, certified reference materials (CRM) were ground to a particle size ≤50 μm. Alkaline treatment was carried out by placing about 250 mg of the sample in polypropylene flasks, adding 2 mL of 25% m/v tetramethylammonium hydroxide and de-ionized water. Due to its unique capacity of providing a 3-D spectral plot, a high-resolution continuum source (HR-CS) graphite furnace atomic absorption spectrometry was used as a tool to evaluate potential spectral interferences, including background absorption for both sample introduction procedures, revealing that a continuous background preceded the atomic signal for pyrolysis temperatures lower than 700 deg. C. Molecular absorption bands with pronounced rotational fine structure appeared for atomization temperatures >1800 deg. C probably as a consequence of the formation of PO. After optimization had been carried out using high resolution continuum source atomic absorption spectrometry, the optimized conditions were adopted also for line-source atomic absorption spectrometry. Six biological certified reference materials were analyzed, with calibration against aqueous standards, resulting in agreement with the certified values (according to the t-test for a 95% confidence level) and in detection limits as low as 5 ng g -1

Stir-bar supported micro-solid-phase extraction for the determination of polychlorinated biphenyl congeners in serum samples.

Science.gov (United States)

Sajid, Muhammad; Basheer, Chanbasha

2016-07-15

In present work, a new configuration of micro-solid phase extraction was introduced and termed as stir-bar supported micro-solid-phase extraction (SB-μ-SPE). A tiny stir-bar was packed inside the porous polypropylene membrane along with sorbent material and the edges of membrane sheet were heat sealed to secure the contents. The packing of stir-bar inside the μ-SPE device does not allow the device to stick with the wall or any corner of the sample vial during extraction, which is, however, a frequent observation in routine μ-SPE. Moreover, it enhances effective surface area of the sorbent exposed to sample solution through continuous agitation (motion and rotation). It also completely immerses the SB-μ-SPE device in the sample solution even for non-polar sorbents. Polychlorinated biphenyls (PCBs) were selected as model compounds and the method performance was evaluated in human serum samples. After extraction, samples were analyzed by gas chromatography mass spectrometry (GC-MS). The factors that affect extraction efficiency of SB-μ-SPE were optimized. Under optimum conditions, a good linearity (0.1-100ngmL(-1)) with coefficients of determinations ranging from 0.9868 to 0.9992 was obtained. Limits of detections were ranged between 0.003 and 0.047ngmL(-1). Acceptable values for inter-day (3.2-9.1%) and intra-day (3.1-7.2%) relative standard deviations were obtained. The optimized method was successfully applied to determine the concentration of PCB congeners in human serum samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of Sr-90 in environmental samples using solid phase extraction disk

International Nuclear Information System (INIS)

Zal U'yun Wan Mahmood

2002-01-01

A method is described for determination of Sr-90 in environmental samples using solid phase extraction disk (Empore TM Strontium Rad Disk) and GM counter. To determine the optimum condition for capacity of Empore TM Strontium Rad Disk, its characterization studies such as the effects Sr content, acidity (molarity) of acids, presence of Ca 2+ and other major ions (Na + , Mg 2+ etc), influence of interference (Pb and Bi) and others were carried out. An optimized the using of Empore TM Strontium Rad Disk for determination of Sr-90 was validated by application to environmental samples. Quantitative recoveries above 95%for Sr (stable) were recorded in 6M HCl condition. Typical environmental samples may contain an assortment of anionic and cationic species, but in general, Empore TM Strontium Rad Disk has enough capacity to effectively separate Sr for wide variety of aqueous solutions. Sr recovery in a matrix-free or the content of matrix less than 300 mg/sample is typically greater than 99% is reported in this research work. In particular, sample, which may contain interference such as Pb and Bi would require an addition separation step before processing to ensure an accurate measurement of Sr. In this research work, radiotracer 85 Sr was used to monitor the behavior of Sr and calculation its recovery. For analytical methods that can count Y-90, the Sr-90 activity/concentration in environmental sample was calculated. The concentration of Sr-90 in ash sample (Quality Controled Sample) of 276 ± 18 Bq/kg ash was determined from Y-90 activity. The relative percent difference of 1.1% was achievable for Empore TM Sr-Rad Disk methods when compared to the conventional method (fumed-HNO 3 method) - 279 ± 11 Bq/kg ash. (Author)

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.

Chromium speciation in environmental samples using a solid phase spectrophotometric method

Science.gov (United States)

Amin, Alaa S.; Kassem, Mohammed A.

2012-10-01

A solid phase extraction technique is proposed for preconcentration and speciation of chromium in natural waters using spectrophotometric analysis. The procedure is based on sorption of chromium(III) as 4-(2-benzothiazolylazo)2,2'-biphenyldiol complex on dextran-type anion-exchange gel (Sephadex DEAE A-25). After reduction of Cr(VI) by 0.5 ml of 96% concentrated H2SO4 and ethanol, the system was applied to the total chromium. The concentration of Cr(VI) was calculated as the difference between the total Cr and the Cr(III) content. The influences of some analytical parameters such as: pH of the aqueous solution, amounts of 4-(2-benzothiazolylazo)2,2'-biphenyldiol (BTABD), and sample volumes were investigated. The absorbance of the gel, at 628 and 750 nm, packed in a 1.0 mm cell, is measured directly. The molar absorptivities were found to be 2.11 × 107 and 3.90 × 107 L mol-1 cm-1 for 500 and 1000 ml, respectively. Calibration is linear over the range 0.05-1.45 μg L-1 with RSD of <1.85% (n = 8.0). Using 35 mg exchanger, the detection and quantification limits were 13 and 44 ng L-1 for 500 ml sample, whereas for 1000 ml sample were 8.0 and 27 ng L-1, respectively. Increasing the sample volume can enhance the sensitivity. No considerable interferences have been observed from other investigated anions and cations on the chromium speciation. The proposed method was applied to the speciation of chromium in natural waters and total chromium preconcentration in microwave digested tobacco, coffee, tea, and soil samples. The results were simultaneously compared with those obtained using an ET AAS method, whereby the validity of the method has been tested.

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.

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 solid recovered fuel produced meets the European Union standard requirements and can be classified with the class code: Net heating value (3); chlorine (1); mercury (1).

Glove box adaptation, installation and commissioning of an assembled modular type atomic absorption unit with GF atomizer

International Nuclear Information System (INIS)

Gupta, Santosh Kumar; Thulasidas, S.K.; Goyal, Neelam; Godbole, S.V.

2013-09-01

The report describes glove box adaptation of an in-house developed AAS unit with GF as atomization source for determination of trace metallic elements in Pu bearing samples. In order to replace the old Varian Techtron GF-AAS which was utilized for analysis of Pu bearing samples for the last thirty seven years, and as of late was giving too many practical problems, a new GF-AAS was designed and reassembled. The original compact flame AAS unit available with M/s. Thermo Fisher India Pvt. Ltd, Nashik, was converted into separated modular unit viz. Hollow Cathode Lamp unit, Atomizer unit and Monochromator - Detector - Readout unit. In addition, these modular units were modified with respect to their dimensions so as to enable their use with existing glove box facility developed earlier in 1980 for glove box incorporation. These units were separated from each other at their factory site so as to enable us to incorporate atomizer unit alone in the glove box. Glove box adapted GF-AAS is essential for Radiochemistry Division to provide analytical services to Chemical Quality Control of Pu bearing nuclear and related materials and also as an analytical support to the R and D activities of the Radiochemistry Division, BARC. (author)

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...... electrolytic or aqueous leaching, on-line dialysis/microdialysis, in-line filtration, and pervaporation-based procedures have been successfully implemented in continuous flow/flow injection systems. In this communication, the new generation of flow analysis, including sequential injection, multicommutated flow.......g., soils, sediments, sludges), and thus, ascertaining the potential mobility, bioavailability and eventual impact of anthropogenic elements on biota [2]. In this context, the principles of sequential injection-microcolumn extraction (SI-MCE) for dynamic fractionation are explained in detail along...

Preparation of solid-state samples of a transition metal coordination compound for synchrotron radiation photoemission studies

CERN Document Server

Crotti, C; Celestino, T; Fontana, S

2003-01-01

The aim of this research was to identify a sample preparation method suitable for the study of transition metal complexes by photoemission spectroscopy with synchrotron radiation as the X-ray source, even in the case where the compound is not evaporable. Solid-phase samples of W(CO) sub 4 (dppe) [dppe=1,2-bis(diphenylphosphino)ethane] were prepared according to different methods and their synchrotron radiation XPS spectra measured. The spectra acquired from samples prepared by spin coating show core level peaks only slightly broader than the spectrum recorded from UHV evaporated samples. Moreover, for these samples the reproducibility of the binding energy values is excellent. The dependence of the spin coating technique on parameters such as solvent and solution concentration, spinning speed and support material was studied. The same preparation method also allowed the acquisition of valence band spectra, the main peaks of which were clearly resolved. The results suggest that use of the spin coating techniqu...

Liquid-solid extraction of uranium (VI) with TOPO - molten naphthalene and determination by laser fluorimetry in geological samples

International Nuclear Information System (INIS)

Kumar, Sanjay; Krishnakumar, M.; Patwardhan, A.A.

2007-01-01

A simple, rapid, sensitive, cost-effective and efficient method for separation of uranium using tri-n-octylphosphine oxide (TOPO)-molten naphthalene as solid phase extractant and its determination by laser fluorimetry in geological samples (rock, soil, sediment) was developed. Under optimum conditions, using 50 mg TOPO and 100 mg naphthalene, 50 - 5000 ng of uranium in 10 ml sample solution (3% (v/v) HNO 3 ) could be extracted quantitatively. The extracted uranium was stripped using tetra sodium pyrophosphate (5% (v/v) solution, pH adjusted to 7.0 with H 3 PO 4 ) and determined by laser fluorimetry. The influence of different acid concentrations, the amount of solid phase extractant, sample volumes, different stripping reagents, their volumes and effect of foreign ions on the extraction and determination of uranium (VI) were investigated. Synthetic samples of varying concentration as regards uranium were prepared and analysed. Recoveries ranging from 90% to 105% were obtained. The method was validated by analyzing four certified reference materials namely, BL-5, DH-1a, SY-2, SY-3 and the values obtained for uranium agreed well with the certified values. The method was also applied to the determination of uranium in geological samples (rock, soil and sediment) by laser fluorimetry and the results obtained compared favorably with those obtained from the pellet fluorimetry method. Following the proposed method, determination limit for uranium was found to be 1 μg/g with RSD ± 10%. (author)

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

Science.gov (United States)

Flórián, K; Hassler, J; Förster, O

2001-12-01

The validation procedure based on ISO 17025 standard has been used to study and illustrate both the longterm 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.

Monitoring and Method development of Hg in Istanbul Airborne Particulates by Solid Sampling Continuum Source-High Resolution Electrothermal Atomic Absorption Spectromerty

Directory of Open Access Journals (Sweden)

Soydemir E.

2014-07-01

Full Text Available In this work, a method has been developed and monitoring for the determination of mercury in PM2.5 airborne particulates by solid sampling high-resolution continuum source electrothermal atomic absorption spectrometry. The PM2.5 airborne particulates were collected on quartz filters using high volume samplers (500 L/min in Istanbul (Turkey for 96 hours every month in one year. At first, experimental conditions as well as the validation tests were optimized using collected filter. For this purpose, the effects of atomization temperature, amount of sample intoduced in to the furnace, addition of acids and/or KMnO4 on the sample, covering of graphite tube and platform or using of Ag nanoparticulates, Au nanoparticulates, and Pd solutions on the accuracy and precision were investigated. After optimization of the experimental conditions, the mercury concentrations were determined in the collected filter. The filters with PM2.5 airborne particulates were dried, divided into small fine particles and then Hg concentrations were determined directly. In order to eliminate any error due to the sensitivity difference between aqueous standards and solid samples, the quantification was performed using solid calibrants. The limit of detection, based on three times the standard deviations for ten atomizations of an unused filter, was 30 ng/g. The Hg content was dependent on the sampling site, season etc, ranging from samples, addition of AuNPs, AgNPs and Pd solution for amalgamation effects on the recoveries were investigated. The results were compared using statistical tests.

Assessment of Metaborate Fusion for the Rapid Dissolution of Solid Samples: Suitability with the Northstar ARSIIe

Science.gov (United States)

2016-07-01

5 Table 3. Residual Silicates avec Flocculation in Glass Beaker or Polyethylene Cone ................ 8 Table 4...is formed. Since the concentration of silicates in soil or sediment is high (up to 70-75% in silicon dioxide ( SiO2 ) in some cases), the condensation...flux, for the fusion of acidic samples such as solids containing a significant portion of SiO2 . Conversely, lithium tetraborate, an acidic flux, will

In-situ pre-concentration through repeated sampling and pyrolysis for ultrasensitive determination of thallium in drinking water by electrothermal atomic absorption spectrometry.

Science.gov (United States)

Liu, Liwei; Zheng, Huaili; Xu, Bincheng; Xiao, Lang; Chigan, Yong; Zhangluo, Yilan

2018-03-01

In this paper, a procedure for in-situ pre-concentration in graphite furnace by repeated sampling and pyrolysis is proposed for the determination of ultra-trace thallium in drinking water by graphite furnace atomic absorption spectrometry (GF-AAS). Without any other laborious enrichment processes that routinely result in analyte loss and contamination, thallium was directly concentrated in the graphite furnace automatically and subsequently subject to analysis. The effects of several key factors, such as the temperature for pyrolysis and atomization, the chemical modifier, and the repeated sampling times were investigated. Under the optimized conditions, a limit of detection of 0.01µgL -1 was obtained, which fulfilled thallium determination in drinking water by GB 5749-2006 regulated by China. Successful analysis of thallium in certified water samples and drinking water samples was demonstrated, with analytical results in good agreement with the certified values and those by inductively coupled plasma mass spectrometry (ICP-MS), respectively. Routine spike-recovery tests with randomly selected drinking water samples showed satisfactory results of 80-96%. The proposed method is simple and sensitive for screening of ultra-trace thallium in drinking water samples. Copyright © 2017. Published by Elsevier B.V.

System and process for dissolution of solids

Science.gov (United States)

Liezers, Martin; Farmer, III, Orville T.

2017-10-10

A system and process are disclosed for dissolution of solids and "difficult-to-dissolve" solids. A solid sample may be ablated in an ablation device to generate nanoscale particles. Nanoparticles may then swept into a coupled plasma device operating at atmospheric pressure where the solid nanoparticles are atomized. The plasma exhaust may be delivered directly into an aqueous fluid to form a solution containing the atomized and dissolved solids. The composition of the resulting solution reflects the composition of the original solid sample.

Interfering removal in samples with high amounts of dissolved solids for the determination of arsenic and selenium by TXRF

International Nuclear Information System (INIS)

Menegario, Amauri A.; Gomes, Ana Carla F.; Pellegrinotti, Daniel C.; Gine, Maria F.; Krug, Francisco J.; Nascimento Filho, Virgilio F.

2002-01-01

A matrix separation flow system coupled with total reflection X-ray fluorescence (TXRF) is proposed to remove Ca ++ , Mg ++ , Na + and K + major cations from samples containing high amounts of totally dissolved solids, using solid-liquid phases in flow system. This system is assembled with a 1.25 mL column of AG50W-X8 resin (in protonated form) and manual commutator, allowed the separation, addition of internal standard and subsequently a 40 μL aliquot of the eluate was deposited in the reflector support, dried in a furnace for 12 hours at 60 ± 5 deg C and analysed by TXRF. All the procedure is carried out in about 90 s and 0.5 mL of sample are required. The proposed approach was applied for determination of As and Se in plant material and sea water samples. When comparing with direct analysis (without separation), a reduction of 2 to 6 times on the limits of detection for these elements was attained. The accuracy of this methodology was satisfactory for As and Se in sea water and Se in rice certified samples. This procedure could be also used for Pb interference removal in the determination of As by X-ray fluorescence. (author)

Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD) and Dispersive Solid Phase Extraction (d-SPE) of Plant Samples

Science.gov (United States)

Sowa, Ireneusz; Wójciak-Kosior, Magdalena; Strzemski, Maciej; Sawicki, Jan; Staniak, Michał; Dresler, Sławomir; Szwerc, Wojciech; Mołdoch, Jarosław; Latalski, Michał

2018-01-01

Polyaniline (PANI) is one of the best known conductive polymers with multiple applications. Recently, it was also used in separation techniques, mostly as a component of composites for solid-phase microextraction (SPME). In the present paper, sorbent obtained by in situ polymerization of aniline directly on silica gel particles (Si-PANI) was used for dispersive solid phase extraction (d-SPE) and matrix solid–phase extraction (MSPD). The efficiency of both techniques was evaluated with the use of high performance liquid chromatography with diode array detection (HPLC-DAD) quantitative analysis. The quality of the sorbent was verified by Raman spectroscopy and microscopy combined with automated procedure using computer image analysis. For extraction experiments, triterpenes were chosen as model compounds. The optimal conditions were as follows: protonated Si-PANI impregnated with water, 160/1 sorbent/analyte ratio, 3 min of extraction time, 4 min of desorption time and methanolic solution of ammonia for elution of analytes. The proposed procedure was successfully used for pretreatment of plant samples. PMID:29565297

Selective solid-phase extraction of Ni(II) by an ion-imprinted polymer from water samples

International Nuclear Information System (INIS)

Saraji, Mohammad; Yousefi, Hamideh

2009-01-01

A new ion-imprinted polymer (IIP) material was synthesized by copolymerization of 4-vinylpyridine as monomer, ethyleneglycoldimethacrylate as crosslinking agent and 2,2'-azobis-sobutyronitrile as initiator in the presence of Ni-dithizone complex. The IIP was used as sorbent in a solid-phase extraction column. The effects of sampling volume, elution conditions, sample pH and sample flow rate on the extraction of Ni ions form water samples were studied. The maximum adsorption capacity and the relative selectivity coefficients of imprinted polymer for Ni(II)/Co(II), Ni(II)/Cu(II) and Ni(II)/Cd(II) were calculated. Compared with non-imprinted polymer particles, the IIP had higher selectivity for Ni(II). The relative selectivity factor (α r ) values of Ni(II)/Co(II), Ni(II)/Cu(II) and Ni(II)/Cd(II) were 21.6, 54.3, and 22.7, respectively, which are greater than 1. The relative standard deviation of the five replicate determinations of Ni(II) was 3.4%. The detection limit for 150 mL of sample was 1.6 μg L -1 using flame atomic absorption spectrometry. The developed method was successfully applied to the determination of trace nickel in water samples with satisfactory results.

Solid phase extraction for sample preparation in trace analysis of ionogenic compounds by capillary isotachophoresis

International Nuclear Information System (INIS)

Hutta, M.; Kaniansky, D.; Simunicova, E.; Zelenska, V.; Madajova, V.; Siskova, A.

1992-01-01

Various sorbents recommended for solid phase extraction (SPE) in sample preparation procedures were studied for use in combination with capillary isotachophoresis (ITP). They were very efficient in achieving trace concentration levels (low ppb, i.e., low parts per 10 9 ) for different types of ITP analytes present in environmental and biological matrices. A macroporous carbon sorbent was convenient for sample preparation in ITP analysis of short chain fatty acids (C 4 -C 9 ) in drinking water. Chelating sorbents based on hydroxyalkyl methacrylate matrix with salicylate, thioglycolate and 8-hydroxyquinolinate functionalities were found to be very suitable for preconcentration of heavy metals with an inherent sample clean-up. An octadecyl-bonded silica sorbent enabled in ITP a photometric detection of γ-aminobutyrate (labeled with a 2,4,6-trinitrophenyl group) at concentrations considerably lower than required for the determination of this amino acid in cerebrospinal fluid (∼5*10 -8 mol/l). (author) 34 refs.; 3 figs.; 1 tab

Hexagonal boron nitride nanosheets as adsorbents for solid-phase extraction of polychlorinated biphenyls from water samples

Energy Technology Data Exchange (ETDEWEB)

Jia, Shiliang; Wang, Zhenhua; Ding, Ning [Key Laboratory for Applied Technology of Sophisticated Analytical Instruments, Shandong Academy of Sciences, Jinan, Shandong (China); Elaine Wong, Y.-L. [Department of Chemistry, The Chinese University of Hong Kong, Hong Kong Special Administrative Region (Hong Kong); Chen, Xiangfeng, E-mail: xiangfchensdas@163.com [Key Laboratory for Applied Technology of Sophisticated Analytical Instruments, Shandong Academy of Sciences, Jinan, Shandong (China); Department of Chemistry, The Chinese University of Hong Kong, Hong Kong Special Administrative Region (Hong Kong); Qiu, Guangyu [Department of Physics and Materials Science, City University of Hong Kong, Hong Kong Special Administrative Region (Hong Kong); Dominic Chan, T.-W., E-mail: twdchan@cuhk.edu.hk [Department of Chemistry, The Chinese University of Hong Kong, Hong Kong Special Administrative Region (Hong Kong)

2016-09-14

The adsorptive potential of hexagonal boron nitride nanosheets (h-BNNSs) for solid-phase extraction (SPE) of pollutants was investigated for the first time. Seven indicators of polychlorinated biphenyls (PCBs) were selected as target analytes. The adsorption of PCBs on the surface of the h-BNNSs in water was simulated by the density functional theory and molecular dynamics. The simulation results indicated that the PCBs are adsorbed on the surface by π–π, hydrophobic, and electrostatic interactions. The PCBs were extracted with an h-BNNS-packed SPE cartridge, and eluted by dichloromethane. Gas chromatography–tandem mass spectrometry working in the multiple reaction monitor mode was used for the sample quantification. The effect of extraction parameters, including the flow rate, pH value, breakthrough volume, and the ionic strength, were investigated. Under the optimal working conditions, the developed method showed low limits of detection (0.24–0.50 ng L{sup −1}; signal-to-noise ratio = 3:1), low limits of quantification (0.79–1.56 ng L{sup −1}; signal-to-noise ratio = 10:1), satisfactory linearity (r > 0.99) within the concentration range of 2–1000 ng L{sup −1}, and good precision (relative standard deviation < 12%). The PCBs concentration in environmental water samples was determined by the developed method. This results demonstrate that h-BNNSs have high analytical potential in the enrichment of pollutants. - Highlights: • The hexagonal boron nitride nanosheets were synthesized. • The nanosheets were used as adsorbent for solid-phase extraction. • The h-BN demonstrates remarkable adsorption of PCBs from water samples. • The method was successfully applied in determination of PCBs in water samples.

Development of Solid Ceramic Dosimeters for the Time-Integrative Passive Sampling of Volatile Organic Compounds in Waters.

Science.gov (United States)

Bonifacio, Riza Gabriela; Nam, Go-Un; Eom, In-Yong; Hong, Yong-Seok

2017-11-07

Time-integrative passive sampling of volatile organic compounds (VOCs) in water can now be accomplished using a solid ceramic dosimeter. A nonporous ceramic, which excludes the permeation of water, allowing only gas-phase diffusion of VOCs into the resin inside the dosimeter, effectively captured the VOCs. The mass accumulation of 11 VOCs linearly increased with time over a wide range of aqueous-phase concentrations (16.9 to 1100 μg L -1 ), and the linearity was dependent upon the Henry's constant (H). The average diffusivity of the VOCs in the solid ceramic was 1.46 × 10 -10 m 2 s -1 at 25 °C, which was 4 orders of magnitude lower than that in air (8.09 × 10 -6 m 2 s -1 ). This value was 60% greater than that in the water-permeable porous ceramic (0.92 × 10 -10 m 2 s -1 ), suggesting that its mass accumulation could be more effective than that of porous ceramic dosimeters. The mass accumulation of the VOCs in the solid ceramic dosimeter increased in the presence of salt (≥0.1 M) and with increasing temperature (4 to 40 °C) but varied only slightly with dissolved organic matter concentration. The solid ceramic dosimeter was suitable for the field testing and measurement of time-weighted average concentrations of VOC-contaminated waters.

Preconcentration and separation of nickel, copper and cobalt using solid phase extraction and their determination in some real samples

International Nuclear Information System (INIS)

Ghaedi, M.; Ahmadi, F.; Soylak, M.

2007-01-01

A solid phase extraction method has been developed to separate and concentrate trace amounts of nickel, cobalt and copper ions from aqueous samples for the measurement by flame atomic absorption spectrometry. By the passage of aqueous samples through activated carbon modified by dithioxamide (rubeanic acid) (DTO), Ni 2+ , Cu 2+ and Co 2+ ions adsorb quantitatively. The recoveries of analytes at pH 5.5 with 500 mg solid phase were greater than 95% without interference from alkaline, earth alkaline and some metal ions. The enrichment factor was 330. The detection limits by three sigma were 0.50 μg L -1 for copper, 0.75 μg L -1 for nickel and 0.80 μg L -1 for cobalt. The loading capacity was 0.56 mg g -1 for Ni 2+ , 0.50 mg g -1 for Cu 2+ and 0.47 mg g -1 for Co 2+ . The presented procedure was applied to the determination of analytes in tap, river and sea waters, vegetable, soil and blood samples with successfully results (recoveries greater than 95%, R.S.D. lower than 2% for n = 3)

Preconcentration and separation of nickel, copper and cobalt using solid phase extraction and their determination in some real samples

Energy Technology Data Exchange (ETDEWEB)

Ghaedi, M. [Chemistry Department, University of Yasouj, Yasouj 75914-353 (Iran, Islamic Republic of)]. E-mail: m_ghaedi@mail.yu.ac.ir; Ahmadi, F. [Gachsaran Azad University, Gachsaran (Iran, Islamic Republic of); Soylak, M. [Chemistry Department, University of Erciyes, 38039 Kayseri (Turkey)

2007-08-17

A solid phase extraction method has been developed to separate and concentrate trace amounts of nickel, cobalt and copper ions from aqueous samples for the measurement by flame atomic absorption spectrometry. By the passage of aqueous samples through activated carbon modified by dithioxamide (rubeanic acid) (DTO), Ni{sup 2+}, Cu{sup 2+} and Co{sup 2+} ions adsorb quantitatively. The recoveries of analytes at pH 5.5 with 500 mg solid phase were greater than 95% without interference from alkaline, earth alkaline and some metal ions. The enrichment factor was 330. The detection limits by three sigma were 0.50 {mu}g L{sup -1} for copper, 0.75 {mu}g L{sup -1} for nickel and 0.80 {mu}g L{sup -1} for cobalt. The loading capacity was 0.56 mg g{sup -1} for Ni{sup 2+}, 0.50 mg g{sup -1} for Cu{sup 2+} and 0.47 mg g{sup -1} for Co{sup 2+}. The presented procedure was applied to the determination of analytes in tap, river and sea waters, vegetable, soil and blood samples with successfully results (recoveries greater than 95%, R.S.D. lower than 2% for n = 3)

Preconcentration and separation of nickel, copper and cobalt using solid phase extraction and their determination in some real samples.

Science.gov (United States)

Ghaedi, M; Ahmadi, F; Soylak, M

2007-08-17

A solid phase extraction method has been developed to separate and concentrate trace amounts of nickel, cobalt and copper ions from aqueous samples for the measurement by flame atomic absorption spectrometry. By the passage of aqueous samples through activated carbon modified by dithioxamide (rubeanic acid) (DTO), Ni2+, Cu2+ and Co2+ ions adsorb quantitatively. The recoveries of analytes at pH 5.5 with 500 mg solid phase were greater than 95% without interference from alkaline, earth alkaline and some metal ions. The enrichment factor was 330. The detection limits by three sigma were 0.50 microg L(-1) for copper, 0.75 microg L(-1) for nickel and 0.80 microg L(-1) for cobalt. The loading capacity was 0.56 mg g(-1) for Ni2+, 0.50 mg g(-1) for Cu2+ and 0.47 mg g(-1) for Co2+. The presented procedure was applied to the determination of analytes in tap, river and sea waters, vegetable, soil and blood samples with successfully results (recoveries greater than 95%, R.S.D. lower than 2% for n=3).

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

Science.gov (United States)

Bladergroen, Marco R.; van der Burgt, Yuri E. M.

2015-01-01

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. PMID:25692071

Analysis of microcontaminants in aqueous samples by fully automated on-line solid-phase extraction-gas chromatography-mass selective detection.

NARCIS (Netherlands)

Louter, A.J.H.; van Beekvelt, C.A.; Cid Montanes, P.; Slobodník, J.; Vreuls, J.J.; Brinkman, U.A.T.

1996-01-01

The trace-level analysis of unknown organic pollutants in water requires the use of fast and sensitive methods which also provide structural information. In the present study, an on-line technique was used which combines sample preparation by means of solid-phase extraction (SPE) on a small

Marine sediments monitoring studies for trace elements with the application of fast temperature programs and solid sampling high resolution continuum source atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

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

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

Preliminary evaluation of new polymer matrix for solid-phase extraction of nonylphenol from water samples.

Science.gov (United States)

Guerreiro, António; Soares, Ana; Piletska, Elena; Mattiasson, Bo; Piletsky, Sergey

2008-03-31

Molecularly imprinted (MIP) and blank polymers with affinity for nonylphenol were designed using computational modelling. Chromatographic tests demonstrated higher affinity of imprinted polymers towards the template nonylphenol as compared with blank polymers. The performance of both polymers in solid-phase extraction was however very similar. Both blank and imprinted polymers appeared to be suitable for the removal and pre-concentration of nonylphenol from contaminated water samples with 99% efficiency of the recovery. The commercial resins PH(EC) (Biotage) and C18 (Varian) tested in the same conditions used for comparative purposes had recovery rate <84%. The polymer capacity for nonylphenol was 231 mg g(-1) for blank and 228 mg g(-1) for MIP. The synthesised materials can have significance for sample pre-concentration and environmental analysis of this class of compounds.

Major- and minor-metal composition of three distinct solid material fractions associated with Juan de Fuca hydrothermal fluids (northeast Pacific), and calculation of dilution fluid samples

Science.gov (United States)

Hinkley, T.K.; Seeley, J.L.; Tatsumoto, M.

1988-01-01

Three distinct types of solid material are associated with each sample of the hydrothermal fluid that was collected from the vents of the Southern Juan de Fuca Ridge. The solid materials appear to be representative of deposits on ocean floors near mid-ocean ridges, and interpretation of the chemistry of the hydrothermal solutions requires understanding of them. Sr isotopic evidence indicates that at least two and probably all three of these solid materials were removed from the solution with which they are associated, by precipitation or adsorption. This occurred after the "pure" hydrothermal fluid was diluted and thoroughly mixed with ambient seawater. The three types of solid materials, are, respectively, a coarse Zn- and Fe-rich material with small amounts of Na and Ca; a finer material also rich in Zn and Fe, but with alkali and alkaline-earth metals; and a scum composed of Ba or Zn, with either considerable Fe or Si, and Sr. Mineral identification is uncertain because of uncertain anion composition. Only in the cases of Ba and Zn were metal masses greater in solid materials than in the associated fluids. For all other metals measured, masses in fluids dwarf those in solids. The fluids themselves contain greater concentrations of all metals measured, except Mg, than seawater. We discuss in detail the relative merits of two methods of determining the mixing proportions of "pure" hydrothermal solution and seawater in the fluids, one based on Sr isotopes, and another previously used method based on Mg concentrations. Comparison of solute concentrations in the several samples shows that degree of dilution of "pure" hydrothermal solutions by seawater, and amounts of original solutes that were removed from it as solid materials, are not related. There is no clear evidence that appreciable amounts of solid materials were not conserved (lost) either during or prior to sample collection. ?? 1988.

Fluorine determination in coal using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

Energy Technology Data Exchange (ETDEWEB)

Machado, Patrícia M.; Morés, Silvane; Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Welz, Bernhard, E-mail: w.bernardo@terra.com.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Carasek, Eduardo [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Andrade, Jailson B. de [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil)

2015-03-01

The absorption of the calcium mono-fluoride (CaF) molecule has been employed in this study for the determination of fluorine in coal using direct solid sample analysis and high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS). The rotational line at 606.440 nm was used for measuring the molecular absorption in the gas phase. The pyrolysis and vaporization temperatures were 700 °C and 2100 °C, respectively. Different chemical modifiers have been studied, such as Pd and Ir as permanent modifiers, and Pd and the mixed Pd/Mg modifier in solution. The limit of detection and the characteristic mass were 0.3 and 0.1 ng F, respectively. One certified reference material (CRM) of coal (NIST 1635) and four CRMs with a non-certified value for F (SARM 18, SARM 20, BCR 40, BCR 180) were used to evaluate the accuracy and precision of the method, obtaining good agreement (104%) with the certified value and with the informed values (ranging from 90 to 103%). - Highlights: • High-resolution Graphite Furnace Molecular Absorption Spectrometry (HR-GF MAS) • Fluorine has been determined using HR-GF MAS of the CaF molecule. • The CaF molecule was generated in a graphite furnace at a temperature of 2100 °C • Coal samples have been analyzed using direct solid sample introduction. • Aqueous standard solutions have been used for calibration.

Study on Solid Phase Extraction and Spectrophotometric Determination of Nickel in Waters and Biological Samples

International Nuclear Information System (INIS)

Hu, Qiufen; Yang, Guangyu; Huang, Zhangjie; Yin, Jiayuan

2004-01-01

A sensitive, selective and rapid method for the determination of nickel based on the rapid reaction of nickel(II) with QADMAA and the solid phase extraction of the Ni(II)-QADMAA chelate with C 18 membrane disks has been developed. In the presence of pH 6.0 buffer solution and sodium dodecyl sulfonate (SDS) medium, QADMAA reacts with nickel to form a violet complex of a molar ratio of 1 : 2 (nickel to QADMAA). This chelate was enriched by solid phase extraction with C 18 membrane disks. An enrichment factor of 50 was obtained by elution of the chelates form the disks with the minimal amount of isopentyl alcohol. The molar absorptivity of the chelate was 1.32 x 10 5 L mol -1 cm -1 at 590 nm in the measured solution. Beer's law was obeyed in the range of 0.01-0.6 μg/mL. This method was applied to the determination of nickel in water and biological samples with good results

Solid phase assays

International Nuclear Information System (INIS)

Reese, M.G.; Johnson, L.R.; Ransom, D.K.

1980-01-01

In a solid phase assay for quantitative determination of biological and other analytes, a sample such as serum is contacted with a receptor for the analyte being assayed, the receptor being supported on a solid support. No tracer for the analyte is added to the sample before contacting with the receptor; instead the tracer is contacted with the receptor after unbound analyte has been removed from the receptor. The assay can be otherwise performed in a conventional manner but can give greater sensitivity. (author)

Comparison of 22G reverse-beveled versus standard needle for endoscopic ultrasound-guided sampling of solid pancreatic lesions

Science.gov (United States)

Alatawi, Abdullah; Beuvon, Frédéric; Grabar, Sophie; Leblanc, Sarah; Chaussade, Stanislas; Terris, Benoit; Barret, Maximilien

2015-01-01

Objectives Endoscopic ultrasound-guided fine-needle aspiration (EUS-FNA) using standard needles has a high diagnostic value in the evaluation of solid pancreatic masses. Fenestrated needles have been developed to improve the quality of EUS-guided tissue sampling by providing core biopsies (FNB). Methods Patients with solid pancreatic masses of >2 cm were prospectively included in our study and randomized to receive EUS sampling, using either a standard 22G FNA or a 22G Procore® FNB needle. The main study endpoint was the number of needle passes required to obtain a diagnosis in more than 90% of cases. Results We included 100 patients (male = 63, female = 37; mean age = 68.4 years) in our study. We found that 88% of the lesions were malignant, with a mean size of 32 mm. A sample adequate for diagnosis was obtained in more than 90% of cases after the second needle pass in the FNB group, versus the third needle pass in the FNA group. Slide cellularity and presence of tissue microfragments were significantly higher in the FNB group. Sensitivity for the diagnosis of malignancy was 88.4% versus 97.8% for the EUS-FNA and EUS-FNB group, respectively, while specificity for both techniques was 100%. No complications were recorded. Conclusions Although the accuracy of both needle types for proving malignancy was similar, a lower number of passes was required with the FNB needles to achieve the same contributive sample rate as with the FNA needles. FNB also improved the histopathological quality of specimens, suggesting an overall superiority of FNB sampling. PMID:26279842

Perspectives of an acoustic–electrostatic/electrodynamic hybrid levitator for small fluid and solid samples

International Nuclear Information System (INIS)

Lierke, E G; Holitzner, L

2008-01-01

The feasibility of an acoustic–electrostatic hybrid levitator for small fluid and solid samples is evaluated. A proposed design and its theoretical assessment are based on the optional implementation of simple hardware components (ring electrodes) and standard laboratory equipment into typical commercial ultrasonic standing wave levitators. These levitators allow precise electrical charging of drops during syringe- or ink-jet-type deployment. The homogeneous electric 'Millikan field' between the grounded ultrasonic transducer and the electrically charged reflector provide an axial compensation of the sample weight in an indifferent equilibrium, which can be balanced by using commercial optical position sensors in combination with standard electronic PID position control. Radial electrostatic repulsion forces between the charged sample and concentric ring electrodes of the same polarity provide stable positioning at the centre of the levitator. The levitator can be used in a pure acoustic or electrostatic mode or in a hybrid combination of both subsystems. Analytical evaluations of the radial–axial force profiles are verified with detailed numerical finite element calculations under consideration of alternative boundary conditions. The simple hardware modification with implemented double-ring electrodes in ac/dc operation is also feasible for an electrodynamic/acoustic hybrid levitator

Determination of Fe, Mn and Pb by GFAAS in red wine

International Nuclear Information System (INIS)

Ying Zhecong; Jin Hua; Su Yulan

2008-01-01

A method for determination of Fe, Mn and Pb in red wine samples was developed by the graphite furnace atomic absorption spectrometric. Several different matrix modifiers were necessary because of evident analyte losses that occurred immediately in sample incineration. Red wine samples were analyzed after microwave digestion using HNO 3 . Standard addition method was used, the calibration concentration was 1 ng · ml -1 , 3 ng · ml -1 , 5 ng · ml -1 which containing 580 μg/ml KNO 3 as matrix and 0.2% HNO 3 . The correlation coefficient of the calibration line was very good within the measurement area. The recovery with red wine sample was very good at the range from 95%-107.5%. (authors)

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

International Nuclear Information System (INIS)

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

2005-01-01

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 deg. 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 deg. C and 2300 deg. C for Cu, and 700 deg. C and 1700 deg. 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

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.

Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD and Dispersive Solid Phase Extraction (d-SPE of Plant Samples

Directory of Open Access Journals (Sweden)

Ireneusz Sowa

2018-03-01

Full Text Available Polyaniline (PANI is one of the best known conductive polymers with multiple applications. Recently, it was also used in separation techniques, mostly as a component of composites for solid-phase microextraction (SPME. In the present paper, sorbent obtained by in situ polymerization of aniline directly on silica gel particles (Si-PANI was used for dispersive solid phase extraction (d-SPE and matrix solid–phase extraction (MSPD. The efficiency of both techniques was evaluated with the use of high performance liquid chromatography with diode array detection (HPLC-DAD quantitative analysis. The quality of the sorbent was verified by Raman spectroscopy and microscopy combined with automated procedure using computer image analysis. For extraction experiments, triterpenes were chosen as model compounds. The optimal conditions were as follows: protonated Si-PANI impregnated with water, 160/1 sorbent/analyte ratio, 3 min of extraction time, 4 min of desorption time and methanolic solution of ammonia for elution of analytes. The proposed procedure was successfully used for pretreatment of plant samples.

STEALTH: a Lagrange explicit finite difference code for solids, structural, and thermohydraulic analysis. Volume 2: sample and verification problems. Computer code manual

International Nuclear Information System (INIS)

Hofmann, R.

1982-08-01

STEALTH sample and verification problems are presented to help users become familiar with STEALTH capabilities, input, and output. Problems are grouped into articles which are completely self-contained. The pagination in each article is A.n, where A is a unique alphabetic-character article identifier and n is a sequential page number which starts from 1 on the first page of text for each article. Articles concerning new capabilities will be added as they become available. STEALTH sample and verification calculations are divided into the following general categories: transient mechanical calculations dealing with solids; transient mechanical calculations dealing with fluids; transient thermal calculations dealing with solids; transient thermal calculations dealing with fluids; static and quasi-static calculations; and complex boundary interaction calculations

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

International Nuclear Information System (INIS)

Filik, Hayati; Yanaz, Zeynep

2009-01-01

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 ∼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%.

Box-Behnken design in modeling of solid-phase tea waste extraction for the removal of uranium from water samples

Energy Technology Data Exchange (ETDEWEB)

Khajeh, Mostafa; Jahanbin, Elham; Ghaffari-Moghaddam, Mansour; Moghaddam, Zahra Safaei [Zabol Univ. (Iran, Islamic Republic of). Dept. of Chemistry; Bohlooli, Mousa [Zabol Univ. (Iran, Islamic Republic of). Dept. of Biology

2015-07-01

In this study, the solid-phase tea waste procedure was used for separation, preconcentration and determination of uranium from water samples by UV-Vis spectrophotometer. In addition, Box-Behnken experimental design was employed to investigated the influence of six variables including pH, mass of adsorbent, eluent volume, amount of 1-(2-pyridylazo)-2-naphthol (PAN); and sample and eluent flow rates on the extraction of analyte. High determination coefficient (R{sup 2}) of 0.972 and adjusted-R{sup 2} of 0.943 showed the satisfactory adjustment of the polynomial regression model. This method was used for the extraction of uranium from real water samples.

Box-Behnken design in modeling of solid-phase tea waste extraction for the removal of uranium from water samples

International Nuclear Information System (INIS)

Khajeh, Mostafa; Jahanbin, Elham; Ghaffari-Moghaddam, Mansour; Moghaddam, Zahra Safaei; Bohlooli, Mousa

2015-01-01

In this study, the solid-phase tea waste procedure was used for separation, preconcentration and determination of uranium from water samples by UV-Vis spectrophotometer. In addition, Box-Behnken experimental design was employed to investigated the influence of six variables including pH, mass of adsorbent, eluent volume, amount of 1-(2-pyridylazo)-2-naphthol (PAN); and sample and eluent flow rates on the extraction of analyte. High determination coefficient (R 2 ) of 0.972 and adjusted-R 2 of 0.943 showed the satisfactory adjustment of the polynomial regression model. This method was used for the extraction of uranium from real water samples.

EDXRF applied to the chemical element determination of small invertebrate samples

International Nuclear Information System (INIS)

Magalhaes, Marcelo L.R.; Santos, Mariana L.O.; Cantinha, Rebeca S.; Souza, Thomas Marques de; Franca, Elvis J. de

2015-01-01

Energy Dispersion X-Ray Fluorescence - EDXRF is a fast analytical technique of easy operation, however demanding reliable analytical curves due to the intrinsic matrix dependence and interference during the analysis. By using biological materials of diverse matrices, multielemental analytical protocols can be implemented and a group of chemical elements could be determined in diverse biological matrices depending on the chemical element concentration. Particularly for invertebrates, EDXRF presents some advantages associated to the possibility of the analysis of small size samples, in which a collimator can be used that directing the incidence of X-rays to a small surface of the analyzed samples. In this work, EDXRF was applied to determine Cl, Fe, P, S and Zn in invertebrate samples using the collimator of 3 mm and 10 mm. For the assessment of the analytical protocol, the SRM 2976 Trace Elements in Mollusk produced and SRM 8415 Whole Egg Powder by the National Institute of Standards and Technology - NIST were also analyzed. After sampling by using pitfall traps, invertebrate were lyophilized, milled and transferred to polyethylene vials covered by XRF polyethylene. Analyses were performed at atmosphere lower than 30 Pa, varying voltage and electric current according to the chemical element to be analyzed. For comparison, Zn in the invertebrate material was also quantified by graphite furnace atomic absorption spectrometry after acid treatment (mixture of nitric acid and hydrogen peroxide) of samples have. Compared to the collimator of 10 mm, the SRM 2976 and SRM 8415 results obtained by the 3 mm collimator agreed well at the 95% confidence level since the E n Number were in the range of -1 and 1. Results from GFAAS were in accordance to the EDXRF values for composite samples. Therefore, determination of some chemical elements by EDXRF can be recommended for very small invertebrate samples (lower than 100 mg) with advantage of preserving the samples. (author)

Preparation and evaluation of molecularly imprinted solid-phase micro-extraction fibers for selective extraction of phthalates in an aqueous sample

International Nuclear Information System (INIS)

He Juan; Lv Ruihe; Zhan Haijun; Wang Huizhi; Cheng Jie; Lu Kui; Wang Fengcheng

2010-01-01

A novel molecularly imprinted polymer (MIP) that was applied to a solid-phase micro-extraction (SPME) device, which could be coupled directly to gas chromatograph and mass spectrometer (GC/MS), was prepared using dibutyl phthalate (DBP) as the template molecule. The characteristics and application of this fiber were investigated. Electron microscope images indicated that the MIP-coated solid-phase micro-extraction (MI-SPME) fibers were homogeneous and porous. The extraction yield of DBP with the MI-SPME fibers was higher than that of the non-imprinted polymer (NIP)-coated SPME (NI-SPME) fibers. The MI-SPME fibers had a higher selectivity to other phthalates that had similar structures as DBP. A method was developed for the determination of phthalates using MI-SPME fibers coupled with GC/MS. The extraction conditions were optimized. Detection limits for the phthalate samples were within the range of 2.17-20.84 ng L -1 . The method was applied to five kinds of phthalates dissolved in spiked aqueous samples and resulted in recoveries of up to 94.54-105.34%, respectively. Thus, the MI-SPME fibers are suitable for the extraction of trace phthalates in complicated samples.

Design and Characterisation of Solid Electrolytes for All-Solid-State Lithium Batteries

DEFF Research Database (Denmark)

Sveinbjörnsson, Dadi Þorsteinn

The development of all-solid-state lithium batteries, in which the currently used liquid electrolytes are substituted for solid electrolyte materials, could lead to safer batteries offering higher energy densities and longer cycle lifetimes. Designing suitable solid electrolytes with sufficient...... chemical and electrochemical stability, high lithium ion conduction and negligible electronic conduction remains a challenge. The highly lithium ion conducting LiBH4-LiI solid solution is a promising solid electrolyte material. Solid solutions with a LiI content of 6.25%-50% were synthesised by planetary......-rich microstructures during ball milling is found to significantly influence the conductivity of the samples. The long-range diffusion of lithium ions was measured using quasi-elastic neutron scattering. The solid solutions are found to exhibit two-dimensional conduction in the hexagonal plane of the crystal structure...

A method of estimating hydrogen in solid and liquid samples by means of neutron thermalisation

International Nuclear Information System (INIS)

Carter, D.H.; Sanders, J.E.

1967-06-01

The count-rate of a cadmium-covered Pu239 fission chamber placed in a reactor neutron flux increases when a hydrogen-containing material is inserted due to the thermalisation of epicadmium neutrons. This effect forms the basis of a non-destructive method of estimating hydrogen in solid or liquid samples, and trial experiments to demonstrate the principles have been made. The sensitivity is such that hydrogen down to 10 p.p.m. in a typical metal should be detected. A useful feature of the method is its very low response to elements other than hydrogen. (author)

Microporous Carbon Spheres Solid Phase Membrane Tip Extraction for the Analysis of Nitrosamines in Water Samples

International Nuclear Information System (INIS)

Mohammed Salisu Musa; Wan Aini Wan Ibrahim

2015-01-01

A simple solid phase membrane tip extraction (SPMTE) utilizing microporous carbon spheres (MCS) was developed for the analysis of nitrosamines in aqueous samples. The method termed MCS-SPMTE was optimized for various important extraction parameters namely conditioning organic solvent, extraction time, effects of salt addition and pH change, desorption time, desorption solvent and sample volume. Under the optimized conditions, the method indicated good linearity in the range of 10-100 μg/ L with coefficients of determination, r 2 ≥0.9984. The method also demonstrated good reproducibility with % RSDs values ranging from 2.2 - 8.9 (n = 3). Limit of detection (LOD) and limit of quantification (LOQ) for the method ranged from 3.2 - 4.8 μg/ L and 10.9 - 15.9 μg/L respectively. Recoveries for both tap-water and lake water samples spiked at 10 μg/L were in the range of 83.2 - 107.5 %. (author)

Determination of volatile organic hydrocarbons in water samples by solid-phase dynamic extraction

Energy Technology Data Exchange (ETDEWEB)

Jochmann, Maik A.; Schmidt, Torsten C. [Eberhard-Karls-Universitaet Tuebingen, Center for Applied Geoscience (ZAG), Tuebingen (Germany); Chair of Instrumental Analysis, University Duisburg-Essen, Duisburg (Germany); Yuan, Xue [Eberhard-Karls-Universitaet Tuebingen, Center for Applied Geoscience (ZAG), Tuebingen (Germany)

2007-03-15

In the present study a headspace solid-phase dynamic extraction method coupled to gas chromatography-mass spectrometry (HS-SPDE-GC/MS) for the trace determination of volatile halogenated hydrocarbons and benzene from groundwater samples was developed and evaluated. As target compounds, benzene as well as 11 chlorinated and brominated hydrocarbons (vinyl chloride, dichloromethane, cis-1,2-dichloroethylene, trans-1,2-dichloroethylene, carbon tetrachloride, chloroform, trichloroethylene, tetrachloroethylene, bromoform) of environmental and toxicological concern were included in this study. The analytes were extracted using a SPDE needle device, coated with a poly(dimethylsiloxane) with 10% embedded activated carbon phase (50-{mu}m film thickness and 56-mm film length) and were analyzed by GC/MS in full-scan mode. Parameters that affect the extraction yield such as extraction and desorption temperature, salting-out, extraction and desorption flow rate, extraction volume and desorption volume, the number of extraction cycles, and the pre-desorption time have been evaluated and optimized. The linearity of the HS-SPDE-GC/MS method was established over several orders of magnitude. Method detection limits (MDLs) for the compounds investigated ranged between 12 ng/L for cis-dichloroethylene and trans-dichloroethylene and 870 ng/L for vinyl chloride. The method was thoroughly validated, and the precision at two concentration levels (0.1 mg/L and a concentration 5 times above the MDL) was between 3.1 and 16% for the analytes investigated. SPDE provides high sensitivity, short sample preparation and extraction times and a high sample throughput because of full automation. Finally, the applicability to real environmental samples is shown exemplarily for various groundwater samples from a former waste-oil recycling facility. Groundwater from the site showed a complex contamination with chlorinated volatile organic compounds and aromatic hydrocarbons. (orig.)

Determination of volatile organic hydrocarbons in water samples by solid-phase dynamic extraction.

Science.gov (United States)

Jochmann, Maik A; Yuan, Xue; Schmidt, Torsten C

2007-03-01

In the present study a headspace solid-phase dynamic extraction method coupled to gas chromatography-mass spectrometry (HS-SPDE-GC/MS) for the trace determination of volatile halogenated hydrocarbons and benzene from groundwater samples was developed and evaluated. As target compounds, benzene as well as 11 chlorinated and brominated hydrocarbons (vinyl chloride, dichloromethane, cis-1,2-dichloroethylene, trans-1,2-dichloroethylene, carbon tetrachloride, chloroform, trichloroethylene, tetrachloroethylene, bromoform) of environmental and toxicological concern were included in this study. The analytes were extracted using a SPDE needle device, coated with a poly(dimethylsiloxane) with 10% embedded activated carbon phase (50-microm film thickness and 56-mm film length) and were analyzed by GC/MS in full-scan mode. Parameters that affect the extraction yield such as extraction and desorption temperature, salting-out, extraction and desorption flow rate, extraction volume and desorption volume, the number of extraction cycles, and the pre-desorption time have been evaluated and optimized. The linearity of the HS-SPDE-GC/MS method was established over several orders of magnitude. Method detection limits (MDLs) for the compounds investigated ranged between 12 ng/L for cis-dichloroethylene and trans-dichloroethylene and 870 ng/L for vinyl chloride. The method was thoroughly validated, and the precision at two concentration levels (0.1 mg/L and a concentration 5 times above the MDL) was between 3.1 and 16% for the analytes investigated. SPDE provides high sensitivity, short sample preparation and extraction times and a high sample throughput because of full automation. Finally, the applicability to real environmental samples is shown exemplarily for various groundwater samples from a former waste-oil recycling facility. Groundwater from the site showed a complex contamination with chlorinated volatile organic compounds and aromatic hydrocarbons.

Determination of trace aluminum concentration and homogeneity in biological material TORT-1 by instrumental neutron activation and graphite furnace atomic absorption spectrometry

International Nuclear Information System (INIS)

Kratochvil, B.; Motkosky, N.; Duke, M.J.M.; Ng, D.

1987-01-01

The biological reference material TORT-1, lobster hepatopancreas, was analyzed for aluminum by instrumental neutron activation analysis (INAA) and graphite furnace atomic absorption spectroscopy (GFAAS). After correction of the INAA results for interferences from 28 Al produced by 31 P(n,α) 28 Al and 28 (n,p) 28 Al reactions, and use of HNO 3 plus HF for sample dissolution for the GFAAS analyses, the methods gave similar results of 43 ± 3 and 42 ± 2 μg/g respectively for 200 to 300-mg test portions. Analysis of six portions from each of six bottles of TORT-1 showed no statistical difference at the 95% confidence level for the between and within bottle variances. Therefore, The material can be considered homogeneous for aluminum if 200- to 300-mg test portions are taken. The variance was greater and the average lower when 30-mg test portions were analyzed for aluminum by GFAAS. The pattern of the results, together with the need for HF in the dissolution procedure, suggests the presence of aluminum-containing microparticulate mineral matter, perhaps silicate material, in the material

Determination of trace aluminum concentration and homogeneity in biological material TORT-1 by instrumental neutron activation and graphite furnace atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Kratochvil, B; Motkosky, N; Duke, M J.M.; Ng, D

1987-05-01

The biological reference material TORT-1, lobster hepatopancreas, was analyzed for aluminum by instrumental neutron activation analysis (INAA) and graphite furnace atomic absorption spectroscopy (GFAAS). After correction of the INAA results for interferences from /sup 28/Al produced by /sup 31/P(n,..cap alpha..)/sup 28/Al and /sup 28/(n,p)/sup 28/Al reactions, and use of HNO/sub 3/ plus HF for sample dissolution for the GFAAS analyses, the methods gave similar results of 43 +- 3 and 42 +- 2 ..mu..g/g respectively for 200 to 300-mg test portions. Analysis of six portions from each of six bottles of TORT-1 showed no statistical difference at the 95% confidence level for the between and within bottle variances. Therefore, The material can be considered homogeneous for aluminum if 200- to 300-mg test portions are taken. The variance was greater and the average lower when 30-mg test portions were analyzed for aluminum by GFAAS. The pattern of the results, together with the need for HF in the dissolution procedure, suggests the presence of aluminum-containing microparticulate mineral matter, perhaps silicate material, in the material.

Sampling and analytical procedures for the determination of VOCs released into air from natural and anthropogenic sources: A comparison between SPME (Solid Phase Micro Extraction) and ST (Solid Trap) methods

International Nuclear Information System (INIS)

Tassi, F.; Capecchiacci, F.; Buccianti, A.; Vaselli, O.

2012-01-01

In the present study, two sampling and analytical methods for VOC determination in fumarolic exhalations related to hydrothermal-magmatic reservoirs in volcanic and geothermal areas and biogas released from waste landfills were compared: (a) Solid Traps (STs), consisting of three phase (Carboxen B, Carboxen C and Carbosieve S111) absorbent stainless steel tubes and (b) Solid Phase Micro Extraction (SPME) fibers, composed of DiVinylBenzene (DVB), Carboxen and PolyDimethylSiloxane. These techniques were applied to pre-concentrate VOCs discharged from: (i) low-to-high temperature fumaroles collected at Vulcano Island, Phlegrean Fields (Italy), and Nisyros Island (Greece), (ii) recovery wells in a solid waste disposal site located near Florence (Italy). A glass condensing system cooled with water was used to collect the dry fraction of the fumarolic gases, in order to allow more efficient VOC absorption avoiding any interference by water vapor and acidic gases, such as SO 2 , H 2 S, HF and HCl, typically present at relatively high concentrations in these fluids. Up to 37 organic species, in the range of 40–400 m/z, were determined by coupling gas chromatography to mass spectrometry (GC–MS). This study shows that the VOC compositions of fumaroles and biogas determined via SPME and ST are largely consistent and can be applied to the analysis of VOCs in gases released from different natural and anthropogenic environments. The SPME method is rapid and simple and more appropriate for volcanic and geothermal emissions, where VOCs are present at relatively high concentrations and prolonged gas sampling may be hazardous for the operator. The ST method, allowing the collection of large quantities of sample, is to be preferred to analyze the VOC composition of fluids from diffuse emissions and air, where these compounds are present at relatively low concentrations.

Assessment of statistical uncertainty in the quantitative analysis of solid samples in motion using laser-induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Cabalin, L.M.; Gonzalez, A. [Department of Analytical Chemistry, University of Malaga, E-29071 Malaga (Spain); Ruiz, J. [Department of Applied Physics I, University of Malaga, E-29071 Malaga (Spain); Laserna, J.J., E-mail: laserna@uma.e [Department of Analytical Chemistry, University of Malaga, E-29071 Malaga (Spain)

2010-08-15

Statistical uncertainty in the quantitative analysis of solid samples in motion by laser-induced breakdown spectroscopy (LIBS) has been assessed. For this purpose, a LIBS demonstrator was designed and constructed in our laboratory. The LIBS system consisted of a laboratory-scale conveyor belt, a compact optical module and a Nd:YAG laser operating at 532 nm. The speed of the conveyor belt was variable and could be adjusted up to a maximum speed of 2 m s{sup -1}. Statistical uncertainty in the analytical measurements was estimated in terms of precision (reproducibility and repeatability) and accuracy. The results obtained by LIBS on shredded scrap samples under real conditions have demonstrated that the analytical precision and accuracy of LIBS is dependent on the sample geometry, position on the conveyor belt and surface cleanliness. Flat, relatively clean scrap samples exhibited acceptable reproducibility and repeatability; by contrast, samples with an irregular shape or a dirty surface exhibited a poor relative standard deviation.

Assessment of statistical uncertainty in the quantitative analysis of solid samples in motion using laser-induced breakdown spectroscopy

Science.gov (United States)

Cabalín, L. M.; González, A.; Ruiz, J.; Laserna, J. J.

2010-08-01

Statistical uncertainty in the quantitative analysis of solid samples in motion by laser-induced breakdown spectroscopy (LIBS) has been assessed. For this purpose, a LIBS demonstrator was designed and constructed in our laboratory. The LIBS system consisted of a laboratory-scale conveyor belt, a compact optical module and a Nd:YAG laser operating at 532 nm. The speed of the conveyor belt was variable and could be adjusted up to a maximum speed of 2 m s - 1 . Statistical uncertainty in the analytical measurements was estimated in terms of precision (reproducibility and repeatability) and accuracy. The results obtained by LIBS on shredded scrap samples under real conditions have demonstrated that the analytical precision and accuracy of LIBS is dependent on the sample geometry, position on the conveyor belt and surface cleanliness. Flat, relatively clean scrap samples exhibited acceptable reproducibility and repeatability; by contrast, samples with an irregular shape or a dirty surface exhibited a poor relative standard deviation.

Assessment of statistical uncertainty in the quantitative analysis of solid samples in motion using laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Cabalin, L.M.; Gonzalez, A.; Ruiz, J.; Laserna, J.J.

2010-01-01

Statistical uncertainty in the quantitative analysis of solid samples in motion by laser-induced breakdown spectroscopy (LIBS) has been assessed. For this purpose, a LIBS demonstrator was designed and constructed in our laboratory. The LIBS system consisted of a laboratory-scale conveyor belt, a compact optical module and a Nd:YAG laser operating at 532 nm. The speed of the conveyor belt was variable and could be adjusted up to a maximum speed of 2 m s -1 . Statistical uncertainty in the analytical measurements was estimated in terms of precision (reproducibility and repeatability) and accuracy. The results obtained by LIBS on shredded scrap samples under real conditions have demonstrated that the analytical precision and accuracy of LIBS is dependent on the sample geometry, position on the conveyor belt and surface cleanliness. Flat, relatively clean scrap samples exhibited acceptable reproducibility and repeatability; by contrast, samples with an irregular shape or a dirty surface exhibited a poor relative standard deviation.

Develpoment of a procedure for the determination of chromium in samples of urine and serum by neutron activation analysis

International Nuclear Information System (INIS)

Buettner, I.; Hamm, V.; Knoechel, A.; Sen Gupta, R.

1993-01-01

Since the mid-fifties the possibility of a causal relationship between deficient chromium and insulin metabolism and the manifestation of certain varieties of diabetes mellitus has been presumed. The determination of the chromium status under pathophysiological conditions may be helpful for the study of this problem. For these purposes an analytical procedure as reference system was developed which allows the determination of chromium in biological matrices down to the concentration of 0.33 ng/ml. It is based on NAA and is used in the framework of a commonly used procedure based on GF-AAS. For its application blood and urine samples are freeze-dried and irradiated. After wet digestion with HNO 3 in a microwave combustion system chromium is separated for measurement from the matrix nuclides with the help of the ion-exchanger Cellex-P. THe individual steps of the procedure were evaluated by means of tracer experiments. (orig.)

Develpoment of a procedure for the determination of chromium in samples of urine and serum by neutron activation analysis

Energy Technology Data Exchange (ETDEWEB)

Buettner, I [Hamburg Univ. (Germany). Inst. for Inorganic and Applied Chemistry; Hamm, V [Hamburg Univ. (Germany). Inst. for Inorganic and Applied Chemistry; Knoechel, A [Hamburg Univ. (Germany). Inst. for Inorganic and Applied Chemistry; Sen Gupta, R [Hamburg Univ. (Germany). Inst. for Inorganic and Applied Chemistry

1993-06-01

Since the mid-fifties the possibility of a causal relationship between deficient chromium and insulin metabolism and the manifestation of certain varieties of diabetes mellitus has been presumed. The determination of the chromium status under pathophysiological conditions may be helpful for the study of this problem. For these purposes an analytical procedure as reference system was developed which allows the determination of chromium in biological matrices down to the concentration of 0.33 ng/ml. It is based on NAA and is used in the framework of a commonly used procedure based on GF-AAS. For its application blood and urine samples are freeze-dried and irradiated. After wet digestion with HNO[sub 3] in a microwave combustion system chromium is separated for measurement from the matrix nuclides with the help of the ion-exchanger Cellex-P. THe individual steps of the procedure were evaluated by means of tracer experiments. (orig.)

[Determination of fatty acid esters of chloropropanediols in diet samples by gas chromatography-mass spectrometry coupled with solid-supported liquid-liquid extraction].

Science.gov (United States)

Gao, Jie; Liu, Qing; Han, Feng; Miao, Hong; Zhao, Yunfeng; Wu, Yongning

2014-05-01

To establish a method for the determination of fatty acid esters of 3-monochloropropane-1, 2-diol (3-MCPD) and 2-monochloropropane-1, 3-diol (2-MCPD) in diet samples by gas chromatography-mass spectrometry (GC-MS) with solid-supported liquid-liquid extraction (SLE). Diet samples were ultrasonically extracted by hexane, followed by ester cleavage reaction with sodium methylate in methanol, and then purified by solid-supported liquid-liquid extraction. (SLE) using diatomaceous earth as the sorbent. After derivatization with heptafluorobutyrylimidazole, the analytes were detected by GC-MS and quantified by the deuterated internal standards. The limits of detection (LODs) of 3-MCPD esters and 2-MCPD esters in different diet samples were 0.002 - 0.005 mg/kg and 0.002 - 0.006 mg/kg. The average recoveries of 3-MCPD esters and 2-MCPD esters at the spiking levels of 0.05 and 0.1 mg/kg in the diet samples were in the range of 65.9% - 104.2% and 75.4% - 118.0%, respectively, with the relative standard deviations in the range of 2.2% - 14.2% and 0.8% - .13.9%. The method is simple, accurate and rugged for the determination of fatty acid esters of 3-MCPD and 2-MCPD in diet samples.

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.

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

International Nuclear Information System (INIS)

2000-01-01

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).

Solid-Phase Extraction and Large-Volume Sample Stacking-Capillary Electrophoresis for Determination of Tetracycline Residues in Milk

Directory of Open Access Journals (Sweden)

Gabriela Islas

2018-01-01

Full Text Available Solid-phase extraction in combination with large-volume sample stacking-capillary electrophoresis (SPE-LVSS-CE was applied to measure chlortetracycline, doxycycline, oxytetracycline, and tetracycline in milk samples. Under optimal conditions, the proposed method had a linear range of 29 to 200 µg·L−1, with limits of detection ranging from 18.6 to 23.8 µg·L−1 with inter- and intraday repeatabilities < 10% (as a relative standard deviation in all cases. The enrichment factors obtained were from 50.33 to 70.85 for all the TCs compared with a conventional capillary zone electrophoresis (CZE. This method is adequate to analyze tetracyclines below the most restrictive established maximum residue limits. The proposed method was employed in the analysis of 15 milk samples from different brands. Two of the tested samples were positive for the presence of oxytetracycline with concentrations of 95 and 126 µg·L−1. SPE-LVSS-CE is a robust, easy, and efficient strategy for online preconcentration of tetracycline residues in complex matrices.

Multiplexed Colorimetric Solid-Phase Extraction

Science.gov (United States)

Gazda, Daniel B.; Fritz, James S.; Porter, Marc D.

2009-01-01

Multiplexed colorimetric solid-phase extraction (MC-SPE) is an extension of colorimetric solid-phase extraction (C-SPE) an analytical platform that combines colorimetric reagents, solid phase extraction, and diffuse reflectance spectroscopy to quantify trace analytes in water. In CSPE, analytes are extracted and complexed on the surface of an extraction membrane impregnated with a colorimetric reagent. The analytes are then quantified directly on the membrane surface using a handheld diffuse reflectance spectrophotometer. Importantly, the use of solid-phase extraction membranes as the matrix for impregnation of the colorimetric reagents creates a concentration factor that enables the detection of low concentrations of analytes in small sample volumes. In extending C-SPE to a multiplexed format, a filter holder that incorporates discrete analysis channels and a jig that facilitates the concurrent operation of multiple sample syringes have been designed, enabling the simultaneous determination of multiple analytes. Separate, single analyte membranes, placed in a readout cartridge create unique, analyte-specific addresses at the exit of each channel. Following sample exposure, the diffuse reflectance spectrum of each address is collected serially and the Kubelka-Munk function is used to quantify each water quality parameter via calibration curves. In a demonstration, MC-SPE was used to measure the pH of a sample and quantitate Ag(I) and Ni(II).

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.

Use of X-ray diffraction technique and chemometrics to aid soil sampling strategies in traceability studies.

Science.gov (United States)

Bertacchini, Lucia; Durante, Caterina; Marchetti, Andrea; Sighinolfi, Simona; Silvestri, Michele; Cocchi, Marina

2012-08-30

Aim of this work is to assess the potentialities of the X-ray powder diffraction technique as fingerprinting technique, i.e. as a preliminary tool to assess soil samples variability, in terms of geochemical features, in the context of food geographical traceability. A correct approach to sampling procedure is always a critical issue in scientific investigation. In particular, in food geographical traceability studies, where the cause-effect relations between the soil of origin and the final foodstuff is sought, a representative sampling of the territory under investigation is certainly an imperative. This research concerns a pilot study to investigate the field homogeneity with respect to both field extension and sampling depth, taking also into account the seasonal variability. Four Lambrusco production sites of the Modena district were considered. The X-Ray diffraction spectra, collected on the powder of each soil sample, were treated as fingerprint profiles to be deciphered by multivariate and multi-way data analysis, namely PCA and PARAFAC. The differentiation pattern observed in soil samples, as obtained by this fast and non-destructive analytical approach, well matches with the results obtained by characterization with other costly analytical techniques, such as ICP/MS, GFAAS, FAAS, etc. Thus, the proposed approach furnishes a rational basis to reduce the number of soil samples to be collected for further analytical characterization, i.e. metals content, isotopic ratio of radiogenic element, etc., while maintaining an exhaustive description of the investigated production areas. Copyright © 2012 Elsevier B.V. All rights reserved.

Micelle assisted thin-film solid phase microextraction: a new approach for determination of quaternary ammonium compounds in environmental samples.

Science.gov (United States)

Boyacı, Ezel; Pawliszyn, Janusz

2014-09-16

Determination of quaternary ammonium compounds (QACs) often is considered to be a challenging undertaking owing to secondary interactions of the analytes' permanently charged quaternary ammonium head or hydrophobic tail with the utilized labware. Here, for the first time, a micelle assisted thin-film solid phase microextraction (TF-SPME) using a zwitterionic detergent 3-[(3-cholamidopropyl)dimethylammonio]-1-propanesulfonate (CHAPS) as a matrix modifier is introduced as a novel approach for in-laboratory sample preparation of the challenging compounds. The proposed micelle assisted TF-SPME method offers suppression/enhancement free electrospray ionization of analytes in mass spectrometric detection, minimal interaction of the micelles with the TF-SPME coating, and chromatographic stationary phase and analysis free of secondary interactions. Moreover, it was found that the matrix modifier has multiple functions; when its concentration is found below the critical micelle concentration (CMC), the matrix modifier primarily acts as a surface deactivator; above its CMC, it acts as a stabilizer for QACs. Additionally, shorter equilibrium extraction times in the presence of the modifier demonstrated that micelles also assist in the transfer of analytes from the bulk of the sample to the surface of the coating. The developed micelle assisted TF-SPME protocol using the 96-blade system requires only 30 min of extraction and 15 min of desorption. Together with a conditioning step (15 min), the entire method is 60 min; considering the advantage of using the 96-blade system, if all the blades in the brush are used, the sample preparation time per sample is 0.63 min. Moreover, the recoveries for all analytes with the developed method were found to range within 80.2-97.3%; as such, this method can be considered an open bed solid phase extraction. The proposed method was successfully validated using real samples.

AW-101 entrained solids - Solubility versus temperature

International Nuclear Information System (INIS)

GJ Lumetta; RC Lettau; GF Piepel

2000-01-01

This report describes the results of a test conducted by Battelle to assess the solubility of the solids entrained in the diluted AW-101 low-activity waste (LAW) sample. BNFL requested Battelle to dilute the AW-1-1 sample using de-ionized water to mimic expected plant operating conditions. BNFL further requested Battelle to assess the solubility of the solids present in the diluted AW-101 sample versus temperature conditions of 30, 40, and 50 C. BNFL requested these tests to assess the composition of the LAW supernatant and solids versus expected plant-operating conditions. The work was conducted according to test plan BNFL-TP-29953-7, Rev. 0, Determination of the Solubility of LAW Entrained Solids. The test went according to plan, with no deviations from the test plan

A Headspace Solid Phase Microextraction (HS-SPME method for the chromatographic determination of alkylpyrazines in cocoa samples

Directory of Open Access Journals (Sweden)

Pini Gláucia F.

2004-01-01

Full Text Available A Headspace Solid Phase Microextraction (HS-SPME procedure for isolation and determination of alkylpyrazines in cocoa liquor, using Gas Chromatography with Flame Ionization Detection (GC-FID for the separation and detection of the analytes, is presented here. The HS-SPME operational conditions were optimized using extractions of samples spiked with known amounts of alkylpyrazines typically found on cocoa products. The maximum extraction efficiency was obtained using SPME fibers coated with 65 µm Carbowax/divinylbenzene. Additionally, the best results were achieved with extraction temperature of 60 ºC, 15 min of sample/headspace equilibration time and 45 min extraction time. It was also observed that suspending the samples in saturated aqueous NaCl solution during extractions resulted in a significant increment on the peak areas. This procedure was found to be effective to determine the so-called pyrazinic ratios (quotient between peak areas of alkylpyrazines, which are useful as quality parameters for cocoa liquor.

Headspace solid-phase microextraction with 1-pyrenyldiazomethane on-fibre derivatisation for analysis of fluoroacetic acid in biological samples.

Science.gov (United States)

Sporkert, Frank; Pragst, Fritz; Hübner, Sandra; Mills, Graham

2002-05-25

A new and in part automated headspace solid-phase microextraction method for quantitative determination of the highly toxic rodenticide fluoroacetic acid (FAA) in serum and other biological samples has been developed. FAA and deuterated acetic acid (internal standard) were extracted from acidified samples by a StableFlex divinylbenzene-Carboxen on polydimethylsiloxane fibre. The acids were derivatised on the fibre in-situ with 1-pyrenyldiazomethane and detected using gas chromatography-mass spectrometry with electron impact ionisation and selected ion monitoring. The calibration curve for FAA in serum was linear over the range from 0.02 to 5 microg/ml, with limits of detection and quantification of 0.02 and 0.07 microg/ml, respectively. The method was also tested with spiked whole blood, urine, stomach contents and kidney samples. It was sufficiently reliable, reproducible and sensitive for use in routine forensic toxicology applications.

Determination of submicrogram-per-liter concentrations of caffeine in surface water and groundwater samples by solid-phase extraction and liquid chromatography

Science.gov (United States)

Burkhardt, M.R.; Soliven, P.P.; Werner, S.L.; Vaught, D.G.

1999-01-01

A method for determining submicrogram-per-liter concentrations of caffeine in surface water and groundwater samples has been developed. Caffeine is extracted from a 1 L water sample with a 0.5 g graphitized carbon-based solid-phase cartridge, eluted with methylene chloride-methanol (80 + 20, v/v), and analyzed by liquid chromatography with photodiode-array detection. The single-operator method detection limit for organic-free water samples was 0.02 ??g/L. Mean recoveries and relative standard deviations were 93 ?? 13% for organicfree water samples fortified at 0.04 ??g/L and 84 ?? 4% for laboratory reagent spikes fortified at 0.5 ??g/L. Environmental concentrations of caffeine ranged from 0.003 to 1.44 ??g/L in surface water samples and from 0.01 to 0.08 ??g/L in groundwater samples.

Pressure-driven one-step solid phase-based on-chip sample preparation on a microfabricated plastic device and integration with flow-through polymerase chain reaction (PCR).

Science.gov (United States)

Tran, Hong Hanh; Trinh, Kieu The Loan; Lee, Nae Yoon

2013-10-01

In this study, we fabricate a monolithic poly(methylmethacrylate) (PMMA) microdevice on which solid phase-based DNA preparation and flow-through polymerase chain reaction (PCR) units were functionally integrated for one-step sample preparation and amplification operated by pressure. Chelex resin, which is used as a solid support for DNA preparation, can capture denatured proteins but releases DNA, and the purified DNA can then be used as a template in a subsequent amplification process. Using the PMMA microdevices, DNA was successfully purified from both Escherichia coli and human hair sample, and the plasmid vector inserted in E. coli and the D1S80 locus in human genomic DNA were successfully amplified from on-chip purified E. coli and human hair samples. Furthermore, the integration potential of the proposed sample preparation and flow-through PCR units was successfully demonstrate on a monolithic PMMA microdevice with a seamless flow, which could pave the way for a pressure-driven, simple one-step sample preparation and amplification with greatly decreased manufacture cost and enhanced device disposability. Copyright © 2013 Elsevier B.V. All rights reserved.

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)

Investigation of the Effect of Small Hardening Spots Created on the Sample Surface by Laser Complex with Solid-State Laser

Science.gov (United States)

Nozdrina, O.; Zykov, I.; Melnikov, A.; Tsipilev, V.; Turanov, S.

2018-03-01

This paper describes the results of an investigation of the effect of small hardening spots (about 1 mm) created on the surface of a sample by laser complex with solid-state laser. The melted area of the steel sample is not exceed 5%. Steel microhardness change in the region subjected to laser treatment is studied. Also there is a graph of the deformation of samples dependence on the tension. As a result, the yield plateau and plastic properties changes were detected. The flow line was tracked in the series of speckle photographs. As a result we can see how mm surface inhomogeneity can influence on the deformation and strength properties of steel.

Membrane solid-phase extraction: Field application for isolation of polycyclic aromatic hydrocarbons from water samples

International Nuclear Information System (INIS)

Furlong, E.T.; Koleis, J.C.; Gates, P.M.

1995-01-01

Solid-phase extraction (SPE) membranes (M-SPE) were used to isolate microgram-per-liter to nanogram-per-liter quantities of polycyclic aromatic hydrocarbons (PAH) in 4- to 8-liter ground-water samples from a crude-oil-contaminated ground-water site near Bemidji, Minnesota. The M-SPE method was evaluated (1) under laboratory conditions using reagent water fortified with individual PAH at 1.23 micrograms per liter, and (2) at the Bemidji site. At the site, ground-water samples were processed and PAH isolated using a M-SPE system connected directly to the well pump. Following sample isolation, all M-SPE samples were extracted using dichloromethane and analyzed by gas chromatography-mass spectrometry with selected-ion monitoring. Operationally, the M-SPE method provided a simple means to isolate PAH on site at the wellhead, particularly for anoxic water samples. Acceptable recoveries, ranging from 56 to over 100 percent, were observed for lower molecular weight PAH (naphthalene to pyrene) using the M-SPE method. Recoveries using M-SPE were somewhat lower, but reproducible, for higher molecular weight PAH (chrysene to benzo[ghi]perylene), ranging from 18 to 56 percent. M-SPE provides the capability to collect and field isolate PAH from a sufficiently large number of samples to identify environmental chemical processes occurring at individual compound concentrations of 50 to 1,200 nanograms per liter. Using M-SPE, the potential for facilitated transport of PAH by in situ-derived dissolved organic carbon (DOC) was evaluated at the site. Plots comparing DOC and PAH concentrations indicate that PAH concentrations increase exponentially with linear increases in DOC concentrations

Plasma emission induced by an Nd-YAG laser at low pressure on solid organic sample, its mechanism, and analytical application

International Nuclear Information System (INIS)

Suliyanti, Maria Margaretha; Sardy, Sar; Kusnowo, Anung; Hedwig, Rinda; Abdulmadjid, Syahrun Nur; Kurniawan, Koo Hendrik; Lie, T.J.; Pardede, Marincan; Kagawa, Kiichiro; Tjia, M.O.

2005-01-01

An Nd-YAG laser (1064 nm, 120 mJ, 8 ns) was focused on various types of solid organic samples such as a black acrylic plate, a black polyvinyl chloride plastic sheet, and a methoxy polyaniline film coated on the surface of a glass substrate, under a surrounding air pressure of 2 Torr. A modulated plasma technique was used to study the mechanism of excitation of the emission of the organic material. As a result, we conclude that ablated atoms and molecules are excited by a shock-wave mechanism, similar to the case of hard samples such as metal. The ablation speed of hydrogen emission (H I 656.2 nm) was examined and the results show that the release speed of the ablated atoms is relatively low (less than Mach 10) and persists for a longer period of time (around 1 μs); this phenomenon can be understood by assuming that the soft target absorbs recoil energy, causing a low release speed of ablated atoms which would form the shock wave. This was overcome by placing a subtarget on the back of the soft sample so as to enhance the repelling force, thus increasing the release speed of the atoms. A possible application of the low-pressure plasma on an organic solid was demonstrated in the detection of chlorine in a black polyvinyl chloride plastic sheet

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

2018-01-02

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.

On-line preconcentration of ultra-trace thallium(I in water samples with titanium dioxide nanoparticles and determination by graphite furnace atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Saeid Asadpour

2016-11-01

Full Text Available A new method has been developed for the determination of Tl(I based on simultaneous sorption and preconcentration with a microcolumn packed with TiO2 nanoparticle with a high specific surface area prepared by Sonochemical synthesis prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS. The optimum experimental parameters for preconcentration of thallium, such as elution condition, pH, and sample volume and flow rate have been investigated. Tl(I can be quantitatively retained by TiO2 nanoparticles at pH 9.0, then eluted completely with 1.0 mol L−1 HCl. The adsorption capacity of TiO2 nanoparticles for Tl(I was found to be 25 mg g−1. Also detection limit, precision (RSD, n = 8 and enrichment factor for Tl(I were 87 ng L−1, 6.4% and 100, respectively. The method has been applied for the determination of trace amounts of Tl(I in some environmental water samples with satisfactory results.

Modeling an in-register, parallel "iowa" aβ fibril structure using solid-state NMR data from labeled samples with rosetta.

Science.gov (United States)

Sgourakis, Nikolaos G; Yau, Wai-Ming; Qiang, Wei

2015-01-06

Determining the structures of amyloid fibrils is an important first step toward understanding the molecular basis of neurodegenerative diseases. For β-amyloid (Aβ) fibrils, conventional solid-state NMR structure determination using uniform labeling is limited by extensive peak overlap. We describe the characterization of a distinct structural polymorph of Aβ using solid-state NMR, transmission electron microscopy (TEM), and Rosetta model building. First, the overall fibril arrangement is established using mass-per-length measurements from TEM. Then, the fibril backbone arrangement, stacking registry, and "steric zipper" core interactions are determined using a number of solid-state NMR techniques on sparsely (13)C-labeled samples. Finally, we perform Rosetta structure calculations with an explicitly symmetric representation of the system. We demonstrate the power of the hybrid Rosetta/NMR approach by modeling the in-register, parallel "Iowa" mutant (D23N) at high resolution (1.2Å backbone rmsd). The final models are validated using an independent set of NMR experiments that confirm key features. Copyright © 2015 Elsevier Ltd. All rights reserved.

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).

Solid-phase microextraction for gas chromatographic/mass spectrometric analysis of dimethoate in human biological samples.

Science.gov (United States)

Gallardo, E; Barroso, M; Margalho, C; Cruz, A; Vieira, D N; López-Rivadulla, M

2006-01-01

A new, simple and rapid procedure for the determination of dimethoate in urine and blood samples was developed using direct immersion solid-phase microextraction and gas chromatography/mass spectrometry. This technique required only 0.1 mL of sample, and ethion was used as internal standard. Two types of coated fibre were compared (100 microm polydimethylsiloxane, and 65 microm Carbowax/divinylbenzene). Other parameters, such as extraction temperature, adsorption and desorption time, salt addition, agitation and pH, were optimized to enhance the sensitivity of the method. Limits of detection (LODs) and quantitation (LOQs) were 50 and 100 ng/mL for urine and 200 and 500 ng/mL for blood, respectively. The method was found to be linear between the LOQ and 40 microg/mL for urine, and between the LOQ and 50 microg/mL for blood, with correlation coefficients ranging from 0.9923-0.9996. Precision (intra- and interday) and accuracy were in conformity with the criteria normally accepted in bioanalytical method validation. The mean absolute recoveries of dimethoate were 1.24 and 0.50% for urine and blood, respectively. Because of its simplicity and the fact that small volumes of sample are used, the described method can be successfully used in the diagnosis of poisoning by this pesticide, namely in those situations where the sample volume is limited, as frequently occurs in forensic toxicology. Copyright 2006 John Wiley & Sons, Ltd.

Solid lubricants in the power station

International Nuclear Information System (INIS)

Gaensheimer, J.

1981-01-01

Example application are first outlined, followed by descriptions of inorganic solid lubricants and plastics. Waxes, soaps and salts are discussed. Notes for usage are given. Solid lubricants in oils and greases are comprehensively described, followed by the sections entitled Solid lubricants for gearboxes . References to samples, tests, standards and bibliography make up the conclusion. (orig.) [de

[Optimization of solid-phase extraction for enrichment of toxic organic compounds in water samples].

Science.gov (United States)

Zhang, Ming-quan; Li, Feng-min; Wu, Qian-yuan; Hu, Hong-ying

2013-05-01

A concentration method for enrichment of toxic organic compounds in water samples has been developed based on combined solid-phase extraction (SPE) to reduce impurities and improve recoveries of target compounds. This SPE method was evaluated in every stage to identify the source of impurities. Based on the analysis of Waters Oasis HLB without water samples, the eluent of SPE sorbent after dichloromethane and acetone contributed 85% of impurities during SPE process. In order to reduce the impurities from SPE sorbent, soxhlet extraction of dichloromethane followed by acetone and lastly methanol was applied to the sorbents for 24 hours and the results had proven that impurities were reduced significantly. In addition to soxhlet extraction, six types of prevalent SPE sorbents were used to absorb 40 target compounds, the lgK(ow) values of which were within the range of 1.46 and 8.1, and recovery rates were compared. It was noticed and confirmed that Waters Oasis HLB had shown the best recovery results for most of the common testing samples among all three styrenedivinylbenzene (SDB) polymer sorbents, which were 77% on average. Furthermore, Waters SepPak AC-2 provided good recovery results for pesticides among three types of activated carbon sorbents and the average recovery rates reached 74%. Therefore, Waters Oasis HLB and Waters SepPak AC-2 were combined to obtain a better recovery and the average recovery rate for the tested 40 compounds of this new SPE method was 87%.

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.

Sample Results From Tank 48H Samples HTF-48-14-158, -159, -169, and -170

Energy Technology Data Exchange (ETDEWEB)

Peters, T. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Hang, T. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

2015-04-28

Savannah River National Laboratory (SRNL) analyzed samples from Tank 48H in support of determining the cause for the unusually high dose rates at the sampling points for this tank. A set of two samples was taken from the quiescent tank, and two additional samples were taken after the contents of the tank were mixed. The results of the analyses of all the samples show that the contents of the tank have changed very little since the analysis of the previous sample in 2012. The solids are almost exclusively composed of tetraphenylborate (TPB) salts, and there is no indication of acceleration in the TPB decomposition. The filtrate composition shows a moderate increase in salt concentration and density, which is attributable to the addition of NaOH for the purposes of corrosion control. An older modeling simulation of the TPB degradation was updated, and the supernate results from a 2012 sample were run in the model. This result was compared to the results from the 2014 recent sample results reported in this document. The model indicates there is no change in the TPB degradation from 2012 to 2014. SRNL measured the buoyancy of the TPB solids in Tank 48H simulant solutions. It was determined that a solution of density 1.279 g/mL (~6.5M sodium) was capable of indefinitely suspending the TPB solids evenly throughout the solution. A solution of density 1.296 g/mL (~7M sodium) caused a significant fraction of the solids to float on the solution surface. As the experiments could not include the effect of additional buoyancy elements such as benzene or hydrogen generation, the buoyancy measurements provide an upper bound estimate of the density in Tank 48H required to float the solids.

Determination of polycyclic aromatic hydrocarbons in drinking water samples by solid-phase nanoextraction and high-performance liquid chromatography.

Science.gov (United States)

Wang, Huiyong; Campiglia, Andres D

2008-11-01

A novel alternative is presented for the extraction and preconcentration of polycyclic aromatic hydrocarbons (PAH) from water samples. The new approachwhich we have named solid-phase nanoextraction (SPNE)takes advantage of the strong affinity that exists between PAH and gold nanoparticles. Carefully optimization of experimental parameters has led to a high-performance liquid chromatography method with excellent analytical figures of merit. Its most striking feature correlates to the small volume of water sample (500 microL) for complete PAH analyses. The limits of detection ranged from 0.9 (anthracene) to 58 ng.L (-1) (fluorene). The relative standard deviations at medium calibration concentrations vary from 3.2 (acenaphthene) to 9.1% (naphthalene). The analytical recoveries from tap water samples of the six regulated PAH varied from 83.3 +/- 2.4 (benzo[ k]fluoranthene) to 95.7 +/- 4.1% (benzo[ g,h,i]perylene). The entire extraction procedure consumes less than 100 microL of organic solvents per sample, which makes it environmentally friendly. The small volume of extracting solution makes SPNE a relatively inexpensive extraction approach.

Direct Analysis of Amphetamine Stimulants in a Whole Urine Sample by Atmospheric Solids Analysis Probe Tandem Mass Spectrometry

Science.gov (United States)

Crevelin, Eduardo J.; Salami, Fernanda H.; Alves, Marcela N. R.; De Martinis, Bruno S.; Crotti, Antônio E. M.; Moraes, Luiz A. B.

2016-05-01

Amphetamine-type stimulants (ATS) are among illicit stimulant drugs that are most often used worldwide. A major challenge is to develop a fast and efficient methodology involving minimal sample preparation to analyze ATS in biological fluids. In this study, a urine pool solution containing amphetamine, methamphetamine, ephedrine, sibutramine, and fenfluramine at concentrations ranging from 0.5 pg/mL to 100 ng/mL was prepared and analyzed by atmospheric solids analysis probe tandem mass spectrometry (ASAP-MS/MS) and multiple reaction monitoring (MRM). A urine sample and saliva collected from a volunteer contributor (V1) were also analyzed. The limit of detection of the tested compounds ranged between 0.002 and 0.4 ng/mL in urine samples; the signal-to-noise ratio was 5. These results demonstrated that the ASAP-MS/MS methodology is applicable for the fast detection of ATS in urine samples with great sensitivity and specificity, without the need for cleanup, preconcentration, or chromatographic separation. Thus ASAP-MS/MS could potentially be used in clinical and forensic toxicology applications.

A Simple Method for Automated Solid Phase Extraction of Water Samples for Immunological Analysis of Small Pollutants.

Science.gov (United States)

Heub, Sarah; Tscharner, Noe; Kehl, Florian; Dittrich, Petra S; Follonier, Stéphane; Barbe, Laurent

2016-01-01

A new method for solid phase extraction (SPE) of environmental water samples is proposed. The developed prototype is cost-efficient and user friendly, and enables to perform rapid, automated and simple SPE. The pre-concentrated solution is compatible with analysis by immunoassay, with a low organic solvent content. A method is described for the extraction and pre-concentration of natural hormone 17β-estradiol in 100 ml water samples. Reverse phase SPE is performed with octadecyl-silica sorbent and elution is done with 200 µl of methanol 50% v/v. Eluent is diluted by adding di-water to lower the amount of methanol. After preparing manually the SPE column, the overall procedure is performed automatically within 1 hr. At the end of the process, estradiol concentration is measured by using a commercial enzyme-linked immune-sorbent assay (ELISA). 100-fold pre-concentration is achieved and the methanol content in only 10% v/v. Full recoveries of the molecule are achieved with 1 ng/L spiked de-ionized and synthetic sea water samples.

EDXRF applied to the chemical element determination of small invertebrate samples

Energy Technology Data Exchange (ETDEWEB)

Magalhaes, Marcelo L.R.; Santos, Mariana L.O.; Cantinha, Rebeca S.; Souza, Thomas Marques de; Franca, Elvis J. de, E-mail: marcelo_rlm@hotmail.com, E-mail: marianasantos_ufpe@hotmail.com, E-mail: rebecanuclear@gmail.com, E-mail: thomasmarques@live.com.pt, E-mail: ejfranca@cnen.gov.br [Centro Regional de Ciencias Nucleares do Nordeste (CRCN-NE/CNEN-PE), Recife, PE (Brazil)

2015-07-01

Energy Dispersion X-Ray Fluorescence - EDXRF is a fast analytical technique of easy operation, however demanding reliable analytical curves due to the intrinsic matrix dependence and interference during the analysis. By using biological materials of diverse matrices, multielemental analytical protocols can be implemented and a group of chemical elements could be determined in diverse biological matrices depending on the chemical element concentration. Particularly for invertebrates, EDXRF presents some advantages associated to the possibility of the analysis of small size samples, in which a collimator can be used that directing the incidence of X-rays to a small surface of the analyzed samples. In this work, EDXRF was applied to determine Cl, Fe, P, S and Zn in invertebrate samples using the collimator of 3 mm and 10 mm. For the assessment of the analytical protocol, the SRM 2976 Trace Elements in Mollusk produced and SRM 8415 Whole Egg Powder by the National Institute of Standards and Technology - NIST were also analyzed. After sampling by using pitfall traps, invertebrate were lyophilized, milled and transferred to polyethylene vials covered by XRF polyethylene. Analyses were performed at atmosphere lower than 30 Pa, varying voltage and electric current according to the chemical element to be analyzed. For comparison, Zn in the invertebrate material was also quantified by graphite furnace atomic absorption spectrometry after acid treatment (mixture of nitric acid and hydrogen peroxide) of samples have. Compared to the collimator of 10 mm, the SRM 2976 and SRM 8415 results obtained by the 3 mm collimator agreed well at the 95% confidence level since the E{sub n} Number were in the range of -1 and 1. Results from GFAAS were in accordance to the EDXRF values for composite samples. Therefore, determination of some chemical elements by EDXRF can be recommended for very small invertebrate samples (lower than 100 mg) with advantage of preserving the samples. (author)

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.

Solvent-free sample preparation by headspace solid-phase microextraction applied to the tracing of n-butyl nitrite abuse.

Science.gov (United States)

Tytgat, J; Daenens, P

1996-01-01

The most common alkyl nitrites encountered in forensic toxicology are iso-butyl, n-butyl and iso-pentyl(amyl) nitrites. All have become popular as an aphrodisiac, especially among the homosexual population. Alkyl nitrites are a volatile and unstable group of compounds, which hydrolyse in aqueous matrices to the alcohol and nitrite ion. Here we describe a fast, clean and sensitive procedure for the detection of hydrolysed n-butyl nitrite in whole human blood using a new, solvent-free sampling technique, the headspace solid-phase micro-extraction (HSPME), combined with GC/FID analysis. Sample preparation was investigated using two different stationary phases (100 microns polydimethylsiloxane and 85 microns polyacrylate), coating a fused silica fibre. The effect of different sampling times at fixed temperatures was also studied. Our results demonstrate that the HSPME/GC/FID procedure allows tracing of n-butyl nitrite abuse and detects hydrolysed n-butyl nitrite, i.e., released n-butanol, in whole blood at the 1 ng/mL level.

Magnetic solid-phase extraction of tetracyclines using ferrous oxide coated magnetic silica microspheres from water samples.

Science.gov (United States)

Lian, Lili; Lv, Jinyi; Wang, Xiyue; Lou, Dawei

2018-01-26

A novel magnetic solid-phase extraction approach was proposed for extraction of potential residues of tetracyclines (TCs) in tap and river water samples, based on Fe 3 O 4 @SiO 2 @FeO magnetic nanocomposite. Characterized results showed that the received Fe 3 O 4 @SiO 2 @FeO had distinguished magnetism and core-shell structure. Modified FeO nanoparticles with an ∼5 nm size distribution were homogeneously dispersed on the surface of the silica shell. Owing to the strong surface affinity of Fe (II) toward TCs, the magnetic nanocomposite could be applied to efficiently extract three TCs antibiotics, namely, oxytetracycline, tetracycline and chlortetracycline from water samples. Several factors, such as sorbent amount, pH condition, adsorption and desorption time, desorption solvent, selectivity and sample volume, influencing the extraction performance of TCs were investigated and optimized. The developed method showed excellent linearity (R > 0.9992) in the range of 0.133-333 μg L -1 , under optimized conditions. The limits of detection were between 0.027 and 0.107 μg L -1 for oxytetracycline, tetracycline and chlortetracycline, respectively. The feasibility of this method was evaluated by analysis of tap and river water samples. The recoveries at the spiked concentration levels ranged from 91.0% to 104.6% with favorable reproducibility (RSD < 4%). Copyright © 2017 Elsevier B.V. All rights reserved.

Streamlined sample cleanup using combined dispersive solid-phase extraction and in-vial filtration for analysis of pesticides and environmental pollutants in shrimp

Science.gov (United States)

A new method of sample preparation was developed and is reported for the first time. The approach combines in-vial filtration with dispersive solid-phase extraction (d-SPE) in a fast and convenient cleanup of QuEChERS (quick, easy, cheap, effective, rugged, and safe) extracts. The method was appli...

A Lab on a chip device for rapid identification of Avian Influenza virus by on-chip sample preparation and solid phase PCR

DEFF Research Database (Denmark)

Yi, Sun; Dhumpa, Raghuram; Bang, Dang Duong

2009-01-01

In this paper, we describe a novel lab-on-a-chip device for fast AIV screening by integrating DNA microarray-based solid phase PCR on microchip. The device can handle viral samples in an automatic way. Moreover, multiplex PCR and sequence detection are done in one-step, which greatly simplifies...

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.

Magnetic stirrer induced dispersive ionic-liquid microextraction for the determination of vanadium in water and food samples prior to graphite furnace atomic absorption spectrometry.

Science.gov (United States)

Naeemullah; Kazi, Tasneem Gul; Tuzen, Mustafa

2015-04-01

A new dispersive liquid-liquid microextraction, magnetic stirrer induced dispersive ionic-liquid microextraction (MS-IL-DLLME) was developed to quantify the trace level of vanadium in real water and food samples by graphite furnace atomic absorption spectrometry (GFAAS). In this extraction method magnetic stirrer was applied to obtained a dispersive medium of 1-butyl-3-methylimidazolium hexafluorophosphate [C4MIM][PF6] in aqueous solution of (real water samples and digested food samples) to increase phase transfer ratio, which significantly enhance the recovery of vanadium - 4-(2-pyridylazo) resorcinol (PAR) chelate. Variables having vital role on desired microextraction methods were optimised to obtain the maximum recovery of study analyte. Under the optimised experimental variables, enhancement factor (EF) and limit of detection (LOD) were achieved to be 125 and 18 ng L(-1), respectively. Validity and accuracy of the desired method was checked by analysis of certified reference materials (SLRS-4 Riverine water and NIST SRM 1515 Apple leaves). The relative standard deviation (RSD) for 10 replicate determinations at 0.5 μg L(-1) of vanadium level was found to be <5.0%. This method was successfully applied to real water and acid digested food samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

Utilizing a sequential injection system furnished with an extraction microcolumn as a novel approach for executing sequential extractions of metal species in solid samples

DEFF Research Database (Denmark)

Chomchoei, R.; Hansen, Elo Harald; Shiowatana, J.

2007-01-01

This communication presents a novel approach to perform sequential extraction of elements in solid samples by using a sequential injection (SI) system incorporating a specially designed extraction microcolumn. Based on the operation of the syringe pump, different modes of extraction are potentially...... that the system entails many advantages such as being fully automated, and besides being characterised by rapidity, ease of operation and robustness, it is less prone to risks of contamination and personal errors as encountered in traditional batch systems. Moreover, improvement of the precision and accuracy...... of the chemical fractionation of metal in solids as compared with previous reports are obtained. The system ensures that extraction is performed at designated pH values. Variation of sample weight to column volume ratios do not affect the amounts of extractable metals, nor do extraction flow rates ranging from 50...

Analytical results of Tank 38H core samples -- Fall 1999

International Nuclear Information System (INIS)

Swingle, R.F.

2000-01-01

Two samples were pulled from Tank 38H in the Fall of 1999: a variable depth sample (VDS) of the supernate was pulled in October and a core sample from the salt layer was pulled in December. Analysis of the rinse from the outside of the core sample indicated no sign of volatile or semivolatile organics. Both supernate and solids from the VDS and the dried core sample solids were analyzed for isotopes which could pose a criticality concern and also for elements which could serve as neutron poisons, as well as other elements. Results of the elemental analyses of these samples show significant elements present to mitigate the potential for nuclear criticality. However, it should be noted the results given for the VDS solids elemental analyses may be higher than the actual concentration in the solids, since the filter paper was dissolved along with the sample solids

Separation and preconcentration of Arsenic(III ions from aqueous media by adsorption on MWCNTs

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Nahid Tavakkoli

2017-05-01

Full Text Available A simple and sensitive method using mini-column packed with multi-walled carbon nanotubes (MWCNTs combined with graphite furnace atomic absorption spectrometry (GFAAS for preconcentration and determination of ultra trace amounts of As(III in an aqueous medium is proposed. The procedure is based on the solid phase extraction of the As(III-sodium diethyldithiocarbamate (As-NaDDTC chelate on MWCNTs. Various parameters such as the effect of pH, eluent type and volume, amount of sorbent, and matrix effects on the quantitative recoveries of analyte ions were evaluated. It was found that sorption is quantitative and desorption occurs with 4.0 mL of 3.0 mol L−1 HNO3 in acetone. The limit of detection of the method was 0.008 ng mL−1 for GFAAS with enrichment factor of 125 and the relative standard deviation (RSD 0.97% (n = 8, C = 10 ng mL−1. This method has been applied to the determination of ultra trace As(III in water and rice plant and its ash successfully.

Preconcentration and Determination of Perfluoroalkyl Substances (PFASs in Water Samples by Bamboo Charcoal-Based Solid-Phase Extraction Prior to Liquid Chromatography–Tandem Mass Spectrometry

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Ze-Hui Deng

2018-04-01

Full Text Available In this work, bamboo charcoal was used as solid-phase extraction adsorbent for the enrichment of six perfluoroalkyl acids (PFAAs in environmental water samples before liquid chromatography–tandem mass spectrometry analysis. The specific porous structure, high specific surface area, high porosity, and stability of bamboo charcoal were characterized. Several experimental parameters which considerably affect extraction efficiency were investigated and optimized in detail. The experimental data exhibited low limits of detection (LODs (0.01–1.15 ng/L, wide linear range (2–3 orders of magnitude and R ≥ 0.993 within the concentration range of 0.1–1000 ng/L, and good repeatability (2.7–5.0%, n = 5 intraday and 4.8–8.3%, n = 5 interday and reproducibility (5.3–8.0%, n = 3. Bamboo charcoal was successfully used for the enrichment and determination of PFAAs in real environmental water samples. The bamboo charcoal-based solid-phase extraction coupled with liquid chromatography–tandem mass spectrometry analysis possessed great potential in the determination of trace PFAA levels in environmental water samples.

Preparation and characterization of magnetic carboxylated nanodiamonds for vortex-assisted magnetic solid-phase extraction of ziram in food and water samples.

Science.gov (United States)

Yılmaz, Erkan; Soylak, Mustafa

2016-09-01

A simple and rapid vortex-assisted magnetic solid phase extraction (VA-MSPE) method for the separation and preconcentration of ziram (zinc dimethyldithiocarbamate), subsequent detection of the zinc in complex structure of ziram by flame atomic absorption spectrometry (AAS) has been developed. The ziram content was calculated by using stoichiometric relationship between the zinc and ziram. Magnetic carboxylated nanodiamonds (MCNDs) as solid-phase extraction adsorbent was prepared and characterized by Fourier transform infrared (FT-IR) spectra, X-ray diffraction (XRD) spectrometry and scanning electron microscopy (SEM). These magnetic carboxylated nanodiamonds carrying the ziram could be easily separated from the aqueous solution by applying an external magnetic field; no filtration or centrifugation was necessary. Some important factors influencing the extraction efficiency of ziram such as pH of sample solution, amount of adsorbent, type and volume of eluent, extraction and desorption time and sample volume were studied and optimized. The total extraction and detection time was lower than 10min The preconcentration factor (PF), the precision (RSD, n=7), the limit of detection (LOD) and limit of quantification (LOQ) were 160, 7.0%, 5.3µgL(-1) and 17.5µgL(-1), respectively. The interference of various ions has been examined and the method has been applied for the determination of ziram in various waters, foodstuffs samples and synthetic mixtures. Copyright © 2016 Elsevier B.V. All rights reserved.

Preconcentration of copper from natural water samples using ligand-less in situ surfactant-based solid phase extraction prior to FAAS determination

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Sayed Zia Mohammadi

2014-01-01

Full Text Available In the present work, a simple and rapid ligand-less, in situ, surfactant-based solid phase extraction for the preconcentration of copper in water samples was developed. In this method, a cationic surfactant (n-dodecyltrimethylammonium bromide was dissolved in an aqueous sample followed by the addition of an appropriate ion-pairing agent (ClO4-. Due to the interaction between the surfactant and ion-pairing agent, solid particles were formed and subsequently used for the adsorption of Cu(OH2 and CuI. After centrifugation, the sediment was dissolved in 1.0 mL of 1 mol L-1 HNO3 in ethanol and aspirated directly into the flame atomic absorption spectrometer. In order to obtain the optimum conditions, several parameters affecting the performance of the LL-ISS-SPE, including the volumes of DTAB, KClO4, and KI, pH, and potentially interfering ions, were optimized. It was found that KI and phosphate buffer solution (pH = 9 could extract more than 95% of copper ions. The amount of copper ions in the water samples varied from 3.2 to 4.8 ng mL-1, with relative standard deviations of 98.5%-103%. The determination of copper in water samples was linear over a concentration range of 0.5-200.0 ng mL-1. The limit of detection (3Sb/m was 0.1 ng mL-1 with an enrichment factor of 38.7. The accuracy of the developed method was verified by the determination of copper in two certified reference materials, producing satisfactory results.

Accelerated solvent extraction (ASE) - a fast and automated technique with low solvent consumption for the extraction of solid samples (T12)

International Nuclear Information System (INIS)

Hoefler, F.

2002-01-01

Full text: Accelerated solvent extraction (ASE) is a modern extraction technique that significantly streamlines sample preparation. A common organic solvent as well as water is used as extraction solvent at elevated temperature and pressure to increase extraction speed and efficiency. The entire extraction process is fully automated and performed within 15 minutes with a solvent consumption of 18 ml for a 10 g sample. For many matrices and for a variety of solutes, ASE has proven to be equivalent or superior to sonication, Soxhlet, and reflux extraction techniques while requiring less time, solvent and labor. First ASE has been applied for the extraction of environmental hazards from solid matrices. Within a very short time ASE was approved by the U.S. EPA for the extraction of BNAs, PAHs, PCBs, pesticides, herbicides, TPH, and dioxins from solid samples in method 3545. Especially for the extraction of dioxins the extraction time with ASE is reduced to 20 minutes in comparison to 18 h using Soxhlet. In food analysis ASE is used for the extraction of pesticide and mycotoxin residues from fruits and vegetables, the fat determination and extraction of vitamins. Time consuming and solvent intensive methods for the extraction of additives from polymers as well as for the extraction of marker compounds from herbal supplements can be performed with higher efficiencies using ASE. For the analysis of chemical weapons the extraction process and sample clean-up including derivatization can be automated and combined with GC-MS using an online ASE-APEC-GC system. (author)

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

International Nuclear Information System (INIS)

Lee, I-S.; Tsai, S.-W.

2008-01-01

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 deg. 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 μg 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

Development of near-field laser ablation inductively coupled plasma mass spectrometry for sub-micrometric analysis of solid samples

International Nuclear Information System (INIS)

Jabbour, Chirelle

2016-01-01

A near field laser ablation method was developed for chemical analysis of solid samples at sub-micrometric scale. This analytical technique combines a nanosecond laser Nd:YAG, an atomic Force Microscope (AFM), and an inductively coupled plasma mass spectrometer (ICPMS). In order to improve the spatial resolution of the laser ablation process, the near-field enhancement effect was applied by illuminating, by the laser beam, the apex of the AFM conductive sharp tip maintained at a few nanometers (5 to 30 nm) above the sample surface. The interaction between the illuminated tip and the sample surface enhances locally the incident laser energy and leads to the ablation process. By applying this technique to conducting gold and tantalum samples, and semiconducting silicon sample, a lateral resolution of 100 nm and depths of a few nanometers were demonstrated. Two home-made numerical codes have enabled the study of two phenomena occurring around the tip: the enhancement of the laser electrical field by tip effect, and the induced laser heating at the sample surface. The influence of the main operating parameters on these two phenomena, amplification and heating, was studied. an experimental multi-parametric study was carried out in order to understand the effect of different experimental parameters (laser fluence, laser wavelength, number of laser pulses, tip-to-sample distance, sample and tip nature) on the near-field laser ablation efficiency, crater dimensions and amount of ablated material. (author) [fr

Method optimization for non-equilibrium solid phase microextraction sampling of HAPs for GC/MS analysis

Science.gov (United States)

Zawadowicz, M. A.; Del Negro, L. A.

2010-12-01

Hazardous air pollutants (HAPs) are usually present in the atmosphere at pptv-level, requiring measurements with high sensitivity and minimal contamination. Commonly used evacuated canister methods require an overhead in space, money and time that often is prohibitive to primarily-undergraduate institutions. This study optimized an analytical method based on solid-phase microextraction (SPME) of ambient gaseous matrix, which is a cost-effective technique of selective VOC extraction, accessible to an unskilled undergraduate. Several approaches to SPME extraction and sample analysis were characterized and several extraction parameters optimized. Extraction time, temperature and laminar air flow velocity around the fiber were optimized to give highest signal and efficiency. Direct, dynamic extraction of benzene from a moving air stream produced better precision (±10%) than sampling of stagnant air collected in a polymeric bag (±24%). Using a low-polarity chromatographic column in place of a standard (5%-Phenyl)-methylpolysiloxane phase decreased the benzene detection limit from 2 ppbv to 100 pptv. The developed method is simple and fast, requiring 15-20 minutes per extraction and analysis. It will be field-validated and used as a field laboratory component of various undergraduate Chemistry and Environmental Studies courses.

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

Science.gov (United States)

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

2018-06-15

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

Rapid screening of selective serotonin re-uptake inhibitors in urine samples using solid-phase microextraction gas chromatography-mass spectrometry.

Science.gov (United States)

Salgado-Petinal, Carmen; Lamas, J Pablo; Garcia-Jares, Carmen; Llompart, Maria; Cela, Rafael

2005-07-01

In this paper a solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS) method is proposed for a rapid analysis of some frequently prescribed selective serotonin re-uptake inhibitors (SSRI)-venlafaxine, fluvoxamine, mirtazapine, fluoxetine, citalopram, and sertraline-in urine samples. The SPME-based method enables simultaneous determination of the target SSRI after simple in-situ derivatization of some of the target compounds. Calibration curves in water and in urine were validated and statistically compared. This revealed the absence of matrix effect and, in consequence, the possibility of quantifying SSRI in urine samples by external water calibration. Intra-day and inter-day precision was satisfactory for all the target compounds (relative standard deviation, RSD, detection limits achieved were detected and tentatively identified.

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.

The use of EURACHEM guide for comparison of two 210Pb determination methods in solid environmental samples

International Nuclear Information System (INIS)

Al-Masri, M. S.; Hassan, M.; Amin, Y.

2008-07-01

Two techniques for determination of 210 Pb in solid environmental samples have been validated and compared according to Eurachem Guide on method validation. The first technique depended on determination of 210 Po, which equilibrium with 210 Pb, by platting it onto a rotating silver disc. Then, Alpha counting of 210 Po was done using an alpha spectrometer. On the other hand, according to its decay scheme, 210 Pb was measured directly through gamma spectrometry by measuring the 46.5 keV. Detection limits, reproducibility and recovery coefficient were the main validation parameters. In addition, uncertainties of measurement were estimated and compared for the two techniques. The comparison results have shown that, the activity of 210 Pb in the environmental samples can choose which technique is appropriated. It was found that Eurachem Guide and comparison of quality statistical validation parameters can be a good tool for selection of the appropriate method for the application. (Authors)

Role of nanoparticles in analytical solid phase microextraction (SPME)

NARCIS (Netherlands)

Zielinska, K.; Leeuwen, van H.P.

2013-01-01

Solid phase microextraction (SPME) is commonly used to measure the free concentration of fairly hydrophobic substances in aqueous media on the basis of their partitioning between sample solution and a solid phase. Here we study the role of nanoparticles that may sorb the analyte in the sample

The Applicability of the Distribution Coefficient, KD, Based on Non-Aggregated Particulate Samples from Lakes with Low Suspended Solids Concentrations.

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Aine Marie Gormley-Gallagher

Full Text Available Separate phases of metal partitioning behaviour in freshwater lakes that receive varying degrees of atmospheric contamination and have low concentrations of suspended solids were investigated to determine the applicability of the distribution coefficient, KD. Concentrations of Pb, Ni, Co, Cu, Cd, Cr, Hg and Mn were determined using a combination of filtration methods, bulk sample collection and digestion and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS. Phytoplankton biomass, suspended solids concentrations and the organic content of the sediment were also analysed. By distinguishing between the phytoplankton and (inorganic lake sediment, transient variations in KD were observed. Suspended solids concentrations over the 6-month sampling campaign showed no correlation with the KD (n = 15 for each metal, p > 0.05 for Mn (r2 = 0.0063, Cu (r2 = 0.0002, Cr (r2 = 0.021, Ni (r2 = 0.0023, Cd (r2 = 0.00001, Co (r2 = 0.096, Hg (r2 = 0.116 or Pb (r2 = 0.164. The results implied that colloidal matter had less opportunity to increase the dissolved (filter passing fraction, which inhibited the spurious lowering of KD. The findings conform to the increasingly documented theory that the use of KD in modelling may mask true information on metal partitioning behaviour. The root mean square error of prediction between the directly measured total metal concentrations and those modelled based on the separate phase fractions were ± 3.40, 0.06, 0.02, 0.03, 0.44, 484.31, 80.97 and 0.1 μg/L for Pb, Cd, Mn, Cu, Hg, Ni, Cr and Co respectively. The magnitude of error suggests that the separate phase models for Mn and Cu can be used in distribution or partitioning models for these metals in lake water.

Assessment of metal concentrations in sediment samples from Billings Reservoir, Rio Grande tributary, Sao Paulo, Brazil

International Nuclear Information System (INIS)

Bostelmann, Eleine

2006-01-01

The present study chemically characterized sediment samples from the Billings reservoir, Rio Grande tributary, in the Metropolitan region of Sao Paulo, by determining metal concentration and other elements of interest. The chosen chemical parameters for this characterization were Aluminum, Arsenic, Barium, Cadmium, Copper, Chromium, Iron, Lead, Manganese, Mercury, Nickel, Selenium and Zinco. These parameters are also used in the water quality index, with the exception of Selenium. The concentrations were determined through different analytical techniques such as atomic absorption spectrometry (FAAS, GFAAS and CVAAS), optical emission spectrometry (ICP OES) and neutron activation analysis. These analytical methodologies were assessed for precision, accuracy and detection and/or quantification limits for the sediment elements in question. Advantages and disadvantages of each technique for each element and its concentration were also discussed. From these assessments the most adequate technique was selected for the routine analysis of sediment samples for each element concentration determination. This assessment verified also that digestion in a closed microwave system with nitric acid is efficient for the evaluation of extracted metals of environmental interest. The analytical techniques chosen were equally efficient for metals determination. In the case of Cd and Pb, the FAAS technique was selected due to better results than ICP OES, as it does not present matrix interference. The concentration values obtained for metals As, Cd, Cu, Cr, Hg, Ni, Pb and Zn in the sediment samples were compared to Canadian Council of Minister of the Environment (CCME) TEL and PEL values. (author)

Assessment of metal concentrations in sediment samples from Billings reservoir, Rio Grande tributary, Sao Paulo, Brazil

International Nuclear Information System (INIS)

Bostelmann, Eleine

2006-01-01

The present study chemically characterized sediment samples from the Billings reservoir, Rio Grande tributary, in the Metropolitan region of Sao Paulo, by determining metal concentration and other elements of interest. The chosen chemical parameters for this characterization were Aluminum, Arsenic, Barium, Cadmium, Copper, Chromium, Iron, Lead, Manganese, Mercury, Nickel, Selenium and Zinc. These parameters are also used in the water quality index, with the exception of Selenium. The concentrations were determined through different analytical techniques such as atomic absorption spectrometry (FAAS, GFAAS and CVAAS), optical emission spectrometry (ICP OES) and neutron activation analysis. These analytical methodologies were assessed for precision, accuracy and detection and/or quantification limits for the sediment elements in question. Advantages and disadvantages of each technique for each element and its concentration were also discussed. From these assessment the most adequate technique was selected for the routine analysis of sediment samples for each element concentration determination. This assessment verified also that digestion in a closed microwave system with nitric acid is efficient for the evaluation of extracted metals of environmental interest. The analytical techniques chosen were equally efficient for metals determination. In the case of Cd and Pb, the FAAS technique was selected due to better results than ICP OES, as it does not present matrix interference. The concentration values obtained for metals As, Cd, Cu, Cr, Hg, Ni, Pb and Zn in the sediment samples were compared to Canadian Council of Minister of the Environment (CCME) TEL and PEL values. (author)

Solid phase speciation of arsenic by sequential extraction in standard reference materials and industrially contaminated soil samples

International Nuclear Information System (INIS)

Herreweghe, Samuel van; Swennen, Rudy; Vandecasteele, Carlo; Cappuyns, Valerie

2003-01-01

Leaching experiments, a mineralogical survey and larger samples are preferred when arsenic is present as discrete mineral phases. - Availability, mobility, (phyto)toxicity and potential risk of contaminants is strongly affected by the manner of appearance of elements, the so-called speciation. Operational fractionation methods like sequential extractions have been applied for a long time to determine the solid phase speciation of heavy metals since direct determination of specific chemical compounds can not always be easily achieved. The three-step sequential extraction scheme recommended by the BCR and two extraction schemes based on the phosphorus-like protocol proposed by Manful (1992, Occurrence and Ecochemical Behaviours of Arsenic in a Goldsmelter Impacted Area in Ghana, PhD dissertation, at the RUG) were applied to four standard reference materials (SRM) and to a batch of samples from industrially contaminated sites, heavily contaminated with arsenic and heavy metals. The SRM 2710 (Montana soil) was found to be the most useful reference material for metal (Mn, Cu, Zn, As, Cd and Pb) fractionation using the BCR sequential extraction procedure. Two sequential extraction schemes were developed and compared for arsenic with the aim to establish a better fractionation and recovery rate than the BCR-scheme for this element in the SRM samples. The major part of arsenic was released from the heavily contaminated samples after NaOH-extraction. Inferior extraction variability and recovery in the heavily contaminated samples compared to SRMs could be mainly contributed to subsample heterogeneity

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.

Investigation of Tank 241-AN-101 Floating Solids

Energy Technology Data Exchange (ETDEWEB)

Kraft, Douglas P. [Washington River Protection Solutions, LLC, Richland, VA (United States); Meznarich, H. K. [Washington River Protection Solutions, LLC, Richland, VA (United States)

2017-10-30

Tank 241-AN-101 is the receiver tank for retrieval of several C-Farms waste tanks, including Tanks 241-C-102 and 241-C-111. Tank 241 C 111 received first-cycle decontamination waste from the bismuth phosphate process and Plutonium and Uranium Extraction cladding waste, as well as hydraulic fluid. Three grab samples, 1AN-16-01, 1AN-16-01A, and 1AN-16-01B, were collected at the surface of Tank 241-AN-101 on April 25, 2016, after Tank 241-C-111 retrieval was completed. Floating solids were observed in the three grab samples in the 11A hot cell after the samples were received at the 222-S Laboratory. Routine chemical analyses, solid phase characterization on the floating and settled solids, semivolatile organic analysis mainly on the aqueous phase for identification of degradation products of hydraulic fluids were performed. Investigation of the floating solids is reported.

Analysis of non-esterified fatty acids in human samples by solid-phase-extraction and gas chromatography/mass spectrometry.

Science.gov (United States)

Kopf, Thomas; Schmitz, Gerd

2013-11-01

The determination of the fatty acid (FA) profile of lipid classes is essential for lipidomic analysis. We recently developed a GC/MS-method for the analysis of the FA profile of total FAs, i.e. the totality of bound and unbound FAs, in any given biological sample (TOFAs). Here, we present a method for the analysis of non-esterified fatty acids (NEFAs) in biological samples, i.e. the fraction that is present as extractable free fatty acids. Lipid extraction is performed according to Dole using 80/20 2-propanol/n-hexane (v/v), with 0.1% H2SO4. The fatty acid-species composition of this NEFA-fraction is determined as FAME after derivatization with our GC/MS-method on a BPX column (Shimadzu). Validation of the NEFA-method presented was performed in human plasma samples. The validated method has been used with human plasma, cells and tissues, as well as mammalian body fluids and tissue samples. The newly developed solid-phase-extraction (SPE)-GC-MS method allows the rapid separation of the NEFA-fraction from a neutral lipid extract of plasma samples. As a major advantage compared to G-FID-methods, GC-MS allows the use of stable isotope labeled fatty acid precursors to monitor fatty acid metabolism. Copyright © 2013 Elsevier B.V. All rights reserved.

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 -

Possibilities of municipal solid waste incinerator fly ash utilisation.

Science.gov (United States)

Hartmann, Silvie; Koval, Lukáš; Škrobánková, Hana; Matýsek, Dalibor; Winter, Franz; Purgar, Amon

2015-08-01

Properties of the waste treatment residual fly ash generated from municipal solid waste incinerator fly ash were investigated in this study. Six different mortar blends with the addition of the municipal solid waste incinerator fly ash were evaluated. The Portland cement replacement levels of the municipal solid waste incinerator fly ash used were 25%, 30% and 50%. Both, raw and washed municipal solid waste incinerator fly ash samples were examined. According to the mineralogical composition measurements, a 22.6% increase in the pozzolanic/hydraulic properties was observed for the washed municipal solid waste incinerator fly ash sample. The maximum replacement level of 25% for the washed municipal solid waste incinerator fly ash in mortar blends was established in order to preserve the compressive strength properties. Moreover, the leaching characteristics of the crushed mortar blend was analysed in order to examine the immobilisation of its hazardous contents. © The Author(s) 2015.

characterization and composition analysis of municipal solid waste

African Journals Online (AJOL)

userpc

ABSTRACT. Municipal Solid Waste (MSW) is produced through human activities and in the last two ... Solid waste samples were collected and analysed from the four major dumpsites in ..... Technology, Ueberlandstrasse 133,. Switzerland.

Ultrathin-shell boron nitride hollow spheres as sorbent for dispersive solid-phase extraction of polychlorinated biphenyls from environmental water samples.

Science.gov (United States)

Fu, Meizhen; Xing, Hanzhu; Chen, Xiangfeng; Chen, Fan; Wu, Chi-Man Lawrence; Zhao, Rusong; Cheng, Chuange

2014-11-21

Boron nitride hollow spheres with ultrathin-shells were synthesized and used as sorbents for dispersive solid-phase extraction of aromatic pollutants at trace levels from environmental water samples. Polychlorinated biphenyls (PCBs) were selected as target compounds. Sample quantification and detection were performed by gas chromatography-tandem mass spectrometry. Extraction parameters influencing the extraction efficiency were optimized through response surface methodology using the Box-Behnken design. The proposed method achieved good linearity within the concentration range of 0.15-250 ng L(-1) PCBs, low limits of detection (0.04-0.09 ng L(-1), S/N=3:1), good repeatability of the extractions (relative standard deviation, spring waters were analyzed using the developed method. Results demonstrated that the hexagonal boron nitride-based material has significant potential as a sorbent for organic pollutant extraction from environmental water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Laboratory Sampling Guide

Science.gov (United States)

2012-05-11

environment, and by ingestion of foodstuffs that have incorporated C-14 by photosynthesis . Like tritium, C-14 is a very low energy beta emitter and is... bacterial growth and to minimize development of solids in the sample. • Properly identify each sample container with name, SSN, and collection start and...sampling in the same cardboard carton. The sample may be kept cool or frozen during collection to control odor and bacterial growth. • Once

Fabrication of a novel hydrophobic/ion-exchange mixed-mode adsorbent for the dispersive solid-phase extraction of chlorophenols from environmental water samples.

Science.gov (United States)

Gao, Li; Wei, Yinmao

2016-08-01

A novel mixed-mode adsorbent was prepared by functionalizing silica with tris(2-aminoethyl)amine and 3-phenoxybenzaldehyde as the main mixed-mode scaffold due to the presence of the plentiful amino groups and benzene rings in their molecules. The adsorption mechanism was probed with acidic, natural and basic compounds, and the mixed hydrophobic and ion-exchange interactions were found to be responsible for the adsorption of analytes. The suitability of dispersive solid-phase extraction was demonstrated in the determination of chlorophenols in environmental water. Several parameters, including sample pH, desorption solvent, ionic strength, adsorbent dose, and extraction time were optimized. Under the optimal extraction conditions, the proposed dispersive solid-phase extraction coupled with high-performance liquid chromatography showed good linearity range and acceptable limits of detection (0.22∽0.54 ng/mL) for five chlorophenols. Notably, the higher extraction recoveries (88.7∽109.7%) for five chlorophenols were obtained with smaller adsorbent dose (10 mg) and shorter extraction time (15 min) compared with the reported methods. The proposed method might be potentially applied in the determination of trace chlorophenols in real water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

K West Basin Sand Filter Backwash Sample Analysis

Energy Technology Data Exchange (ETDEWEB)

Fiskum, Sandra K. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Smoot, Margaret R. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Coffey, Deborah S. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Pool, Karl N. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

2016-03-01

A sand filter is used to help maintain water clarity at the K West Basin where highly radioactive sludge is stored. Eventually that sand filter will require disposal. The radionuclide content of the solids trapped in the sand filter will affect the selection of the sand filter disposal pathway. The Pacific Northwest National Laboratory (PNNL) was contracted by the K Basin Operations & Plateau Remediation Project (operations contractor CH2M Hill) to analyze the radionuclide content of the solids collected from the backwash of the K West Basin sand filter. The radionuclide composition in the sand filter backwash solids will be used by CH2M Hill to determine if the sand filter media and retained sludge solids will be designated as transuranic waste for disposal purposes or can be processed through less expensive means. On October 19, 2015, K Basin Operations & Plateau Remediation Project staff backwashed the sand filter into the North Load-Out Pit (NLOP) and immediately collected sample slurry from a sampling tube positioned 24 in. above the NLOP floor. The 764 g sand filter backwash slurry sample, KW-105 SFBW-001, was submitted to PNNL for analysis on October 20, 2015. Solids from the slurry sample were consolidated into two samples (i.e., a primary and a duplicate sample) by centrifuging and measured for mass (0.82 g combined – wet centrifuged solids basis) and volume (0.80 mL combined). The solids were a dark brown/orange color, consistent with iron oxide/hydroxide. The solids were dried; the combined dry solids mass was 0.1113 g, corresponding to 0.0146 weight percent (wt%) solids in the original submitted sample slurry. The solids were acid-digested using nitric and hydrochloric acids. Insoluble solids developed upon dilution with 0.5 M HNO₃, corresponding to an average 6.5 wt% of the initial dry solids content. The acid digestate and insoluble solids were analyzed separately by gamma spectrometry. Nominally, 7.7% of the ⁶⁰Co was present

Solid recovered fuels in the cement industry--semi-automated sample preparation unit as a means for facilitated practical application.

Science.gov (United States)

Aldrian, Alexia; Sarc, Renato; Pomberger, Roland; Lorber, Karl E; Sipple, Ernst-Michael

2016-03-01

One of the challenges for the cement industry is the quality assurance of alternative fuel (e.g., solid recovered fuel, SRF) in co-incineration plants--especially for inhomogeneous alternative fuels with large particle sizes (d95⩾100 mm), which will gain even more importance in the substitution of conventional fuels due to low production costs. Existing standards for sampling and sample preparation do not cover the challenges resulting from these kinds of materials. A possible approach to ensure quality monitoring is shown in the present contribution. For this, a specially manufactured, automated comminution and sample divider device was installed at a cement plant in Rohožnik. In order to prove its practical suitability with methods according to current standards, the sampling and sample preparation process were validated for alternative fuel with a grain size >30 mm (i.e., d95=approximately 100 mm), so-called 'Hotdisc SRF'. Therefore, series of samples were taken and analysed. A comparison of the analysis results with the yearly average values obtained through a reference investigation route showed good accordance. Further investigations during the validation process also showed that segregation or enrichment of material throughout the comminution plant does not occur. The results also demonstrate that compliance with legal standards regarding the minimum sample amount is not sufficient for inhomogeneous and coarse particle size alternative fuels. Instead, higher sample amounts after the first particle size reduction step are strongly recommended in order to gain a representative laboratory sample. © The Author(s) 2016.

Determination of Ultra-trace Rhodium in Water Samples by Graphite Furnace Atomic Absorption Spectrometry after Cloud Point Extraction Using 2-(5-Iodo-2-Pyridylazo)-5-Dimethylaminoaniline as a Chelating Agent.

Science.gov (United States)

Han, Quan; Huo, Yanyan; Wu, Jiangyan; He, Yaping; Yang, Xiaohui; Yang, Longhu

2017-03-24

A highly sensitive method based on cloud point extraction (CPE) separation/preconcentration and graphite furnace atomic absorption spectrometry (GFAAS) detection has been developed for the determination of ultra-trace amounts of rhodium in water samples. A new reagent, 2-(5-iodo-2-pyridylazo)-5-dimethylaminoaniline (5-I-PADMA), was used as the chelating agent and the nonionic surfactant TritonX-114 was chosen as extractant. In a HAc-NaAc buffer solution at pH 5.5, Rh(III) reacts with 5-I-PADMA to form a stable chelate by heating in a boiling water bath for 10 min. Subsequently, the chelate is extracted into the surfactant phase and separated from bulk water. The factors affecting CPE were investigated. Under the optimized conditions, the calibration graph was linear in the range of 0.1-6.0 ng/mL, the detection limit was 0.023 ng/mL for rhodium and relative standard deviation was 3.67% ( c = 1.0 ng/mL, n = 11)．The method has been applied to the determination of trace rhodium in water samples with satisfactory results.

Magnetic molecularly imprinted polymer nanoparticles for the solid-phase extraction of paracetamole from plasma samples, followed its determination by HPLC

International Nuclear Information System (INIS)

Azodi-Deilami, Saman; Najafabadi, Alireza Hassani; Asadi, Ebadullah; Abdouss, Majid; Kordestani, Davood

2014-01-01

We are presenting magnetic molecularly imprinted polymer nanoparticles (m-MIPs) for solid-phase extraction and sample clean-up of paracetamole. The m-MIPs were prepared from magnetite (Fe 3 O 4 ) as the magnetic component, paracetamole as the template, methacrylic acid as a functional monomer, and 2-(methacrylamido) ethyl methacrylate as a cross-linker. The m-MIPs were then characterized by transmission electron microscopy, FT-IR spectroscopy, X-ray diffraction and vibrating sample magnetometry. The m-MIPs were applied to the extraction of paracetamole from human blood plasma samples. Following its elution from the column loaded with the m-MIPs with an acetonitrile-buffer (9:1) mixture, it was submitted to HPLC analysis. Paracetamole can be quantified by this method in the 1 μg L −1 to 300 μg L −1 concentration range. The limit of detection and limit of quantification in plasma samples are 0.17 and 0.4 μg L −1 . The preconcentration factor of the m-MIPs is 40. The HPLC method shows good precision (4.5 % at 50 μg L −1 levels) and recoveries (between 83 and 91 %) from spiked plasma samples. (author)

Solid-phase extraction versus matrix solid-phase dispersion: Application to white grapes.

Science.gov (United States)

Dopico-García, M S; Valentão, P; Jagodziñska, A; Klepczyñska, J; Guerra, L; Andrade, P B; Seabra, R M

2007-11-15

The use of matrix solid-phase dispersion (MSPD) was tested to, separately, extract phenolic compounds and organic acids from white grapes. This method was compared with a more conventional analytical method previously developed that combines solid liquid extraction (SL) to simultaneously extract phenolic compounds and organic acids followed by a solid-phase extraction (SPE) to separate the two types of compounds. Although the results were qualitatively similar for both techniques, the levels of extracted compounds were in general quite lower on using MSPD, especially for organic acids. Therefore, SL-SPE method was preferred to analyse white "Vinho Verde" grapes. Twenty samples of 10 different varieties (Alvarinho, Avesso, Asal-Branco, Batoca, Douradinha, Esganoso de Castelo Paiva, Loureiro, Pedernã, Rabigato and Trajadura) from four different locations in Minho (Portugal) were analysed in order to study the effects of variety and origin on the profile of the above mentioned compounds. Principal component analysis (PCA) was applied separately to establish the main sources of variability present in the data sets for phenolic compounds, organic acids and for the global data. PCA of phenolic compounds accounted for the highest variability (77.9%) with two PCs, enabling characterization of the varieties of samples according to their higher content in flavonol derivatives or epicatechin. Additionally, a strong effect of sample origin was observed. Stepwise linear discriminant analysis (SLDA) was used for differentiation of grapes according to the origin and variety, resulting in a correct classification of 100 and 70%, respectively.

Determination of clenbuterol in bovine liver by combining matrix solid phase dispersion and molecularly imprinted solid phase extraction followed by liquid chromatography/electrospray ion trap multiple stage mass spectrometry

NARCIS (Netherlands)

Crescenzi, C; Bayoudh, S; Cormack, P.A G; Klein, T; Ensing, K

2001-01-01

Matrix solid-phase dispersion(MSPD) is a new sample pretreatment for solid samples. This technique greatly simplifies sample pretreatment but, nonetheless, the extracts often still require an extra cleanup step that is both laborious and time-consuming. The potential;of combining MSPD with

Increase by order of magnitude in quality factor during Cherenkov radiation detection in samples on solid carriers in glass cuvettes Kavalier

International Nuclear Information System (INIS)

Podracka, E.; Tykva, R.

The method of measuring Cherenkov radiation is discussed developed by the authors, based on measuring samples on a solid carrier in glass scintillation cuvettes Kavalier. Increased interaction of emitted beta particles and modified measurement configuration were achieved by putting polyethylene foils of 0.3 mm in thickness and 17 mm in diameter straight to the sample or inserting a polyethylene tube of 13 mm in length and 15 mm in diameter down to the bottom of the cuvette in whose axis the sample is mounted. The application of the said technique can increase the quality factor by an order of magnitude when Czechoslovak-made cuvettes are used and a significantly higher value of quality factor can be obtained than when peak standard cuvettes imported from abroad and the original Huelsen and Prenzel's procedure are used. (B.S.)

???????????? SolidWorks/SolidWorks Flow Simulation/SolidWorks Simulation ??? ?????????? ???????? ?? ????????????? ???

OpenAIRE

????????????, ?. ?.; ????????, ?. ?.; ?????, ?. ?.

2012-01-01

? ?????? ???????? ??????? ??????? ???????? ?? ???????????? ??????????? ????????? SolidWorks/SolidWorks Flow Simulation (COSMOSFloWorks)/SolidWorks Simulation ??? ?????????? ???????? ?? ????????????? ???. ??? ???????? ????????? ???????? ?????????? ?? ?????? ???????? ??????? ? ????????????? ?????? ? ????????????? ????????????? ?????????? ???????????? SolidWorks Flow Simulation (COSMOSFloWorks). ??? ???????????? ??????????? ????????????? ?????? ?? ????????? ??????????? ??????? ?? ??????????? ...

Optimization and application of octadecyl-modified monolithic silica for solid-phase extraction of drugs in whole blood samples.

Science.gov (United States)

Namera, Akira; Saito, Takeshi; Ota, Shigenori; Miyazaki, Shota; Oikawa, Hiroshi; Murata, Kazuhiro; Nagao, Masataka

2017-09-29

Monolithic silica in MonoSpin for solid-phase extraction of drugs from whole blood samples was developed to facilitate high-throughput analysis. Monolithic silica of various pore sizes and octadecyl contents were synthesized, and their effects on recovery rates were evaluated. The silica monolith M18-200 (20μm through-pore size, 10.4nm mesopore size, and 17.3% carbon content) achieved the best recovery of the target analytes in whole blood samples. The extraction proceeded with centrifugal force at 1000rpm for 2min, and the eluate was directly injected into the liquid chromatography-mass spectrometry system without any tedious steps such as evaporation of extraction solvents. Under the optimized condition, low detection limits of 0.5-2.0ngmL -1 and calibration ranges up to 1000ngmL -1 were obtained. The recoveries of the target drugs in the whole blood were 76-108% with relative standard deviation of less than 14.3%. These results indicate that the developed method based on monolithic silica is convenient, highly efficient, and applicable for detecting drugs in whole blood samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Nanostructured conducting molecularly imprinted polymer for selective extraction of salicylate from urine and serum samples by electrochemically controlled solid-phase micro-extraction

Energy Technology Data Exchange (ETDEWEB)

Ameli, Akram [Department of Chemistry, Faculty of Science, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Alizadeh, Naader, E-mail: alizaden@modares.ac.ir [Department of Chemistry, Faculty of Science, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of)

2011-11-30

Highlights: Black-Right-Pointing-Pointer Overoxidized polypyrrole templated with salicylate has been utilized as conducting molecular imprinted polymer for EC-SPME. Black-Right-Pointing-Pointer This first study reported on conducting molecular imprinted polymer was used to EC-SPME of salicylate. Black-Right-Pointing-Pointer Proposed method, is particularly effective in sample clean-up and selective monitoring of salicylate in physiological samples. - Abstract: Overoxidized polypyrrole (OPPy) films templated with salicylate (SA) have been utilized as conducting molecular imprinted polymers (CMIPs) for potential-induced selective solid-phase micro-extraction processes. Various important fabrication factors for controlling the performance of the OPPy films have been investigated using fluorescence spectrometry. Several key parameters such as applied potential for uptake, release, pH of uptake and release solution were varied to achieve the optimum micro-extraction procedure. The film template with SA exhibited excellent selectivity over some interference. The calibration graphs were linear in the ranges of 5 Multiplication-Sign 10{sup -8} to 5 Multiplication-Sign 10{sup -4} and 1.2 Multiplication-Sign 10{sup -6} to 5 Multiplication-Sign 10{sup -4} mol mL{sup -1} and the detection limit was 4 Multiplication-Sign 10{sup -8} mol L{sup -1}. The OPPy film as the solid-phase micro-extraction absorbent has been applied for the selective clean-up and quantification of trace amounts of SA from physiological samples. The results of scanning electron microscopy (SEM) have confirmed the nano-structure morphologies of the films.

Nanostructured conducting molecularly imprinted polymer for selective extraction of salicylate from urine and serum samples by electrochemically controlled solid-phase micro-extraction

International Nuclear Information System (INIS)

Ameli, Akram; Alizadeh, Naader

2011-01-01

Highlights: ► Overoxidized polypyrrole templated with salicylate has been utilized as conducting molecular imprinted polymer for EC-SPME. ► This first study reported on conducting molecular imprinted polymer was used to EC-SPME of salicylate. ► Proposed method, is particularly effective in sample clean-up and selective monitoring of salicylate in physiological samples. - Abstract: Overoxidized polypyrrole (OPPy) films templated with salicylate (SA) have been utilized as conducting molecular imprinted polymers (CMIPs) for potential-induced selective solid-phase micro-extraction processes. Various important fabrication factors for controlling the performance of the OPPy films have been investigated using fluorescence spectrometry. Several key parameters such as applied potential for uptake, release, pH of uptake and release solution were varied to achieve the optimum micro-extraction procedure. The film template with SA exhibited excellent selectivity over some interference. The calibration graphs were linear in the ranges of 5 × 10 −8 to 5 × 10 −4 and 1.2 × 10 −6 to 5 × 10 −4 mol mL −1 and the detection limit was 4 × 10 −8 mol L −1 . The OPPy film as the solid-phase micro-extraction absorbent has been applied for the selective clean-up and quantification of trace amounts of SA from physiological samples. The results of scanning electron microscopy (SEM) have confirmed the nano-structure morphologies of the films.

solid phase extraction method for selective determination

African Journals Online (AJOL)

FATOKI

determination of phthalate ester plasticizers in rivers and marine water samples. Of the ... samples that receive effluent from industries that use phthalate esters. ... Keywords Phthalates, Plasticizers, Solid Phase Gas Chromatography.

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.

Solid-phase extraction of iridium from soil and water samples by using activated carbon cloth prior to its spectrophotometric determination.

Science.gov (United States)

Ozkantar, Nebiye; Yilmaz, Erkan; Soylak, Mustafa; Tuzen, Mustafa

2015-08-01

A solid-phase extraction method for separation and preconcentration of Ir(IV) ion by using activated carbon cloth (ACC) has been presented. Ir(IV) as their 1-(2-pyridylazo) 2-naphtol (PAN) chelate was adsorbed on ACC at pH 2.0 and was eluted from ACC with acidic dimethylformamide (DMF). The Ir(IV) concentration was determined at 536 nm as Ir(IV)-PAN complex by using UV-vis spectrophotometer. The analytical parameters including pH, sample and eluent flow rates, amount of PAN, eluent type, concentration, and sample volume were optimized. The effects of foreign ions on the recoveries of iridium were also investigated. The preconcentration factor was calculated as 60. The limit of detection (LOD) and the limit of quantification (LOQ) of the method were found as 0.039 and 0.129 μg L(-1), respectively. The method was applied to soil and water samples for iridium determination.

Ion sources for solids isotopic analysis

Energy Technology Data Exchange (ETDEWEB)

Tyrrell, A. C. [Ministry of Defence, Foulness (UK). Atomic Weapons Research Establishment

1978-12-15

Of the dozen or so methods of producing ions from solid samples only the surface or thermal ionisation method has found general application for precise measurement of isotopic ratios. The author discusses the principal variables affecting the performance of the thermal source; sample preparation, loading onto the filament, sample pre-treatment, filament material.

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).

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

International Nuclear Information System (INIS)

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

2005-01-01

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) (R a = 98.3). An implemented RAGB source (lamp) contained commercially available red, amber, green and blue LEDs (R a 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

Cadmium complexation by solid waste leachates

DEFF Research Database (Denmark)

Xu Ze Lun; Christensen, Thomas H.

1989-01-01

A previously reported method for determination of Cd species in solid waste leachates has been applied to ten leachate samples representing five different types of solid waste: refuse compost, flyash from coal combustion, sewage sludge, refuse incineration residues and landfilled municipal waste......, slowly labile complexes and stable complexes. Leachates originating from the same type of solid waste showed different fractions of Cd, in particular with respect to free divalent Cd and stable Cd complexes. Only coal flyash showed almost identical fractions of Cd in the two leachates. The latter is due...

Ion sources for solids isotopic analysis

International Nuclear Information System (INIS)

Tyrrell, A.C.

Of the dozen or so methods of producing ions from solid samples only the surface or thermal ionisation method has found general application for precise measurement of isotopic ratios. The author discusses the principal variables affecting the performance of the thermal source; sample preparation, loading onto the filament, sample pre-treatment, filament material. (Auth.)

Iron oxide functionalized graphene nano-composite for dispersive solid phase extraction of chemical warfare agents from aqueous samples.

Science.gov (United States)

Chinthakindi, Sridhar; Purohit, Ajay; Singh, Varoon; Tak, Vijay; Goud, D Raghavender; Dubey, D K; Pardasani, Deepak

2015-05-15

Present study deals with the preparation and evaluation of graphene based magnetic nano-composite for dispersive solid phase extraction of Chemical Weapons Convention (CWC) relevant chemicals from aqueous samples. Nano-composite, Fe3O4@SiO2-G was synthesized by covalently bonding silica coated Fe3O4 onto the graphene sheets. Nerve agents (NA), Sulfur mustard (SM) and their non-toxic environmental markers were the target analytes. Extraction parameters like amount of sorbent, extraction time and desorption conditions were optimized. Dispersion of 20 milligram of sorbent in 200mL of water sample for 20min. followed by methanol/chloroform extraction produced average to good recoveries (27-94%) of targeted analytes. Recoveries of real agents exhibited great dependency upon sample pH and ionic strength. Sarin produced maximum recovery under mild acidic conditions (56% at pH 5) while VX demanded alkaline media (83% at pH 9). Salts presence in the aqueous samples was found to be advantageous, raising the recoveries to as high as 94% for SM. Excellent limits of detection (LOD) for sulphur mustard and VX (0.11ngmL(-1) and 0.19ngmL(-1) respectively) proved the utility of the developed method for the off-site analysis of CWC relevant chemicals. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of mineral, trace element, and pesticide levels in honey samples originating from different regions of Malaysia compared to manuka honey.

Science.gov (United States)

Moniruzzaman, Mohammed; Chowdhury, Muhammed Alamgir Zaman; Rahman, Mohammad Abdur; Sulaiman, Siti Amrah; Gan, Siew Hua

2014-01-01

The present study was undertaken to determine the content of six minerals, five trace elements, and ten pesticide residues in honeys originating from different regions of Malaysia. Calcium (Ca), magnesium (Mg), iron (Fe), and zinc (Zn) were analyzed by flame atomic absorption spectrometry (FAAS), while sodium (Na) and potassium (K) were analyzed by flame emission spectrometry (FAES). Trace elements such as arsenic (As), lead (Pb), cadmium (Cd), copper (Cu), and cobalt (Co) were analyzed by graphite furnace atomic absorption spectrometry (GFAAS) following the microwave digestion of honey. High mineral contents were observed in the investigated honeys with K, Na, Ca, and Fe being the most abundant elements (mean concentrations of 1349.34, 236.80, 183.67, and 162.31 mg/kg, resp.). The concentrations of the trace elements were within the recommended limits, indicating that the honeys were of good quality. Principal component analysis reveals good discrimination between the different honey samples. The pesticide analysis for the presence of organophosphorus and carbamates was performed by high performance liquid chromatography (HPLC). No pesticide residues were detected in any of the investigated honey samples, indicating that the honeys were pure. Our study reveals that Malaysian honeys are rich sources of minerals with trace elements present within permissible limits and that they are free from pesticide contamination.

Penicillium digitatum immobilized on pumice stone as a new solid phase extractor for preconcentration and/or separation of trace metals in environmental samples

Energy Technology Data Exchange (ETDEWEB)

Baytak, Sitki [Department of Chemistry, Faculty of Science and Arts, Harran University, 63100 Sanliurfa (Turkey); Kenduezler, Erdal [Department of Primary Education, Faculty of Education, Ahi Evran University, 40100 Kirsehir (Turkey); Tuerker, Ali Rehber [Department of Chemistry, Faculty of Science and Arts, Gazi University, 06500 Ankara (Turkey)], E-mail: aturker@gazi.edu.tr; Goek, Nuray [Department of Environmental Engineering, Faculty of Engineering, Harran University, 63000 Sanliurfa (Turkey)

2008-05-30

This study presents a column solid phase extraction procedure based on column biosorption of Cu(II), Zn(II) and Pb(II) ions on Penicillium digitatum immobilized on pumice stone. The analytes were determined by flame atomic absorption spectrometry (FAAS). The optimum conditions such as: pH values, amount of solid phase, elution solution and flow rate of sample solution were evaluated for the quantitative recovery of the analytes. The effect of interfering ions on the recovery of the analytes has also been investigated. The recoveries of copper, zinc and lead under the optimum conditions were found to be 97 {+-} 2, 98 {+-} 2 and 98 {+-} 2%, respectively, at 95% confidence level. For the analytes, 50-fold preconcentration was obtained. The analytical detection limits for Cu(II), Zn(II) and Pb(II) were 1.8, 1.3 and 5.8 ng mL{sup -1}, respectively. The proposed procedure was applied for the determination of copper, zinc and lead in dam water, waste water, spring water, parsley and carrot. The accuracy of the procedure was checked by determining copper, zinc and lead in standard reference tea samples (GBW-07605)

Penicillium digitatum immobilized on pumice stone as a new solid phase extractor for preconcentration and/or separation of trace metals in environmental samples

International Nuclear Information System (INIS)

Baytak, Sitki; Kenduezler, Erdal; Tuerker, Ali Rehber; Goek, Nuray

2008-01-01

This study presents a column solid phase extraction procedure based on column biosorption of Cu(II), Zn(II) and Pb(II) ions on Penicillium digitatum immobilized on pumice stone. The analytes were determined by flame atomic absorption spectrometry (FAAS). The optimum conditions such as: pH values, amount of solid phase, elution solution and flow rate of sample solution were evaluated for the quantitative recovery of the analytes. The effect of interfering ions on the recovery of the analytes has also been investigated. The recoveries of copper, zinc and lead under the optimum conditions were found to be 97 ± 2, 98 ± 2 and 98 ± 2%, respectively, at 95% confidence level. For the analytes, 50-fold preconcentration was obtained. The analytical detection limits for Cu(II), Zn(II) and Pb(II) were 1.8, 1.3 and 5.8 ng mL -1 , respectively. The proposed procedure was applied for the determination of copper, zinc and lead in dam water, waste water, spring water, parsley and carrot. The accuracy of the procedure was checked by determining copper, zinc and lead in standard reference tea samples (GBW-07605)

Solid-solid and gas-solid interactions induced during high-energy milling to produce PbTe nanopowders

Energy Technology Data Exchange (ETDEWEB)

Rojas-Chavez, H., E-mail: rojas_hugo@ittlahuac2.edu.mx [Instituto Tecnologico de Tlahuac - II (Mexico); Reyes-Carmona, F. [Facultad de Quimica - UNAM (Mexico); Garibay-Febles, V. [Instituto Mexicano del Petroleo, Laboratorio de Microscopia Electronica de Ultra Alta Resolucion (Mexico); Jaramillo-Vigueras, D. [Centro de Investigacion e Innovacion Tecnologica - IPN (Mexico)

2013-05-15

Transformations from precursors to nanoparticles by high-energy milling are promoted by two major driving forces, namely physical and/or chemical. While the former has been difficult to trace since stress, strain and recovery may occur almost simultaneously during milling, the latter has been sequentially followed as an evolution from precursors to intermediate phases and thereof to high purity nanocrystals. The specific objective of this work is to discern how solid-solid and partially solid-gas reactions manifest themselves correspondingly as a short-range diffusion through an interface or how vapor species, as a subliming phenomenon, grows as a different phase on an active local surface. These series of changes were traced by sub-cooling the as-milled powders extracted during a milling cycle. Through this experimental technique, samples were electron microscopically analyzed and where it was required, selected area electron diffraction images were obtained. High-resolution transmission electron microscopy results, unambiguously, confirm that nanocrystals in the last stage show a cubic morphology which average size distributions are around 17 nm.

Determination of neonicotinoid pesticides residues in agricultural samples by solid-phase extraction combined with liquid chromatography-tandem mass spectrometry.

Science.gov (United States)

Xie, Wen; Han, Chao; Qian, Yan; Ding, Huiying; Chen, Xiaomei; Xi, Junyang

2011-07-15

This work reports a new sensitive multi-residue liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for detection, confirmation and quantification of six neonicotinoid pesticides (dinotefuran, thiamethoxam, clothiandin, imidacloprid, acetamiprid and thiacloprid) in agricultural samples (chestnut, shallot, ginger and tea). Activated carbon and HLB solid-phase extraction cartridges were used for cleaning up the extracts. Analysis is performed by LC-MS/MS operated in the multiple reaction monitoring (MRM) mode, acquiring two specific precursor-product ion transitions per target compound. Quantification was carried by the internal standard method with D(4)-labeled imidacloprid. The method showed excellent linearity (R(2)≥0.9991) and precision (relative standard deviation, RSD≤8.6%) for all compounds. Limits of quantification (LOQs) were 0.01 mg kg(-1) for chestnut, shallot, ginger sample and 0.02 mg kg(-1) for tea sample. The average recoveries, measured at three concentrations levels (0.01 mg kg(-1), 0.02 mg kg(-1) and 0.1 mg kg(-1) for chestnut, shallot, ginger sample, 0.02 mg kg(-1), 0.04 mg kg(-1) and 0.2 mg kg(-1) for tea sample), were in the range 82.1-108.5%. The method was satisfactorily validated for the analysis of 150 agricultural samples (chestnut, shallot, ginger and tea). Imidacloprid and acetamiprid were detected at concentration levels ranging from 0.05 to 3.6 mg kg(-1). Copyright © 2011 Elsevier B.V. All rights reserved.

Using reweighting and free energy surface interpolation to predict solid-solid phase diagrams

Science.gov (United States)

Schieber, Natalie P.; Dybeck, Eric C.; Shirts, Michael R.

2018-04-01

Many physical properties of small organic molecules are dependent on the current crystal packing, or polymorph, of the material, including bioavailability of pharmaceuticals, optical properties of dyes, and charge transport properties of semiconductors. Predicting the most stable crystalline form at a given temperature and pressure requires determining the crystalline form with the lowest relative Gibbs free energy. Effective computational prediction of the most stable polymorph could save significant time and effort in the design of novel molecular crystalline solids or predict their behavior under new conditions. In this study, we introduce a new approach using multistate reweighting to address the problem of determining solid-solid phase diagrams and apply this approach to the phase diagram of solid benzene. For this approach, we perform sampling at a selection of temperature and pressure states in the region of interest. We use multistate reweighting methods to determine the reduced free energy differences between T and P states within a given polymorph and validate this phase diagram using several measures. The relative stability of the polymorphs at the sampled states can be successively interpolated from these points to create the phase diagram by combining these reduced free energy differences with a reference Gibbs free energy difference between polymorphs. The method also allows for straightforward estimation of uncertainties in the phase boundary. We also find that when properly implemented, multistate reweighting for phase diagram determination scales better with the size of the system than previously estimated.

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

Determination of copper and mercury in phosphate fertilizers employing direct solid sampling analysis and high resolution continuum source graphite furnace atomic absorption spectrometry

Science.gov (United States)

de Oliveira Souza, Sidnei; François, Luciane Luiza; Borges, Aline Rocha; Vale, Maria Goreti Rodrigues; Araujo, Rennan Geovanny Oliveira

2015-12-01

The present study proposes the determination of copper and mercury in phosphate fertilizers by direct solid sampling analysis (SS) employing high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). For Cu determination, two analytical lines were used: 327.3960 nm and 249.2146 nm. Hg determination was carried out on the line 253.6521 nm and 100 μg KMnO4 was used as chemical modifier. The optimal pyrolysis temperature for Cu determination was 1300 °C. Atomization temperatures for Cu and Hg were 2400 and 1100 °C, respectively. External calibration with aqueous standard solutions was adopted for both elements. The limits of quantification (LoQs) and characteristic mass (m0) obtained for Cu determination were 0.4 μg g- 1 and 1.12 ng, respectively, on line 249.2146 nm, and 64 μg g- 1 and 25 pg on 327.3960 nm. For mercury, LoQ and m0 were 4.8 ng g- 1 and 39 pg, respectively. The accuracy of the proposed methods was confirmed by the analysis of standard reference material (SRM) of Trace Elements in Multi-Nutrient Fertilizer (SRM NIST 695). The precision expressed as relative standard deviation (RSD), was better than 8.2% for Hg and 7.7% for the Cu (n = 5), considered satisfactory for microanalysis in solid sample. Four fertilizer samples acquired in commercial establishments in the city of Salvador, Bahia, Brazil, were analyzed. The optimized analytical methods were simple, fast, accurate, precise and free of spectral interferences for the determination of Cu and Hg in phosphate fertilizer samples by SS-HR-CS GF AAS, avoiding the dissolution of the sample, the use of harmful reagents and the generation of residues.

Solid-phase micro-extraction in bioanalysis, exemplified by lidocaine determination

NARCIS (Netherlands)

de Jong, GJ; Koster, EHM

2000-01-01

Solid-phase micro-extraction (SPME) is a never sample preparation technique that can be used for gaseous, liquid or solid samples in conjunction with GC, HPLC or CE (e.g. [1]). The use of SPME for the analysis of drugs in biofluids is also becoming popular (e.g. [2]). The principle is that a fused

Measurement of solid flow rates and sampling

International Nuclear Information System (INIS)

Caillot, A.

1984-01-01

Given the fact that very fine sediments are carriers of numerous pollutant products, in order to be able to ensure realistic and vigilant control of the aquatic environment we have to take into account sedimentary transport. The movement of sediments may be due to natural events (currents, swell, winds), or to human intervention (dredging, emptying of dam reservoirs, release of wastes and so forth). Their circulation, at times highly complex, especially in estuaries, may alternate with periods of rest - and therefore periods of accumulation of pollutants - which may be fairly long. Despite the plethora of available methods and techniques, the amounts of sediment transported by drift or in suspension are very difficult to assess. The physico-chemical nature and the behaviour of these substances in water makes it awkward to select samples, in space and time, for the purpose of analysis. The sampling should be carried out with the mechanical means suited to the circumstances and to the aim in mind. However, by taking into consideration the hydrosedimentary mechanisms known by the hydrologists and sedimentologists it is possible to improve the selection of the sites to be monitored as well as to choose more carefully (and therefore to limit) the samples to be analysed. Environmental monitoring may thus be performed more efficiently and at lower cost. (author)

Análise direta de sólidos por espectrometria de absorção atômica com atomização em forno de grafite: uma revisão Solid sampling graphite furnace atomic absorption spectrometry: a review

Directory of Open Access Journals (Sweden)

Cassiana Seimi Nomura

2008-01-01

Full Text Available This is a review of direct analysis using solid sampling graphite furnace atomic absorption spectrometry. Greater emphasis is dedicated to sample preparation, sample homogeneity, calibration and its application to microanalysis and micro-homogeneity studies. The main advantages and some difficulties related to the applicability of this technique are discussed. A literature search on the application of solid sampling graphite furnace atomic absorption spectrometry in trace element determination in many kinds of samples, including biological, clinical, technological and environmental ones, is also presented.

Standard test method for graphite furnace atomic absorption spectrometric determination of lead and cadmium extracted from ceramic foodware

CERN Document Server

American Society for Testing and Materials. Philadelphia

2000-01-01

1.1 This test method covers procedures for using graphite furnace atomic absorption spectroscopy (GFAAS) to quantitatively determine lead and cadmium extracted by acetic acid at room temperature from the food-contact surface of foodware. The method is applicable to food-contact surfaces composed of silicate-based materials (earthenware, glazed ceramicware, decorated ceramicware, decorated glass, and lead crystal glass) and is capable of determining lead concentrations greater than 0.005 to 0.020 g/mL and cadmium concentrations greater than 0.0005 to 0.002 g/mL, depending on instrument design. 1.2 This test method also describes quality control procedures to check for contamination and matrix interference during GFAAS analyses and a specific sequence of analytical measurements that demonstrates proper instrument operation during the time period in which sample solutions are analyzed. 1.3 Cleaning and other contamination control procedures are described in this test method. Users may modify contamination cont...

Biocompatible in-tube solid phase microextraction coupled with liquid chromatography-fluorescence detection for determination of interferon α in plasma samples.

Science.gov (United States)

Chaves, Andréa R; Silva, Bruno J G; Lanças, Fernando M; Queiroz, Maria Eugênia C

2011-05-27

The present work demonstrates the successful application of automated biocompatible in-tube solid-phase microextraction coupled with liquid chromatography (in-tube SPME/LC) for determination of interferon alpha(2a) (IFN α(2a)) in plasma samples for therapeutic drug monitoring. A restricted access material (RAM, protein-coated silica) was employed for preparation of a lab-made biocompatible in-tube SPME capillary that enables the direct injection of biological fluids as well as the simultaneous exclusion of macromolecules by chemical diffusion barrier and drug pre-concentration. The in-tube SPME variables, such as sample volume, draw/eject volume, number of draw-eject cycles, and desorption mode were optimized, to improve the sensitivity of the proposed method. The IFN α(2a) analyses in plasma sample were carried out within 25min (sample preparation and LC analyses). The response of the proposed method was linear over a dynamic range, from 0.06 to 3.0MIUmL(-1), with correlation coefficient equal to 0.998. The interday precision of the method presented coefficient of variation lower than 8%. The proposed automated method has adequate analytical sensitivity and selectivity for determination of IFN α(2a) in plasma samples for therapeutic drug monitoring. Copyright © 2010 Elsevier B.V. All rights reserved.

Mechanism to synthesize a ‘moving optical mark’ at solid-ambient interface for the estimation of thermal diffusivity of solid

Directory of Open Access Journals (Sweden)

Settu Balachandar

2016-01-01

Full Text Available A novel mechanism is proposed, involving a novel interaction between solid-sample supporting unsteady heat flow with its ambient-humidity; invokes phase transformation of water-vapour molecule and synthesize a ‘moving optical-mark’ at sample-ambient-interface. Under tailored condition, optical-mark exhibits a characteristic macro-scale translatory motion governed by thermal diffusivity of solid. For various step-temperature inputs via cooling, position-dependent velocities of moving optical-mark are measured at a fixed distance. A new approach is proposed. ‘Product of velocity of optical-mark and distance’ versus ‘non-dimensional velocity’ is plotted. The slope reveals thermal diffusivity of solid at ambient-temperature; preliminary results obtained for Quartz-glass is closely matching with literature.

Natural Arsenic Pollution and Hydrochemistry of Drinking Water of an Urban Part of Iran

Directory of Open Access Journals (Sweden)

Mohammad Mosaferi

2014-12-01

Full Text Available Natural contamination of surface and groundwater resources with arsenic is a worldwide problem. The present study aimed to investigate and report on the quality of drinking water resources with special focus on arsenic presence in an urban part of Iran. Arsenic concentrations were measured by graphite furnace atomic absorption spectroscopy (GFAAS. In both surface and groundwater samples, arsenic concentrations ranged from 6 - 61 µg/L with an average value of 39 ± 20 µg/L. Concentration of arsenic, which was up to six times greater than guideline values (10 µg/L indicates the presence of arsenic bearing materials in the geological structure of the region. It was found that the quality of treated surface water produced by the water treatment facility was good in respect to arsenic (9 µg/L and solid content (EC = µs/cm. However, in drinking water samples of wells, total solids (mean EC = 1580 ± 150 µs/cm, total hardness (mean = 479 + 94 mg/L as CaCO3 and arsenic (mean = 42 + 16 µg/L were significantly higher. Correspondingly, there was a significant correlation between arsenic concentration and EC, Na+, K+ and Cl- values. The type of water in most of groundwater samples (70% was determined as HCO3-Na+. Considering the population of the city and probable health effects due to exposure to arsenic through drinking water, comprehensive measures as well as application of arsenic removal processes in water treatment facilities and replacement of contaminated wells with safe wells are required.

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.

Analysis of environmental samples by roentgen fluorescence spectroscopy

International Nuclear Information System (INIS)

Hroncova, E.; Ladomersky, J.

2004-01-01

We can use it to analyse nearly all elements of solid and liquid samples. The possibility of analysing solid samples in compact shape, in powder or either under shape of fine layers shortens appreciably the total time of analysis, that is in addition to its no destructiveness, the main reason of as a XRF favourite method. (authors)

A visual LISP program for voxelizing AutoCAD solid models

Science.gov (United States)

Marschallinger, Robert; Jandrisevits, Carmen; Zobl, Fritz

2015-01-01

AutoCAD solid models are increasingly recognized in geological and geotechnical 3D modeling. In order to bridge the currently existing gap between AutoCAD solid models and the grid modeling realm, a Visual LISP program is presented that converts AutoCAD solid models into voxel arrays. Acad2Vox voxelizer works on a 3D-model that is made up of arbitrary non-overlapping 3D-solids. After definition of the target voxel array geometry, 3D-solids are scanned at grid positions and properties are streamed to an ASCII output file. Acad2Vox has a novel voxelization strategy that combines a hierarchical reduction of sampling dimensionality with an innovative use of AutoCAD-specific methods for a fast and memory-saving operation. Acad2Vox provides georeferenced, voxelized analogs of 3D design data that can act as regions-of-interest in later geostatistical modeling and simulation. The Supplement includes sample geological solid models with instructions for practical work with Acad2Vox.

DECREASE OF SOLIDS IN GRAY WATER BY AERATION PROCESS

Directory of Open Access Journals (Sweden)

Gerardo Alonso Torres-Avalos

2017-07-01

Full Text Available The activated sludge process is a biological treatment consisting basically of agitation and aeration of a waste water mixture and a selected microorganisms sludge. The oxidation of organic matter was determined with several tests such as BOD5 (Biochemical Oxygen Demand, TSS (Total Sedimented Solids, SS (Sediment Solids, TDS (Total Dissolved Solids, FVS (fixed and volatile solids and finally a measurement of treated water turbidity. The results obtained for the reduction of the organic load during the first two days of treatment (samples 1, 2 and 3 are visible in each of the organic loading tests; during the last two days according to the samples 4 and 5 the solids showed an increase in organic load. The related organoleptic properties such as color showed a notable decrease. As for the tests performed at pH show a change, samples 1, 2 and 3 approaching a range where they are neutral and the last two samples (4 and 5 the pH has an elevation until it becomes alkaline. The efficiency of the method used for the treatment of residual water during the first days reduced the organic load with a variation of TS and TSS of 760, 569 ppm respectively. This is a viable alternative since this is a low cost method with short term results because organoleptic properties such as odor and color were lost during the first day of treatment.

Determination of soy proteins in food samples by dispersive solid-phase immunoextraction and dynamic long-wavelength fluorometry

International Nuclear Information System (INIS)

Molina-Delgado, María Ángeles; Aguilar-Caballos, María Paz; Gomez-Hens, Agustina

2013-01-01

We report on a method for the determination of soy proteins in food samples via dispersive solid-phase immunoextraction using gold-coated magnetic nanoparticles (NPs) as a support. Soy proteins were first extracted using anti-soy protein antibodies immobilized on the NPs, and then quantified by measuring the increase in fluorescence of the long-wavelength fluorophore cresyl violet in the presence of the anionic surfactant sodium dodecyl sulfate at neutral pH in a flow system. The method involves the use of two standard or sample aliquots. The fluorescence intensity of one aliquot is directly measured whereas that of the other aliquot is measured after immunoextraction. The difference between the peak heights of both aliquots serves as the analytical information that is directly proportional to the protein concentration. The limit of detection is 0.35 mg L −1 , the linear range is from 1 to 15 mg L −1 , and the relative standard deviation is < 5 %. Proteins such as bovine serum albumin and globulins do not interfere at the same concentration level. The method was applied to the analysis of soy-based beverages and gave recoveries in the range between 80.0 and 107.3 %. (author)

Results of Characterization and Retrieval Testing on Tank 241-C-109 Heel Solids

Energy Technology Data Exchange (ETDEWEB)

Callaway, William S.

2013-09-26

Eight samples of heel solids from tank 241-C-109 were delivered to the 222-S Laboratory for characterization and dissolution testing. After being drained thoroughly, one-half to two-thirds of the solids were off-white to tan solids that, visually, were fairly evenly graded in size from coarse silt (30-60 μm) to medium pebbles (8-16 mm). The remaining solids were mostly strongly cemented aggregates ranging from coarse pebbles (16-32 mm) to fine cobbles (6-15 cm) in size. Solid phase characterization and chemical analysis indicated that the air-dry heel solids contained ≈58 wt% gibbsite [Al(OH){sub 3}] and ≈37 wt% natrophosphate [Na{sub 7}F(PO{sub 4}){sub 2}·19H{sub 2}O]. The strongly cemented aggregates were mostly fine-grained gibbsite cemented with additional gibbsite. Dissolution testing was performed on two test samples. One set of tests was performed on large pieces of aggregate solids removed from the heel solids samples. The other set of dissolution tests was performed on a composite sample prepared from well-drained, air-dry heel solids that were crushed to pass a 1/4-in. sieve. The bulk density of the composite sample was 2.04 g/mL. The dissolution tests included water dissolution followed by caustic dissolution testing. In each step of the three-step water dissolution tests, a volume of water approximately equal to 3 times the initial volume of the test solids was added. In each step, the test samples were gently but thoroughly mixed for approximately 2 days at an average ambient temperature of 25 °C. The caustic dissolution tests began with the addition of sufficient 49.6 wt% NaOH to the water dissolution residues to provide ≈3.1 moles of OH for each mole of Al estimated to have been present in the starting composite sample and ≈2.6 moles of OH for each mole of Al potentially present in the starting aggregate sample. Metathesis of gibbsite to sodium aluminate was then allowed to proceed over 10 days of gentle mixing of the

Solid-phase extraction followed by dispersive liquid-liquid microextraction for the sensitive determination of ecstasy compounds and amphetamines in biological samples

Directory of Open Access Journals (Sweden)

H. A. Mashayekhi

2014-09-01

Full Text Available A novel approach for the determination of ecstasy and amphetamines (3,4-methylenedioxymethylamphetamine (MDMA, Ecstasy, 3,4-methylenedioxyamphetamine (MDA, 3,4-methylenedioxyethylamphetamine (MDEA and 3,4-methylenedioxypropylamphetamine (MDPA in biological samples is presented. The analytes were extracted from the matrix and transferred to a small volume of a high density, water insoluble solvent using solid-phase extraction (SPE followed by dispersive liquid-liquid microextraction (DLLME. This combination not only resulted in a high enrichment factor, but also it could be used in complex matrices (biological samples. Some important extraction parameters, such as sample solution flow rate, sample pH, type and volume of extraction and disperser solvents as well as the salt addition, were studied and optimized. Under the optimized conditions, the calibration graphs were linear in the range of 0.5-500 µg L-1 and 1.0-500 µg L-1 with detection limits in the range of 0.1-0.3 µg L-1 and 0.2-0.7 µg L-1 in urine and plasma samples, respectively. The results showed that SPE-DLLME is a suitable method for the determination of ecstasy components and amphetamines in biological and water samples. DOI: http://dx.doi.org/10.4314/bcse.v28i3.3

Sample container for neutron activation analysis

International Nuclear Information System (INIS)

Lersmacher, B.; Verheijke, M.L.; Jaspers, H.J.

1983-01-01

The sample container avoids contaminating the sample substance by diffusion of foreign matter from the wall of the sample container into the sample. It cannot be activated, so that the results of measurements are not falsified by a radioactive container wall. It consists of solid carbon. (orig./HP) [de

Clinical evaluation of high-risk HPV detection on self-samples using the indicating FTA-elute solid-carrier cartridge.

Science.gov (United States)

Geraets, D T; van Baars, R; Alonso, I; Ordi, J; Torné, A; Melchers, W J G; Meijer, C J L M; Quint, W G V

2013-06-01

High-risk human papillomavirus (hrHPV) testing in cervical screening is usually performed on physician-taken cervical smears in liquid-based medium. However, solid-state specimen carriers allow easy, non-hazardous storage and transportation and might be suitable for self-collection by non-responders in screening and in low-resource settings. We evaluated the adequacy of self-collected cervicovaginal (c/v) samples using a Viba-brush stored on an Indicating FTA-elute cartridge (FTA-based self-sampling) for hrHPV testing in women referred to a gynecology clinic due to an abnormal smear. 182 women accepted to self-collect a c/v sample. After self-sampling, a physician obtained a conventional liquid-based cervical smear. Finally, women were examined by colposcopy and a biopsy was taken when clinically indicated. Self-samples required only simple DNA elution, and DNA was extracted from physician-obtained samples. Both samples were tested for 14 hrHPVs by GP5+/6+-EIA-LQ Test and SPF(10)-DEIA-LiPA(25). Both assays detected significantly more hrHPV in physician-collected specimens than in self-collected samples (75.3% and 67.6% by SPF(10); 63.3% and 53.3% by GP5+/6+, respectively). The combination of physician-collected specimen and GP5+/6+ testing demonstrated the optimal balance in sensitivity (98.0%) and specificity (48.1%) for CIN2+ detection in this referral population. A test system of FTA-based self-collection and SPF(10) hrHPV detection approached this sensitivity (95.9%) and specificity (42.9%). These results show that the clinical performance of hrHPV detection is determined by both the sample collection system and the test method. FTA-based self-collection with SPF(10) testing might be valuable when a liquid-based medium cannot be used, but requires further investigation in screening populations. Copyright © 2013 Elsevier B.V. All rights reserved.

Determination of trace elements and screening of metalloproteins in human blood and tissues

International Nuclear Information System (INIS)

Prohaska, K.

2003-02-01

Sequential and simultaneous atomic spectrometric detection was applied for the determination of metals in human whole blood, blood fractions and joint tissues. For this purpose ICP-OES (inductively coupled plasma - optical emission spectrometry) and GFAAS (graphite furnace - atomic absorption spectrometry) were optimized. The nebulizing technique of the ICP-OES causes a high consumption of the sample (2.4 mL /min uptake rate). Using the simultaneous modus of measurement it is possible to determine up to 20 elements in the samples of interest. Using GFAAS the elements can be detected sequentially only, the method is more time consuming in comparison. For the direct sample injection into the graphite tube only 20 aeL are needed. Since 1 mL sample has to be filled in the sample vessel of the autosampler, up to six elements can be determined in this volume. The most important advantage of the simultaneous multi-element detection is the low sample consumption, which is essential for analysis of biological samples. Normally only small amounts of human blood or tissues can be collected, and the concentrations of analytes are usually very low. Therefore in many cases a sample preparation is of advantage, which enables a pre-concentration of the analyte. The sample digestion was optimized with respect to the possible pre-concentration of the analytes. Ashing of the freeze-dried blood enabled a six fold higher concentration in the measuring solution compared with wet digestion of blood. For the ICP-OES sample introduction system two different nebulizers were tested in the complex matrix of the digested blood samples. A Meinhard and the microconcentric nebulizer were compared according to their analytical performance. The matrix of the samples caused LODs three to five times higher than in the aqueous standards. The application of the Meinhard nebulizer enabled sufficiently low LODs in the matrix for some elements of interest (Ca, Cu, Fe, Mg, P, S, Zn in freeze-dried blood

Amoco-US Environmental Protection Agency, pollution prevention project, Yorktown, Virginia: Solid waste data

International Nuclear Information System (INIS)

Kizior, G.J.

1991-01-01

In late 1989 Amoco and the US Environmental Protection Agency initiated a joint project to review pollution prevention alternatives at Amoco Oil Company's Yorktown, Virginia, Refinery as a case study site. The report summarizes the solid waste emissions inventory, solids source identification, and the solid waste sampling program that was conducted at the Amoco Yorktown Refinery on September 25-27, 1990, in support of the Pollution Prevention Project. Major findings showed that the majority of solid waste generation occurs as end-of-pipe solids resulting from the treatment of wastewaters from the refinery sewer. Based on a regression analysis of the composition data for samples collected during this project, major upstream contributors to these solids appear to be soils. Solids from process units are also significant contributors

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.)

Thermally stimulated exoelectron emission from solid Xe

International Nuclear Information System (INIS)

Khyzhniy, I.V.; Grigorashchenko, O.N.; Savchenko, E.V.; Ponomarev, A.N.; Bondybey, V.E.

2007-01-01

Thermally-stimulated emission of exoelectrons and photons from solid Xe pre-irradiated by low-energy electrons were studied. A high sensitivity of thermally-stimulated luminescence (TSL) and thermally-stimulated exoelectron emission (TSEE) to sample prehistory was demonstrated. It was shown that electron traps in unannealed samples are characterized by much broader distribution of trap levels in comparison with annealed samples and their concentration exceeds in number that in annealed samples. Both phenomena, TSL and TSEE, were found to be triggered by release of electrons from the same kind of traps. The data obtained suggest a competition between two relaxation channels: charge recombination and electron transport terminated by TSL and TSEE. It was found that TSEE predominates at low temperatures while at higher temperatures TSL prevails. An additional relaxation channel, a photon-stimulated exoelectron emission pre-irradiated solid Xe, was revealed

Plasma dynamics from laser ablated solid lithium

Indian Academy of Sciences (India)

b; 52.25.-b; 52.70.-m. 1. Introduction. Pulsed laser ablation of a solid sample generates a dense plasma emission in the shape of ... The multichannel analyser plate of the ICCD was gated for as less as 4 ns using ... to explain the atomic collision processes [4]. .... Within duration of laser pulse, there occurs laser-solid interac-.

Sampling and sample handling procedures for priority pollutants in surface coal mining wastewaters. [Detailed list to be analyzed for

Energy Technology Data Exchange (ETDEWEB)

Hayden, R. S.; Johnson, D. O.; Henricks, J. D.

1979-03-01

The report describes the procedures used by Argonne National Laboratory to sample surface coal mine effluents in order to obtain field and laboratory data on 110 organic compounds or classes of compounds and 14 metals and minerals that are known as priority pollutants, plus 5-day biochemical oxygen demand (BOD/sub 5/), total organic carbon (TOC), chemical oxygen demand (COD), total dissolved solids (TDS), and total suspended solids (TSS). Included are directions for preparation of sampling containers and equipment, methods of sampling and sample preservation, and field and laboratory protocols, including chain-of-custody procedures. Actual analytical procedures are not described, but their sources are referenced.

Core-shell Fe3O4 polydopamine nanoparticles as sorbent for magnetic dispersive solid-phase extraction of copper from food samples.

Science.gov (United States)

Yavuz, Emre; Tokalıoğlu, Şerife; Patat, Şaban

2018-10-15

In the present study, core-shell Fe 3 O 4 polydopamine nanoparticles were synthesized and used for the first time as an adsorbent for the vortex assisted magnetic dispersive solid phase extraction of copper from food samples. After elution, copper in the solutions was determined by FAAS. The adsorbent was characterized using X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller surface area, and zeta potential measurements. Various parameters affecting the magnetic dispersive solid-phase extraction were evaluated. The optimum pH and magnetic adsorbent amount were found to be 5 and 40 mg, respectively. Elution was made by 3 mL of 2 mol L -1 HNO 3 .The major advantage of the method is the fast equilibration during adsorption without the need for vortexing or shaking. The preconcentration factor and detection limit of the method were found to be 150 and 0.22 mg L -1 , respectively. The precision (as RSD%) and adsorption capacity of the method were 3.7% and 28 mg g -1 , respectively. The method was successfully verified by analyzing four certified reference materials (SPS-WW1 Batch 114 Wastewater, TMDA-53.3 Lake water, BCR-482 Lichen and 1573a Tomato Leaves) and by addition/recovery tests of copper standard solution in organic baby food, muesli, macaroni, honey, and milk samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

Trace-level mercury ion (Hg2+) analysis in aqueous sample based on solid-phase extraction followed by microfluidic immunoassay.

Science.gov (United States)

Date, Yasumoto; Aota, Arata; Terakado, Shingo; Sasaki, Kazuhiro; Matsumoto, Norio; Watanabe, Yoshitomo; Matsue, Tomokazu; Ohmura, Naoya

2013-01-02

Mercury is considered the most important heavy-metal pollutant, because of the likelihood of bioaccumulation and toxicity. Monitoring widespread ionic mercury (Hg(2+)) contamination requires high-throughput and cost-effective methods to screen large numbers of environmental samples. In this study, we developed a simple and sensitive analysis for Hg(2+) in environmental aqueous samples by combining a microfluidic immunoassay and solid-phase extraction (SPE). Using a microfluidic platform, an ultrasensitive Hg(2+) immunoassay, which yields results within only 10 min and with a lower detection limit (LOD) of 0.13 μg/L, was developed. To allow application of the developed immunoassay to actual environmental aqueous samples, we developed an ion-exchange resin (IER)-based SPE for selective Hg(2+) extraction from an ion mixture. When using optimized SPE conditions, followed by the microfluidic immunoassay, the LOD of the assay was 0.83 μg/L, which satisfied the guideline values for drinking water suggested by the United States Environmental Protection Agency (USEPA) (2 μg/L; total mercury), and the World Health Organisation (WHO) (6 μg/L; inorganic mercury). Actual water samples, including tap water, mineral water, and river water, which had been spiked with trace levels of Hg(2+), were well-analyzed by SPE, followed by microfluidic Hg(2+) immunoassay, and the results agreed with those obtained from reduction vaporizing-atomic adsorption spectroscopy.

Low-impact sampling under an active solid low-level radioactive waste disposal unit using horizontal drilling technology

International Nuclear Information System (INIS)

Puglisi, C.V.; Vold, E.L.

1995-01-01

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 ampersand 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

Preparation of milk samples for immunoassay and liquid chromatographic screening using matrix solid-phase dispersion.

Science.gov (United States)

Barker, S A; Long, A R

1994-01-01

The use of drugs to maintain the health and maximize the output of dairy cattle has made the monitoring of milk for such agents essential. Screening tests based on immunological, microbial inhibition, and bacterial receptor assays have been developed for the detection of violative levels of therapeutic substances. However, such assays are not infallible, and false positive or negative results can occur when contaminants bind receptors or compete for the binding of the target residues. Such effects may arise from dietary sources, diseases, or other variables. Thus, a violation by such a test is not definitive until further confirmation is obtained. Our laboratory has developed extraction procedures for several drugs used in dairy production. Our method uses matrix solid-phase dispersion (MSPD) to isolate drugs away from contaminants and to eliminate many possible interferences. MSPD can also be used to enhance the specificity of such assays by fractionating various classes of drugs that may cross-react. Similarly, such methods may be used for liquid chromatographic screening and confirmation of a suspect sample.

Computer aided testing of steel samples deformation at coexistence liquid and solid phase

International Nuclear Information System (INIS)

Hojny, M.; Glowacki, M.

2007-01-01

The paper reports the results of experimental and theoretical work leading to construction of a CAE system dedicated to the numerical simulation of plastic deformation of steel at coexistence liquid and solid phase. A coupled thermal-mechanical model including inverse analysis technique was adopted for the solver. The advantage of the solution was the analytical form of both incompressibility and mass conservation conditions. This can prevent usual FEM variational solution problems concerning unintentional specimen volume loss caused by the numerical errors. The only well known machine allowing tests in the discussed temperature range is the GLEEBLE thermo-mechanical simulator. Experiments of deformation of steel in semi-solid state by using this machine are very expensive. Therefore, application of dedicated computer simulation system with inverse method makes tests possible and results in lowering testing cost

Pressure effects in hollow and solid iron oxide nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Silva, N.J.O., E-mail: nunojoao@ua.pt [Departamento de Física and CICECO, Universidade de Aveiro, 3810-193 Aveiro (Portugal); Saisho, S.; Mito, M. [Faculty of Engineering, Kyushu Institute of Technology, Kitakyushu 804-8550 (Japan); Millán, A.; Palacio, F. [Instituto de Ciencia de Materiales de Aragón, CSIC - Universidad de Zaragoza. Departamento de Física de la Materia Condensada, Facultad de Ciencias, 50009 Zaragoza (Spain); Cabot, A. [Universitat de Barcelona and Catalonia Energy Research Institute, Barcelona (Spain); Iglesias, Ò.; Labarta, A. [Departament de Física Fonamental, Universitat de Barcelona and Institut de Nanociència i Nanotecnologia, Universitat de Barcelona, Martí i Franquès 1, 08028 Barcelona (Spain)

2013-06-15

We report a study on the pressure response of the anisotropy energy of hollow and solid maghemite nanoparticles. The differences between the maghemite samples are understood in terms of size, magnetic anisotropy and shape of the particles. In particular, the differences between hollow and solid samples are due to the different shape of the nanoparticles and by comparing both pressure responses it is possible to conclude that the shell has a larger pressure response when compared to the core. - Highlights: ► Study of the pressure response of core and shell magnetic anisotropy. ► Contrast between hollow and solid maghemite nanoparticles. ► Disentanglement of nanoparticles core and shell magnetic properties.

High resolution spectroscopy in solids by nuclear magnetic resonance

International Nuclear Information System (INIS)

Bonagamba, T.J.

1991-07-01

The nuclear magnetic resonance (NMR) techniques for High Resolution Spectroscopy in Solids are described. Also the construction project of a partially home made spectrometer and its applications in the characterization of solid samples are shown in detail. The high resolution spectrometer used is implemented with the double resonance multiple pulses sequences and magic angle spinning (MAS) and can be used with solid and liquid samples. The maximum spinning frequency for the MAS experiment is in excess of 5 Khz, the double resonance sequences can be performed with any type of nucleus, in the variable temperature operating range with nitrogen gas: -120 0 C to +160 0 C, and is fully controlled by a Macintosh IIci microcomputer. (author)

A comparison study on a sulfonated graphene-polyaniline nanocomposite coated fiber for analysis of nicotine in solid samples through the traditional and vacuum-assisted HS-SPME.

Science.gov (United States)

Ghiasvand, Alireza; Koonani, Samira; Yazdankhah, Fatemeh; Farhadi, Saeid

2018-02-05

A simple, rapid, and reliable headspace solid-phase microextraction (HS-SPME) procedure, reinforced by applying vacuum in the extraction vial, was developed. It was applied for the extraction of nicotine in solid samples prior to determination by gas chromatography-flame ionization detection (GC-FID). First, the surface of a narrow stainless steel wire was made porous and adhesive by platinization to obtain a durable, higher surface area, and resistant fiber. Then, a thin film of sulfonated graphene/polyaniline (Sulf-G/PANI) nanocomposite was synthesized and simultaneously coated on the platinized fiber using the electrophoretic deposition (EPD) method. It was demonstrated that the extraction efficiency remarkably increased by applying the reduced-pressure condition in the extraction vial. To evaluate the conventional HS-SPME and vacuum-assisted HS-SPME (VA-HS-SPME) platforms, all experimental parameters affecting the extraction efficiency including desorption time and temperature, extraction time and temperature and moisture content of sample matrix were optimized. The highest extraction efficiency was obtained at 60°C, 10min (extraction temperature and time) and 280°C, 2min (desorption condition), for VA-HS-SPME strategy, while for conventional HS-SPME the extraction and desorption conditions found to be 100°C, 30min and 280°C, 2min, respectively. The Sulf-G/PANI coated fiber showed high thermal stability, good chemical/mechanical resistance, and long lifetime. For analysis of nicotine in solid samples using VA-HS-SPME-GC-FID, linear dynamic range (LDR) was 0.01-30μgg -1 (R 2 =0.996), the relative standard deviation (RSD%, n=6), for analyses of 1μgg -1 nicotine was calculated 3.4% and limit of detection (LOD) found to be 0.002μgg -1 . The VA-HS-SPME-GC-FID strategy was successfully carried out for quantitation of nicotine in hair and tobacco real samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Mass spectrometry of solid samples in open air using combined laser ionization and ambient metastable ionization

International Nuclear Information System (INIS)

He, X.N.; Xie, Z.Q.; Gao, Y.; Hu, W.; Guo, L.B.; Jiang, L.; Lu, Y.F.

2012-01-01

Mass spectrometry of solid samples in open air was carried out using combined laser ionization and metastable ionization time-of-flight mass spectrometry (LI-MI-TOFMS) in ambient environment for qualitative and semiquantitative (relative analyte information, not absolute information) analysis. Ambient metastable ionization using a direct analysis in realtime (DART) ion source was combined with laser ionization time-of-flight mass spectrometry (LI-TOFMS) to study the effects of combining metastable and laser ionization. A series of metallic samples from the National Institute of Standards and Technology (NIST 494, 495, 498, 499, and 500) and a pure carbon target were characterized using LI-TOFMS in open air. LI-MI-TOFMS was found to be superior to laser-induced breakdown spectroscopy (LIBS). Laser pulse energies between 10 and 200 mJ at the second harmonic (532 nm) of an Nd:YAG laser were applied in the experiment to obtain a high degree of ionization in plasmas. Higher laser pulse energy improves signal intensities of trace elements (such as Fe, Cr, Mn, Ni, Ca, Al, and Ag). Data were analyzed by numerically calculating relative sensitivity coefficients (RSCs) and limit of detections (LODs) from mass spectrometry (MS) and LIBS spectra. Different parameters, such as boiling point, ionization potential, RSC, LOD, and atomic weight, were shown to analyze the ionization and MS detection processes in open air.

Final Report For The Initial Solid Phase Characterization Of The 2011 Grab Samples And Composite For The C-109 Hard Heel Study

International Nuclear Information System (INIS)

Page, J.S.; Cooke, G.A.; Pestovich, J.A.

2011-01-01

On May 3, 2011, solid phase characterization subsamples were taken from six of the eight grab samples that had been collected from tank 241-C-109 in April, 2011 and delivered to the 222-S Laboratory. These subsamples were characterized in order to guide the creation of the composite for the C-109 hard heel study. Visual observation showed that there was a large variability in the physical characteristics of the eight individual grab samples. Several of the grab samples consisted of 'stone-like' cobbles (several > 25 mm in diameter) while the other grab samples were of a finer granular composition referred to as 'bulk material'. Half of the six subsamples taken for this initial SPC were of crushed cobbles and half were of the bulk material. Scanning electron microscopy was performed on all six subsamples, and X-ray diffraction was performed on all three of the 'bulk material' samples and one of the crushed cobble samples. The crushed cobbles were found to be composed primarily of gibbsite (Al(OHh) 3 ). Analysis by X-ray diffraction indicated gibbsite to be the only crystalline phase detected, and scanning electron microscopy showed the crushed cobbles to consist primarily of aggregates of euhedral to subhedral gibbsite crystals that were 20 to 100 μm in size. The aggregates, having a moderate amount of pore space, were cemented primarily by recrystallized gibbsite making them resistant to crushing. The bulk material consisted of coarse to fine-grained pebble-sized (2 to 20 mm) particles. The X-ray diffraction analysis showed them to be a mixture of natrophosphate (Na 7 (PO 4 ) 2 F·19(H 2 O)) and gibbsite crystals in varying amounts in each of the three subsamples (i.e., some grab samples were primarily natrophosphate while others were mixed with gibbsite). The scanning electron microscopy analysis of the bulk material showed the crystals to be euhedral to anhedral (rounded) in shape. Trace phases, too minor to be detected by XRD, were observed in the SEM analysis

Comparison of sampling methods for animal manure

NARCIS (Netherlands)

Derikx, P.J.L.; Ogink, N.W.M.; Hoeksma, P.

1997-01-01

Currently available and recently developed sampling methods for slurry and solid manure were tested for bias and reproducibility in the determination of total phosphorus and nitrogen content of samples. Sampling methods were based on techniques in which samples were taken either during loading from

Metal geochemistry of Nerus River, Terengganu

International Nuclear Information System (INIS)

Chee, Poh Seng; Suhaimi Suratman; Keat, Chew Choon; Norhayati Mohd Tahir

2008-01-01

The Nerus River passes through the Setiu and Kuala Terengganu districts, on the east coast of Peninsular Malaysia. It passes through the populated urban area of northeastern Kuala Terengganu and receives and carries different kinds of agricultural and urban solid and liquid wastes produces by agricultural based industries and domestic sewage. The objective of this study is to investigate trace metal concentration in suspended particulate and water of the Nerus River and relate this to the anthropogenic activities. Water samples were collected from nine sites during dry and pre monsoon seasons (from May to October). Water pH, temperature, electric conductivity and salinity were measured in-situ. The suspended particulate was separated from water by using 0.45 μm pore size acetate cellulose membrane filter. Water (filtered) samples were subjected to APDC-MIBK pre-concentration and particulate samples were totally digested by using strong acids. Cd, Cu, Zn and Pb were analyzed using GFAAS and ICP-OES. Although the overall concentration of the metals obtained were still within Class I limit of the INWQS, however the results indicated that there is an increasing trend of Cu and Zn concentration in Nerus River water compared to previous study done in 2001. High Cu and Zn concentration in suspended matter sampled at downstream station which received effluent from nearby factories. (author)

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.

Municipal Household Solid Waste Compost: Effects on Carrot ...

African Journals Online (AJOL)

An experiment was conducted to evaluate the impact of municipal household solid waste compost on N, P and K uptake and yield of carrot (Daucus carrota), using a coastal savanna Haplic Acrisol. Bulked samples of fresh solid waste from 45 households within the Cape Coast Municipality in the Central Region of Ghana ...

Investigation of environmental samples by low-level gamma spectrometry

Energy Technology Data Exchange (ETDEWEB)

Koehler, M [Nuclear Engineering and Analytics Rossendorf, Inc., Dresden (Germany); Niese, S [Nuclear Engineering and Analytics Rossendorf, Inc., Dresden (Germany)

1997-03-01

The average sample number in our laboratory is about 200 per month (12% technical solid state, 30% geological solid state, 6% geological solid state with low mass, 12% biological, 11% water directly, 25% water after chemical separation, 4% others). In 54% of the measurements the background continuum, and though the detection limit, is determined only by the detector himself and not by the compton continuum from high energy lines in the sample. Some examples in the presented work aim to prove the advantages of gamma ray spectrometry in the underground laboratory Felsenkeller. (orig./DG)

The indicating FTA elute cartridge a solid sample carrier to detect high-risk HPV and high-grade cervical lesions.

Science.gov (United States)

de Bie, Roosmarie P; Schmeink, Channa E; Bakkers, Judith M J E; Snijders, Peter J F; Quint, Wim G V; Massuger, Leon F A G; Bekkers, Ruud L M; Melchers, Willem J G

2011-07-01

The clinically validated high-risk human papillomavirus (hrHPV) Hybrid Capture 2 (HC2) and GP5+/6+-PCR assays were analyzed on an Indicating FTA Elute cartridge (FTA cartridge). The FTA cartridge is a solid dry carrier that allows safe transport of cervical samples. FTA cartridge samples were compared with liquid-based samples for hrHPV and high-grade cervical intraepithelial neoplasia (CIN) detection. One cervical sample was collected in a liquid-based medium, and one was applied to the FTA cartridge. DNA was eluted directly from the FTA cartridge by a simple elution step. HC2 and GP5+/6+-PCR assays were performed on both the liquid-based and the FTA-eluted DNA of 88 women. Overall agreement between FTA and liquid-based samples for the presence of hrHPV was 90.9% with GP5+/6+-PCR and 77.3% with HC2. The sensitivity for high-grade CIN of hrHPV testing on the FTA cartridges was 84.6% with GP5+/6+-PCR and only 53.8% with HC2. By comparison, these sensitivities on liquid-based samples were 92.3% and 100% for GP5+/6+-PCR and HC2, respectively. Therefore, the FTA cartridge shows reasonably good overall agreement for hrHPV detection with liquid-based media when using GP5+/6+-PCR but not HC2 testing. Even with GP5+/6+-PCR, the FTA cartridge is not yet capable of detecting all high-grade CIN lesions. Copyright © 2011 American Society for Investigative Pathology and the Association for Molecular Pathology. Published by Elsevier Inc. All rights reserved.

Solid Loss of Carrots During Simulated Gastric Digestion.

Science.gov (United States)

Kong, Fanbin; Singh, R Paul

2011-03-01

The knowledge of solid loss kinetics of foods during digestion is crucial for understanding the factors that constrain the release of nutrients from the food matrix and their fate of digestion. The objective of this study was to investigate the solid loss of carrots during simulated gastric digestion as affected by pH, temperature, viscosity of gastric fluids, mechanical force present in stomach, and cooking. Cylindrical carrot samples were tested by static soaking method and using a model stomach system. The weight retention, moisture, and loss of dry mass were determined. The results indicated that acid hydrolysis is critical for an efficient mass transfer and carrot digestion. Internal resistance rather than external resistance is dominant in the transfer of soluble solids from carrot to gastric fluid. Increase in viscosity of gastric fluid by adding 0.5% gum (w/w) significantly increased the external resistance and decreased mass transfer rate of carrots in static soaking. When mechanical force was not present, 61% of the solids in the raw carrot samples were released into gastric fluid after 4 h of static soaking in simulated gastric juice. Mechanical force significantly increased solid loss by causing surface erosion. Boiling increased the disintegration of carrot during digestion that may favor the loss of solids meanwhile reducing the amount of solids available for loss in gastric juice. Weibull function was successfully used to describe the solid loss of carrot during simulated digestion. The effective diffusion coefficients of solids were calculated using the Fick's second law of diffusion for an infinite cylinder, which are between 0.75 × 10(-11) and 8.72 × 10(-11) m(2)/s, depending on the pH of the gastric fluid.

Polyaniline-coated cigarette filters as a solid-phase extraction sorbent for the extraction and enrichment of polycyclic aromatic hydrocarbon in water samples.

Science.gov (United States)

Bunkoed, Opas; Rueankaew, Thanaschaphorn; Nurerk, Piyaluk; Kanatharana, Proespichaya

2016-06-01

Polyaniline coated cigarette filters were successfully synthesized and used as a solid-phase extraction sorbent for the extraction and preconcentration of polycyclic aromatic hydrocarbons in water samples. The polyaniline helped to enhance the adsorption ability of polycyclic aromatic hydrocarbons on the sorbent through π-π interactions. The high porosity and large surface area of the cigarette filters helped to reduce backpressure and can be operated with high sample flow rate without loss of extraction efficiency. The developed sorbent was characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. The parameters that affected the extraction efficiencies, i.e. polymerization time, type of desorption solvent and its volume, sample flow rate, sample volume, sample pH, ionic strength, and organic modifier were investigated. Under the optimal conditions, the method was linear over the range of 0.5-10 μg/L and a detection limit of 0.5 ng/L. This simple, rapid, and cost-effective method was successfully applied to the preconcentration of polycyclic aromatic hydrocarbons from water samples. The developed method provided a high enrichment factor with good extraction efficiency (85-98%) and a relative standard deviation <10%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

AUTOMATED ANALYSIS OF AQUEOUS SAMPLES CONTAINING PESTICIDES, ACIDIC/BASIC/NEUTRAL SEMIVOLATILES AND VOLATILE ORGANIC COMPOUNDS BY SOLID PHASE EXTRACTION COUPLED IN-LINE TO LARGE VOLUME INJECTION GC/MS

Science.gov (United States)

Data is presented on the development of a new automated system combining solid phase extraction (SPE) with GC/MS spectrometry for the single-run analysis of water samples containing a broad range of organic compounds. The system uses commercially available automated in-line 10-m...

Bovine serum albumin-Cu(II) hybrid nanoflowers: An effective adsorbent for solid phase extraction and slurry sampling flame atomic absorption spectrometric analysis of cadmium and lead in water, hair, food and cigarette samples

Energy Technology Data Exchange (ETDEWEB)

Yilmaz, Erkan [Department of Chemistry, Faculty of Sciences, Erciyes University, Kayseri 38039 (Turkey); Ocsoy, Ismail [Department of Analytical Chemistry, Faculty of Pharmacy, Erciyes University, Kayseri 38039 (Turkey); Nanotechnology Research Center (ERNAM), Erciyes University, Kayseri 38039 (Turkey); Ozdemir, Nalan [Department of Chemistry, Faculty of Sciences, Erciyes University, Kayseri 38039 (Turkey); Soylak, Mustafa, E-mail: soylak@erciyes.edu.tr [Department of Chemistry, Faculty of Sciences, Erciyes University, Kayseri 38039 (Turkey)

2016-02-04

Herein, the synthesis of bovine serum albumin-Cu(II) hybrid nanoflowers (BSA-NFs) through the building blocks of bovine serum albumin (BSA) and copper(II) ions in phosphate buffered saline (PBS) and their use as adsorbent for cadmium and lead ions are reported. The BSA-NFs, for the first time, were efficiently utilized as novel adsorbent for solid phase extraction (SPE) of cadmium and lead ions in water, food, cigarette and hair samples. The method is based on the separation and pre-concentration of Cd(II) and Pb(II) by BSA-NFs prior to determination by slurry analysis via flame atomic absorption spectrometry (FAAS). The analytes were adsorbed on BSA-NFs under the vortex mixing and then the ion-loaded slurry was separated and directly introduced into the flame AAS nebulizer by using a hand-made micro sample introduction system to eliminate a number of drawbacks. The effects of analytical key parameters, such as pH, amount of BSA-NFs, vortexing time, sample volume, and matrix effect of foreign ions on adsorbing of Cd(II) and Pb(II) were systematically investigated and optimized. The limits of detection (LODs) for Cd(II) and Pb(II) were calculated as 0.37 μg L{sup −1} and 8.8 μg L{sup −1}, respectively. The relative standard deviation percentages (RSDs) (N = 5) for Cd(II) and Pb(II) were 7.2%, and 5.0%, respectively. The accuracy of the developed procedure was validated by the analysis of certified reference materials (TMDA-53.3 Fortified Water, TMDA-70 Fortified Water, SPS-WW2 Waste Water, NCSDC-73349 Bush Branches and Leaves) and by addition/recovery analysis. The quantitative recoveries were obtained for the analysis of certified reference materials and addition/recovery tests. The method was successfully applied to the analysis of cadmium and lead in water, food, cigarette and hair samples. - Highlights: • The synthesis of bovine serum albumin-Cu(II) hybrid nanoflowers is reported. • The nanoflowers were utilized for solid phase microextraction of

Determination of trace amounts of plutonium in environmental samples by RIMS using a high repetition rate solid state laser system

International Nuclear Information System (INIS)

Gruening, C.; Kratz, J.V.; Trautmann, N.; Waldek, A.; Huber, G.; Passler, G.; Wendt, K.

2001-01-01

A reliable and easy to handle high repetition rate solid state laser system has been set up for routine applications of Resonance Ionization Mass Spectrometry (RIMS). It consists of three Titanium-Sapphire (Ti:Sa) lasers pumped by one Nd:YAG laser, providing up to 3 W of tunable laser light each in a wavelength range from 725 nm to 895 nm. The isotope shifts for 238 Pu to 244 Pu have been measured in an efficient ionization scheme with λ 1 =420.76 nm, λ 2 =847.28 nm and λ 3 =767.53 nm. An overall detection efficiency of the RIMS apparatus of ε=1x10 -5 is routinely reached, resulting in a detection limit of 2x10 6 atoms (0.8 fg) of plutonium. The isotopic compositions of synthetic samples and the NIST standard reference material SRM996 were measured. The content of 238 Pu to 242 Pu has been determined in dust samples from the surroundings of a nuclear power plant and 244 Pu was determined in urine samples for the National Radiation Protection Board (NRPB), U.K. Routine operation of plutonium ultratrace detection could thus be established

Zincon-modified activated carbon for solid-phase extraction and preconcentration of trace lead and chromium from environmental samples.

Science.gov (United States)

Li, Zhenhua; Chang, Xijun; Hu, Zheng; Huang, Xinping; Zou, Xiaojun; Wu, Qiong; Nie, Rong

2009-07-15

A new method that utilizes zincon-modified activated carbon (AC-ZCN) as a solid-phase extractant has been developed for simultaneous preconcentration of trace Cr(III) and Pb(II) prior to the measurement by inductively coupled plasma optical emission spectrometry (ICP-OES). The separation/preconcentration conditions of analytes were investigated, including effects of pH, the shaking time, the sample flow rate and volume, the elution condition and the interfering ions. At pH 4, the maximum adsorption capacity of Cr(III) and Pb(II) onto the AC-ZCN were 17.9 and 26.7 mg g(-1), respectively. The adsorbed metal ions were quantitatively eluted by 1 mL of 0.1 mol L(-1) HCl. Common coexisting ions did not interfere with the separation. According to the definition of IUPAC, the detection limits (3 sigma) of this method for Cr(III) and Pb(II) were 0.91 and 0.65 ng mL(-1), respectively. The relative standard deviation under optimum condition is less than 3.5% (n=8). The method has been applied for the determination of Cr(III) and Pb(II) in biological materials and water samples with satisfactory results.

Optimizing sampling approaches along ecological gradients

DEFF Research Database (Denmark)

Schweiger, Andreas; Irl, Severin D. H.; Steinbauer, Manuel

2016-01-01

1. Natural scientists and especially ecologists use manipulative experiments or field observations along gradients to differentiate patterns driven by processes from those caused by random noise. A well-conceived sampling design is essential for identifying, analysing and reporting underlying...... patterns in a statistically solid and reproducible manner, given the normal restrictions in labour, time and money. However, a technical guideline about an adequate sampling design to maximize prediction success under restricted resources is lacking. This study aims at developing such a solid...... and reproducible guideline for sampling along gradients in all fields of ecology and science in general. 2. We conducted simulations with artificial data for five common response types known in ecology, each represented by a simple function (no response, linear, exponential, symmetric unimodal and asymmetric...

Determination of Mineral, Trace Element, and Pesticide Levels in Honey Samples Originating from Different Regions of Malaysia Compared to Manuka Honey

Science.gov (United States)

Moniruzzaman, Mohammed; Chowdhury, Muhammed Alamgir Zaman; Rahman, Mohammad Abdur; Sulaiman, Siti Amrah; Gan, Siew Hua

2014-01-01

The present study was undertaken to determine the content of six minerals, five trace elements, and ten pesticide residues in honeys originating from different regions of Malaysia. Calcium (Ca), magnesium (Mg), iron (Fe), and zinc (Zn) were analyzed by flame atomic absorption spectrometry (FAAS), while sodium (Na) and potassium (K) were analyzed by flame emission spectrometry (FAES). Trace elements such as arsenic (As), lead (Pb), cadmium (Cd), copper (Cu), and cobalt (Co) were analyzed by graphite furnace atomic absorption spectrometry (GFAAS) following the microwave digestion of honey. High mineral contents were observed in the investigated honeys with K, Na, Ca, and Fe being the most abundant elements (mean concentrations of 1349.34, 236.80, 183.67, and 162.31 mg/kg, resp.). The concentrations of the trace elements were within the recommended limits, indicating that the honeys were of good quality. Principal component analysis reveals good discrimination between the different honey samples. The pesticide analysis for the presence of organophosphorus and carbamates was performed by high performance liquid chromatography (HPLC). No pesticide residues were detected in any of the investigated honey samples, indicating that the honeys were pure. Our study reveals that Malaysian honeys are rich sources of minerals with trace elements present within permissible limits and that they are free from pesticide contamination. PMID:24982869

Determination of Mineral, Trace Element, and Pesticide Levels in Honey Samples Originating from Different Regions of Malaysia Compared to Manuka Honey

Directory of Open Access Journals (Sweden)

Mohammed Moniruzzaman

2014-01-01

Full Text Available The present study was undertaken to determine the content of six minerals, five trace elements, and ten pesticide residues in honeys originating from different regions of Malaysia. Calcium (Ca, magnesium (Mg, iron (Fe, and zinc (Zn were analyzed by flame atomic absorption spectrometry (FAAS, while sodium (Na and potassium (K were analyzed by flame emission spectrometry (FAES. Trace elements such as arsenic (As, lead (Pb, cadmium (Cd, copper (Cu, and cobalt (Co were analyzed by graphite furnace atomic absorption spectrometry (GFAAS following the microwave digestion of honey. High mineral contents were observed in the investigated honeys with K, Na, Ca, and Fe being the most abundant elements (mean concentrations of 1349.34, 236.80, 183.67, and 162.31 mg/kg, resp.. The concentrations of the trace elements were within the recommended limits, indicating that the honeys were of good quality. Principal component analysis reveals good discrimination between the different honey samples. The pesticide analysis for the presence of organophosphorus and carbamates was performed by high performance liquid chromatography (HPLC. No pesticide residues were detected in any of the investigated honey samples, indicating that the honeys were pure. Our study reveals that Malaysian honeys are rich sources of minerals with trace elements present within permissible limits and that they are free from pesticide contamination.

The Sample Analysis at Mars Investigation and Instrument Suite

Science.gov (United States)

Mahaffy, Paul; Webster, Christopher R.; Conrad, Pamela G.; Arvey, Robert; Bleacher, Lora; Brinckerhoff, William B.; Eigenbrode, Jennifer L.; Chalmers, Robert A.; Dworkin, Jason P.; Errigo, Therese;

Order-parameter-aided temperature-accelerated sampling for the exploration of crystal polymorphism and solid-liquid phase transitions

International Nuclear Information System (INIS)

Yu, Tang-Qing; Vanden-Eijnden, Eric; Chen, Pei-Yang; Chen, Ming; Samanta, Amit; Tuckerman, Mark

2014-01-01

The problem of predicting polymorphism in atomic and molecular crystals constitutes a significant challenge both experimentally and theoretically. From the theoretical viewpoint, polymorphism prediction falls into the general class of problems characterized by an underlying rough energy landscape, and consequently, free energy based enhanced sampling approaches can be brought to bear on the problem. In this paper, we build on a scheme previously introduced by two of the authors in which the lengths and angles of the supercell are targeted for enhanced sampling via temperature accelerated adiabatic free energy dynamics [T. Q. Yu and M. E. Tuckerman, Phys. Rev. Lett. 107, 015701 (2011)]. Here, that framework is expanded to include general order parameters that distinguish different crystalline arrangements as target collective variables for enhanced sampling. The resulting free energy surface, being of quite high dimension, is nontrivial to reconstruct, and we discuss one particular strategy for performing the free energy analysis. The method is applied to the study of polymorphism in xenon crystals at high pressure and temperature using the Steinhardt order parameters without and with the supercell included in the set of collective variables. The expected fcc and bcc structures are obtained, and when the supercell parameters are included as collective variables, we also find several new structures, including fcc states with hcp stacking faults. We also apply the new method to the solid-liquid phase transition in copper at 1300 K using the same Steinhardt order parameters. Our method is able to melt and refreeze the system repeatedly, and the free energy profile can be obtained with high efficiency

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

African Journals Online (AJOL)

NICO

for the addition of organic modifier, sample load volume, conditioning solvent, washing solvent and ... Solid phase extraction, polycyclic aromatic hydrocarbons, water samples, ... such as polymeric, activated carbon or silica modified with.

Determination of 13 endocrine disrupting chemicals in environmental solid samples using microwave-assisted solvent extraction and continuous solid-phase extraction followed by gas chromatography-mass spectrometry.

Science.gov (United States)

Azzouz, Abdelmonaim; Ballesteros, Evaristo

2016-01-01

Soil can contain large numbers of endocrine disrupting chemicals (EDCs). The varied physicochemical properties of EDCs constitute a great challenge to their determination in this type of environmental matrix. In this work, an analytical method was developed for the simultaneous determination of various classes of EDCs, including parabens, alkylphenols, phenylphenols, bisphenol A, and triclosan, in soils, sediments, and sewage sludge. The method uses microwave-assisted extraction (MAE) in combination with continuous solid-phase extraction for determination by gas chromatography-mass spectrometry. A systematic comparison of the MAE results with those of ultrasound-assisted and Soxhlet extraction showed MAE to provide the highest extraction efficiency (close to 100%) in the shortest extraction time (3 min). The proposed method provides a linear response over the range 2.0 - 5000 ng kg(-1) and features limits of detection from 0.5 to 4.5 ng kg(-1) depending on the properties of the EDC. The method was successfully applied to the determination of target compounds in agricultural soils, pond and river sediments, and sewage sludge. The sewage sludge samples were found to contain all target compounds except benzylparaben at concentration levels from 36 to 164 ng kg(-1). By contrast, the other types of samples contained fewer EDCs and at lower concentrations (5.6 - 84 ng kg(-1)).

Speciation of selenium in environmental samples by solid-phase spectrophotometry using 2,3-dichloro-6-(2,7-dihydroxy-naphthylazo)quinoxaline.

Science.gov (United States)

Amin, Alaa S

2014-01-01

Solid-phase spectrophotometry was applied to determination of trace amounts of selenium (Se) in water, soil, plant materials, human hair, and a cosmetic preparation (lipstick). Se(IV) was sorbed in a dextran type lipophilic gel as a complex with 2,3-dichloro-6-(2,7-dihydroxy-naphthylazo)quinoxaline (DCDHNAQ), whereas Se(VI) was determined after boiling in HCI for 10 min to convert Se(VI) to Se(IV). Resin phase absorbances at 588 and 800 nm were measured directly, which allowed the determination of Se in the range of 0.2-3.3 microg/L with an RSD of 1.22%. The influences of analytical parameters including pH of the aqueous solution, amounts of DCDHNAQ, and sample volume were investigated. The molar absorptivities were found to be 1.09 x 10(6), 4.60 x 10(6), and 1.23 x 10(7) L/mol cm for 100, 500, and 1000 mL, respectively. The LOD and LOQ of the 500 mL sample method were 110 and 360 ng/L, respectively, when using 50 mg dextran type lipophilic gel. For a 1000 mL sample, the LOD and LOQ were 60 and 200 ng/L, respectively, using 50 mg of the exchanger. Increasing the sample volume enhanced the sensitivity. No considerable interferences were observed from other investigated anions and cations on the Se determination.

Solid phase microextraction.

Science.gov (United States)

Pawliszyn, J

2001-01-01

Solid Phase Microextraction (SPME) uses a small volume of sorbent dispersed typically on the surface of small fibres, to isolate and concentrate analytes from sample matrix. After contact with sample, analytes are absorbed or adsorbed by the fibre phase (depending on the nature of the coating) until an equilibrium is reached in the system. The amount of an analyte extracted by the coating at equilibrium is determined by the magnitude of the partition coefficient of the analyte between the sample matrix and the coating material. After the extraction step, the fibres are transferred, with the help of a syringe-like handling device, to analytical instrument, for separation and quantitation of target analytes. This technique integrates sampling, extraction and sample introduction and is a simple way of facilitating on-site monitoring. Applications of this technique include environmental monitoring, industrial hygiene, process monitoring, clinical, forensic, food, flavour, fragrance and drug analyses, in laboratory and on-site analysis.

The potential of household solid waste reduction in Sukomanunggal District, Surabaya

Science.gov (United States)

Warmadewanthi, I. D. A. A.; Kurniawati, S.

2018-01-01

The rapid population growth affects the amount of waste generated. Sukomanunggal Subdistrict is the densest area in West Surabaya which has a population of 100,602 inhabitants with a total area of 11.2 km2. The population growth significantly affects the problem of limited land for landfill facilities (final processing sites). According to the prevailing regulations, solid waste management solutions include the solid waste reduction and management. This study aims to determine the potential reduction of household solid waste at the sources. Household solid waste samplings were performed for eight consecutive days. The samples were then analyzed to obtain the generation rate, density, and composition so that the household solid waste reduction potential for the next 20 years could be devised. Results of the analysis showed that the value of waste is 0.27 kg/person/day, while the total household solid waste generation amounted to 27,162.58 kg/day or 187.70 m3/day. Concerning the technical aspects, the current solid waste reduction in Sukomanunggal Subdistrict has reached 2.1% through the application of waste bank, composting, and scavenging activities at the dumping sites by the garbage collectors. In the year of 2036, the potential reduction of household solid waste in Sukomanunggal Subdistrict has been estimated to reach 28.0%.

Municipal Solid Waste Characterization according to Different Income Levels: A Case Study

Directory of Open Access Journals (Sweden)

Huseyin Kurtulus Ozcan

2016-10-01

Full Text Available Solid waste generation and characterization are some of the most important parameters which affect environmental sustainability. Municipal solid waste (MSW characterization depends on social structure and income levels. This study aims to determine the variations in waste components within MSW mass by income levels and seasonal conditions following the analysis conducted on the characterization of solid wastes produced in the Kartal district of the province of Istanbul, which is the research area of this study. To this end, 1.9 tons of solid waste samples were collected to represent four different lifestyles (high, medium, and low income levels, and downtown in the winter and summer periods, and characterization was made on these samples. In order to support waste characterization, humidity content and calorific value analyses were also conducted and various suggestions were brought towards waste management in line with the obtained findings. According to the results obtained in the study, organic waste had the highest rate of waste mass by 57.69%. Additionally, significant differences were found in municipal solid waste components (MSWC based on income level. Average moisture content (MC of solid waste samples was 71.1% in moisture analyses. The average of calorific (heating value (HHV was calculated as 2518.5 kcal·kg−1.

Determination of multi-class herbicides in soil by liquid-solid extraction coupled with headspace solid phase microextraction method

Directory of Open Access Journals (Sweden)

Đurović-Pejčev Rada

2016-01-01

Full Text Available A method is described for simultaneous determination of five herbicides (metribuzin, acetochlor, clomazone, oxyfluorfen and dimethenamid belonging to different pesticides groups in soil samples. Developed headspace solid phase microextraction method (HS-SPME in combination with liquid-solid sample preparation (LS was optimized and applied in the analysis of some agricultural samples. Optimization of microextraction conditions, such as temperature, extraction time and sodium chloride (NaCl content was perfor-med using 100 μm polydimethyl-siloxane (PDMS fiber. The extraction effi-ciencies of methanol, methanol:acetone=1:1 and methanol:acetone:hexane= =2:2:1 and the optimum number of extraction steps during the sample prepa-ration, were tested, as well. Gas chromatography-mass spectrometry (GC-MS was used for detection and quantification, obtaining relative standard deviation (RSD below 13%, and recovery values higher than 83% for multiple analyses of soil samples fortified at 30 μg kg-1 of each herbicide. Limits of detection (LOD were less than 1.2 μg kg-1 for all the studied herbicides. [Projekat Ministarstva nauke Republike Srbije, br. TR31043 i br. III43005

Characterization of domestic graywater and graywater solids.

Science.gov (United States)

Sievers, Jan Christian; Londong, Jörg

2018-03-01

The knowledge of loads and concentrations is fundamental for the design of graywater treatment units, but the data on the characteristics of graywater and in particular graywater solids are weak. As general design values regarding graywater treatment facilities are not available for Germany, the objective of this article is to elaborate the characteristics of graywater and graywater solids. This paper describes the results of six sampling campaigns carried out on graywater systems in the German cities Berlin, Lübeck and Kiel. All graywater samples were collected proportional to the flow and the graywater solids were gathered separately. The collected data include graywater volumes and characteristics regarding the organic pollution (chemical oxygen demand (COD), 5-day biochemical oxygen demand (BOD 5 )) and nutrients (total nitrogen (TN), total phosphorus (TP)). The graywater volume fluctuated depending on the location. The specific average flow was 68 litre per inhabitant per day (L/inh.d). Inhabitant-specific loads of 49.3 gCOD t /inh·d, 28 gBOD 5 /inh.d, 1 gTN t /inh.d and 0.38 gTP t /inh.d (subscript 't' = total) were found. Information about the composition of graywater solids in terms of quantity and quality is seriously lacking. Therefore, graywater solids were examined with respect to organic matter (COD) and nutrients (TN, TP). The contribution of graywater solids with particle sizes over 200 microns in relation to the total inhabitant-specific load was approximately 3-8% depending on the parameter. The qualitative and quantitative characteristics of the investigated graywater fractions may serve as a base for the estimation of design values.

An improved sampling system installed for reprocessing

International Nuclear Information System (INIS)

Finsterwalder, L.; Zeh, H.

1979-03-01

Sampling devices are needed for taking representative samples from individual process containers during the reprocessing of irradiated fuel. The aqueous process stream in a reprocessing plant frequently contains, in addition to the dissolved radioactive materials, more or less small quantities of solid matter fraction of fuel material still remaining undissolved, insoluble fission-, corrosion-, or degradation products as well, in exceptional cases, ion exchange resin or silica gel. The solid matter is deposited partly on the upper surfaces of the sampling system and the radiation due to this makes maintenance and repair of the sampler more difficult. The purpose of the development work was to reduce the chance of accident and the maintenance costs and to lower the radiation exposure of the personnel. A new sampling system was developed and is described. (author)

Effect of plastic deformation and impurities on internal friction in solid He4

International Nuclear Information System (INIS)

Tsymbalenko, V.L.; AN SSSR, Chernogolovka. Inst. Fiziki Tverdogo Tela)

1979-01-01

The internal friction in solid He 4 samples of 20.55 cm 3 molar volume is measured at frequencies of 15 and 78 kHz. The samples are grown under constant pressure and also by the blocked capillary technique. The construction of the container was such that the damping on plastic deformation of solid helium could be measured. Internal friction is also investigated in solid helium samples containing admixtures of He 3 (from 0.01 to 0.1 at.%). A number of dislocation parameters could be determined on basis of the temperature and amplitude dependences of the damping predicted by the Granato-Lucke theory

Novel polyamide-based nanofibers prepared by electrospinning technique for headspace solid-phase microextraction of phenol and chlorophenols from environmental samples

Energy Technology Data Exchange (ETDEWEB)

Bagheri, Habib, E-mail: bagheri@sharif.edu [Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, Azadi Av., P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of); Aghakhani, Ali; Baghernejad, Masoud; Akbarinejad, Alireza [Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, Azadi Av., P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of)

2012-02-24

A novel solid phase microextraction (SPME) fiber was fabricated by electrospinning method in which a polymeric solution was converted to nanofibers using high voltages. A thin stainless steel wire was coated by the network of polymeric nanofibers. The polymeric nanofiber coating on the wire was mechanically stable due to the fine and continuous nanofibers formation around the wire with a three dimensional structure. Polyamide (nylon 6), due to its suitable characteristics was used to prepare the unbreakable SPME nanofiber. The scanning electron microscopy (SEM) images of this new coating showed a diameter range of 100-200 nm for polyamide nanofibers with a homogeneous and porous surface structure. The extraction efficiency of new coating was investigated for headspace solid-phase microextraction (HS-SPME) of some environmentally important chlorophenols from aqueous samples followed by gas chromatography-mass spectrometry (GC-MS) analysis. Effect of different parameters influencing the extraction efficiency including extraction temperature, extraction time, ionic strength and polyamide amount were investigated and optimized. In order to improve the chromatographic behavior of phenolic compounds, all the analytes were derivatized prior to the extraction process using basic acetic anhydride. The detection limits of the method under optimized conditions were in the range of 2-10 ng L{sup -1}. The relative standard deviations (RSD) (n = 3) at the concentration level of 1.7-6.7 ng mL{sup -1} were obtained between 1 and 7.4%. The calibration curves of chlorophenols showed linearity in the range of 27-1330 ng L{sup -1} for phenol and monochlorophenols and 7-1000 ng L{sup -1} for dichloro and trichlorophenols. Also, the proposed method was successfully applied to the extraction of phenol and chlorophenols from real water samples and relative recoveries were between 84 and 98% for all the selected analytes except for 2,4,6 tricholophenol which was between 72 and 74%.

Equipment and techniques for remote sampling of stored radioactive waste

International Nuclear Information System (INIS)

Nance, T.A.

1996-01-01

Several tools have been developed at the Savannah River Site (SRS) to remotely sample stored radioactive waste. These sampling tools have been developed to determine the chemical characteristics of the waste prior to processing. The processing of waste material varies according to the chemical characteristics of the waste, which change due to additions, settling, mixing, and chemical reactions during storage. Once the waste has been sampled to identify its characteristics, the chemical composition of the waste can then be altered if needed to prepare for processing. Various types of waste material in several types of containment must be sampled at SRS. Stored waste materials consist of liquids, floating organics, sludge, salt and solids. Waste is stored in four basic types of tanks with different means of access and interior obstructions. The waste tanks can only be accessed by small openings: access ports, risers and downcomers. Requirements for sampling depend on the type of tank being accessed, the waste within the tank, and the particular location in the tank desired for taking the sample. Sampling devices have been developed to sample all of the waste material forms found in the SRS tank farms. The fluid type samplers are capable of sampling surface liquid, subsurface liquid at varying depth, surface sludge, subsurface sludge, and floating organics. The solid type samplers are capable of sampling salt, sampling a solid layer on the bottom of the tank, and capturing a small solid mass on the tank bottom. The sampling devices are all designed to access the tanks through small access ports. The samplers are reusable and are designed to allow quick transfer of the samples to shielded packaging for transport, reducing the amount of radiation exposure to sampling personnel. The samplers weigh less than 100 lb. and are designed in sections to allow easy disassembly for storage and transport by personnel. (Abstract Truncated)

Determination of tellurium at ultra-trace levels in drinking water by on-line solid phase extraction coupled to graphite furnace atomic absorption spectrometer

International Nuclear Information System (INIS)

Pedro, Juana; Stripekis, Jorge; Bonivardi, Adrian; Tudino, Mabel

2008-01-01

In this paper, two time-based flow injection (FI) separation pre-concentration systems coupled to graphite furnace atomic absorption spectrometry (GFAAS) for tellurium determination are studied and compared. The first alternative involves the pre-concentration of the analyte onto Dowex 1X8 employed as packaging material of a micro-column inserted in the flow system. The second set-up is based on the co-precipitation of tellurium with La(OH) 3 followed by retention onto XAD resins. Both systems are compared in terms of limit of detection, linear range, RSD%, sample throughput, micro-columns lifetime and aptitude for fully automatic operation. The features of the Dowex system are: 37% efficiency of retention and an enhancement factor of 42 for a pre-concentration time of 180 seconds (sample flow rate = 3 ml min -1 ) with acetic acid elution volumes of 80 μl. The detection limit (3 s) is 7 ng l -1 and the relative standard deviation (n = 7200 ng l -1 ) is 5.8%. The analytical performance of the XAD system is: 72% efficiency of retention and an enhancement factor of 25 for a pre-concentration time of 180 s (sample flow rate = 3 ml min -1 ) with nitric acid elution volumes of 300 μl. The detection limit is 66 ng l -1 and the relative standard deviation (n = 7200 ng l -1 ) is 8.3%. Applications to the determination of tellurium in tap water and the validation of the analytical methodology employing SRM 1643e as certified reference material are shown

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

Determination of thallium at ultra-trace levels in water and biological samples using solid phase spectrophotometry.

Science.gov (United States)

Amin, Alaa S; El-Sharjawy, Abdel-Azeem M; Kassem, Mohammed A

2013-06-01

A new simple, very sensitive, selective and accurate procedure for the determination of trace amounts of thallium(III) by solid-phase spectrophotometry (SPS) has been developed. The procedure is based on fixation of Tl(III) as quinalizarin ion associate on a styrene-divinylbenzene anion-exchange resin. The absorbance of resin sorbed Tl(III) ion associate is measured directly at 636 and 830 nm. Thallium(I) was determined by difference measurements after oxidation of Tl(I) to Tl(III) with bromine. Calibration is linear over the range 0.5-12.0 μg L(-1) of Tl(III) with relative standard deviation (RSD) of 1.40% (n=10). The detection and quantification limits are 150 and 495 ng L(-1) using 0.6 g of the exchanger. The molar absorptivity and Sandell sensitivity are also calculated and found to be 1.31×10(7) L mol(-1)cm(-1) and 0.00156 ng cm(-2), respectively. The proposed procedure has been successfully applied to determine thallium in water, urine and serum samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Determination of thallium at ultra-trace levels in water and biological samples using solid phase spectrophotometry

Science.gov (United States)

Amin, Alaa S.; El-Sharjawy, Abdel-Azeem M.; Kassem, Mohammed A.

2013-06-01

A new simple, very sensitive, selective and accurate procedure for the determination of trace amounts of thallium(III) by solid-phase spectrophotometry (SPS) has been developed. The procedure is based on fixation of Tl(III) as quinalizarin ion associate on a styrene-divinylbenzene anion-exchange resin. The absorbance of resin sorbed Tl(III) ion associate is measured directly at 636 and 830 nm. Thallium(I) was determined by difference measurements after oxidation of Tl(I) to Tl(III) with bromine. Calibration is linear over the range 0.5-12.0 μg L-1 of Tl(III) with relative standard deviation (RSD) of 1.40% (n = 10). The detection and quantification limits are 150 and 495 ng L-1 using 0.6 g of the exchanger. The molar absorptivity and Sandell sensitivity are also calculated and found to be 1.31 × 107 L mol-1 cm-1 and 0.00156 ng cm-2, respectively. The proposed procedure has been successfully applied to determine thallium in water, urine and serum samples.

Solid-phase extraction of polar pesticides from environmental water samples on graphitized carbon and Empore-activated carbon disks and on-line coupling to octadecyl-bonded silica analytical columns.

NARCIS (Netherlands)

Slobodník, J.; Oztekizan, O.; Lingeman, H.; Brinkman, U.A.T.

1996-01-01

The suitability of Empore-activated carbon disks (EACD), Envi-Carb graphitized carbon black (GCB) and CPP-50 graphitized carbon for the trace enrichment of polar pesticides from water samples was studied by means of off-line and on-line solid-phase extraction (SPE). In the off-line procedure, 0.5-2

Determination of structure of oriented samples using two-dimensional solid state NMR techniques

International Nuclear Information System (INIS)

Jin Hong; Harbison, G.S.

1990-01-01

One dimensional and two-dimensional MAS techniques can give detailed information about the structure and dynamics of oriented systems. We describe the application of such techniques to the liquid-crystalline polymer poly(p-phenyleneterphtalimide) (PPTA), and thence deduce the solid-state structure of the material. (author). 9 refs.; 6 figs

Forensic analysis of high explosives residues in post-blast water samples employing solid phase extraction for analyte pro-concentration

International Nuclear Information System (INIS)

Umi Kalsom Ahmad; Rajendran, Sumathy; Ling, Lee Woan

2008-01-01

Nitro aromatic, nitramine and nitrate ester compounds are a major group of high order explosive or better known as military explosives. Octahydro-1,3,5,7-tetrazocine (HMX), 1,3,5-hexahydro-1,3,5-trinitro triazine (RDX), 2,4,6-trinitro-toluene (TNT), pentaerythritol tetranitrate (PETN) and 2,4-dinitrotoluene (2,4-DNT) are secondary high explosives classified as most commonly used explosives components. There is an increasing demand for pre-concentration of these compounds in water samples as the sensitivity achieved by instrumental analytical methods for these high explosives residues are the main drawback in the application at trace levels for forensic analysis. Hence, a simple cartridge solid phase extraction (SPE) procedure was optimized as the off-line extraction and pre-concentration method to enhance the detection limit of high explosive residues using micellar electrokinetic chromatography (MEKC) and gas chromatography with electron-capture detection (GC-ECD) methods. The SPE cartridges utilized LiChrolut EN as the SPE adsorbent. By emplying pre-concentration using SPE, the detection limits of the target analytes in water sample were lowered by more than 1000 times with good percentage recovery (>87%) for MEKC method and lowered by 120 times with more than 2 % percentage recovery for GC-ECD methods. In order to test the feasibility of the developed method to real cases, post-blast water samples were analyzed. The post-blast water samples which were collected from Baling Bom training range, Ulu Kinta, Perak contained RDX and PETN in the range of 0.05 - 0.17 ppm and 0.0124 - 0.0390 ppm respectively. (author)

[Monitoring of the residue of fosthiazate in water samples using solid-phase extraction coupled with gas chromatography/mass spectrometry].

Science.gov (United States)

Zhu, Jing; Zhou, Xin; Fu, Chunmei; Liu, Sankang; Li, Zhangwan

2004-11-01

Solid-phase extraction (SPE) coupled with gas chromatography/mass spectrometry (GC/MS) was used to determine the fosthiazate residue in water samples. The water samples were first filtered through cellulose filters (0.45 microm pore size). A 100 mL volume of filtered water, in which 1 mL of methanol has been added, was then passed through a pre-conditioned 3 cm C18 cartridge at a flow-rate of 1.5 mL/min. Elution was performed by 1 mL of methanol. The eluant was finally dried under reduced pressure for solvent evaporation. The volume was quantitatively adjusted to 0.5 mL with methanol. The analysis was carried out on GC/MS. The mass spectrometer was operated in selected ion monitoring (SIM) mode. According to mass spectrum of fosthiazate, three selected ions at m/z of 126, 195, 283, respectively, were monitored for identification and quantification. High sensitivity and selectivity were achieved by using this method. The limit of detection for fosthiazate in water samples was determined to be 56.4 ng/L. The linearity was demonstrated over a wide range of concentrations covering from 0.282 to 141 microg/L. The recoveries were more than 85.5% and the relative standard deviations for the overall procedure were less than 4.42%. The fosthiazate residue was detected in the water samples from a pool near cropland where fosthiazate was used. The results demonstrate the suitability of the SPE-GC/MS approach for the analysis of fosthiazate in water.

Influence of sampling frequency and load calculation methods on quantification of annual river nutrient and suspended solids loads.

Science.gov (United States)

Elwan, Ahmed; Singh, Ranvir; Patterson, Maree; Roygard, Jon; Horne, Dave; Clothier, Brent; Jones, Geoffrey

2018-01-11

Better management of water quality in streams, rivers and lakes requires precise and accurate estimates of different contaminant loads. We assessed four sampling frequencies (2 days, weekly, fortnightly and monthly) and five load calculation methods (global mean (GM), rating curve (RC), ratio estimator (RE), flow-stratified (FS) and flow-weighted (FW)) to quantify loads of nitrate-nitrogen (NO 3 - -N), soluble inorganic nitrogen (SIN), total nitrogen (TN), dissolved reactive phosphorus (DRP), total phosphorus (TP) and total suspended solids (TSS), in the Manawatu River, New Zealand. The estimated annual river loads were compared to the reference 'true' loads, calculated using daily measurements of flow and water quality from May 2010 to April 2011, to quantify bias (i.e. accuracy) and root mean square error 'RMSE' (i.e. accuracy and precision). The GM method resulted into relatively higher RMSE values and a consistent negative bias (i.e. underestimation) in estimates of annual river loads across all sampling frequencies. The RC method resulted in the lowest RMSE for TN, TP and TSS at monthly sampling frequency. Yet, RC highly overestimated the loads for parameters that showed dilution effect such as NO 3 - -N and SIN. The FW and RE methods gave similar results, and there was no essential improvement in using RE over FW. In general, FW and RE performed better than FS in terms of bias, but FS performed slightly better than FW and RE in terms of RMSE for most of the water quality parameters (DRP, TP, TN and TSS) using a monthly sampling frequency. We found no significant decrease in RMSE values for estimates of NO 3 - N, SIN, TN and DRP loads when the sampling frequency was increased from monthly to fortnightly. The bias and RMSE values in estimates of TP and TSS loads (estimated by FW, RE and FS), however, showed a significant decrease in the case of weekly or 2-day sampling. This suggests potential for a higher sampling frequency during flow peaks for more precise

High-Precision In Situ 87Sr/86Sr Analyses through Microsampling on Solid Samples: Applications to Earth and Life Sciences

Directory of Open Access Journals (Sweden)

Sara Di Salvo

2018-01-01

Full Text Available An analytical protocol for high-precision, in situ microscale isotopic investigations is presented here, which combines the use of a high-performing mechanical microsampling device and high-precision TIMS measurements on micro-Sr samples, allowing for excellent results both in accuracy and precision. The present paper is a detailed methodological description of the whole analytical procedure from sampling to elemental purification and Sr-isotope measurements. The method offers the potential to attain isotope data at the microscale on a wide range of solid materials with the use of minimally invasive sampling. In addition, we present three significant case studies for geological and life sciences, as examples of the various applications of microscale 87Sr/86Sr isotope ratios, concerning (i the pre-eruptive mechanisms triggering recent eruptions at Nisyros volcano (Greece, (ii the dynamics involved with the initial magma ascent during Eyjafjallajökull volcano’s (Iceland 2010 eruption, which are usually related to the precursory signals of the eruption, and (iii the environmental context of a MIS 3 cave bear, Ursus spelaeus. The studied cases show the robustness of the methods, which can be also be applied in other areas, such as cultural heritage, archaeology, petrology, and forensic sciences.

Packed in-tube solid phase microextraction with graphene oxide supported on aminopropyl silica: Determination of target triazines in water samples.

Science.gov (United States)

De Toffoli, Ana L; Fumes, Bruno H; Lanças, Fernando M

2018-02-22

On-line in-tube solid phase microextraction (in-tube SPME) coupled to high performance liquid chromatography and tandem mass spectrometry (HPLC-MS/MS) was successfully applied to the determination of selected triazines in water samples. The method based on the employment of a packed column containing graphene oxide (GO) supported on aminopropyl silica (Si) showed that the extraction phase has a high potential for triazines extraction aiming to its physical-chemical properties including ultrahigh specific surface area, good mechanical and thermal stability and high fracture strength. Injection volume and loading time were both investigated and optimized. The method validation using Si-GO to extract and concentrate the analytes showed satisfactory results, good sensitivity, good linearity (0.2-4.0 µg L -1 ) and low detection limits (1.1-2.9 ng L -1 ). The high extraction efficiency was determined with enrichment factors ranging from 1.2-2.9 for the lowest level, 1.3-4.9 intermediate level and 1.2-3.0 highest level (n = 3). Although the analytes were not detected in the real samples evaluated, the method has demonstrated to be efficient through its application in the analysis of spiked triazines in ground and mineral water samples.

Rheology and TIC/TOC results of ORNL tank samples

International Nuclear Information System (INIS)

Pareizs, J. M.; Hansen, E. K.

2013-01-01

The Savannah River National Laboratory (SRNL)) was requested by Oak Ridge National Laboratory (ORNL) to perform total inorganic carbon (TIC), total organic carbon (TOC), and rheological measurements for several Oak Ridge tank samples. As received slurry samples were diluted and submitted to SRNL-Analytical for TIC and TOC analyses. Settled solids yield stress (also known as settled shear strength) of the as received settled sludge samples were determined using the vane method and these measurements were obtained 24 hours after the samples were allowed to settled undisturbed. Rheological or flow properties (Bingham Plastic viscosity and Bingham Plastic yield stress) were determined from flow curves of the homogenized or well mixed samples. Other targeted total suspended solids (TSS) concentrations samples were also analyzed for flow properties and these samples were obtained by diluting the as-received sample with de-ionized (DI) water

Culture methods of allograft musculoskeletal tissue samples in Australian bacteriology laboratories.

Science.gov (United States)

Varettas, Kerry

2013-12-01

Samples of allograft musculoskeletal tissue are cultured by bacteriology laboratories to determine the presence of bacteria and fungi. In Australia, this testing is performed by 6 TGA-licensed clinical bacteriology laboratories with samples received from 10 tissue banks. Culture methods of swab and tissue samples employ a combination of solid agar and/or broth media to enhance micro-organism growth and maximise recovery. All six Australian laboratories receive Amies transport swabs and, except for one laboratory, a corresponding biopsy sample for testing. Three of the 6 laboratories culture at least one allograft sample directly onto solid agar. Only one laboratory did not use a broth culture for any sample received. An international literature review found that a similar combination of musculoskeletal tissue samples were cultured onto solid agar and/or broth media. Although variations of allograft musculoskeletal tissue samples, culture media and methods are used in Australian and international bacteriology laboratories, validation studies and method evaluations have challenged and supported their use in recovering fungi and aerobic and anaerobic bacteria.

Determination of fluorine in copper concentrate via high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis - Comparison of three target molecules.

Science.gov (United States)

Cadorim, Heloisa R; de Gois, Jefferson S; Borges, Aline R; Vale, Maria Goreti R; Welz, Bernhard; Gleisner, Heike; Ott, Christina

2018-01-01

The chemical composition of complex inorganic materials, such as copper concentrate, may influence the economics of their further processing because most smelters, and particularly the producers of high-purity electrolyte copper, have strict limitations for the permissible concentration of impurities. These components might be harmful to the quality of the products, impair the production process and be hazardous to the environment. The goal of the present work is the development of a method for the determination of fluorine in copper concentrate using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis. The molecular absorption of the diatomic molecule CaF was measured at 606.440nm. The molecule CaF was generated by the addition of 200µg Ca as the molecule-forming reagent; the optimized pyrolysis and vaporization temperatures were 900°C and 2400°C, respectively. The characteristic mass and limit of detection were 0.5ng and 3ng, respectively. Calibration curves were established using aqueous standard solutions containing the major components Cu, Fe, S and the minor component Ag in optimized concentrations. The accuracy of the method was verified using certified reference materials. Fourteen copper concentrate samples from Chile and Australia were analyzed to confirm the applicability of the method to real samples; the concentration of fluorine ranged from 34 to 5676mgkg -1 . The samples were also analyzed independently at Analytik Jena by different operators, using the same equipment, but different target molecules, InF and GaF, and different operating conditions; but with a few exceptions, the results agreed quite well. The results obtained at Analytik Jena using the GaF molecule and our results obtained with CaF, with one exception, were also in agreement with the values informed by the supplier of the samples, which were obtained using ion selective electrode potentiometry after alkaline fusion. A comparison will

Photothermoacoustic effect in solids with piezoelectric detection

International Nuclear Information System (INIS)

Kozachenko, V. V.; Kucherov, I.Ya.

2004-01-01

Full text: In the last few years, a growing interest has been expressed in studies of substances in different aggregate states which were performed with the help of the photothermoacoustic PTA effect. Main in this method is use of thermal waves as the carrier of the information about properties of explored substance. The excitation of thermal waves is carried out, as a rule, by modulated light flux. A specific feature of the PTA effect is the dependence of the information obtained from it on the method used for detecting thermal waves. One of the most sensitive methods for detecting a PTA signal is the piezoelectric method. For studies of solids, the PTA effect in plates offers considerable promise. In this work, PTA effect in a solid-piezoelectric layered structure is studied theoretically and experimentally. The layered plate consisting of an isotropic solid and piezoelectric crystal of a class 6 mm (or piezoelectric ceramics) is considered. The surface of a solid body is uniformly irradiated with a modulated light flux. The sample is heated and the thermal waves are generated. In the sample, the temperature field of thermal waves generates, due to the thermoelastic effect, acoustic vibration and waves that are registered by a piezoelectric. Expressions for the potential difference U across an arbitrary layer of piezoelectric transducer are derived. The solid bodies with various optical and thermal properties for cases of one-layer and two-layer piezoelectric transducer are analyzed. In particular, is shown, that for the case two-layer piezoelectric transducer, in the high-frequency region, the amplitude ratio U 1 / U 2 the tangent of the phase difference tg(Δφ) of signals taken from individual layers of the transducer depend almost linearly on the inverse square root of the frequency f -1/2 . With use of these features, the new method of definition of some elastic and thermal parameters of solid bodies offered. An experiment is performed with samples Cu, Fe

Granular deformation mechanisms in semi-solid alloys

International Nuclear Information System (INIS)

Gourlay, C.M.; Dahle, A.K.; Nagira, T.; Nakatsuka, N.; Nogita, K.; Uesugi, K.; Yasuda, H.

2011-01-01

Deformation mechanisms in equiaxed, partially solid Al-15 wt.% Cu are studied in situ by coupling shear-cell experiments with synchrotron X-ray radiography. Direct evidence is presented for granular deformation mechanisms in both globular and equiaxed-dendritic samples at solid fractions shortly after crystal impingement. It is demonstrated that dilatancy, arching and jamming occur at the crystal scale, and that these can cause stick-slip flow due to periodic dilation and compaction at low displacement rate. Granular deformation is found to be similar in globular and equiaxed-dendritic samples if length is scaled by the crystal size and packing is considered to occur among crystal envelopes. Rheological differences between the morphologies are discussed in terms of the competition between crystal rearrangement and crystal deformation.

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.

Cork as a new (green) coating for solid-phase microextraction: Determination of polycyclic aromatic hydrocarbons in water samples by gas chromatography–mass spectrometry

International Nuclear Information System (INIS)

Dias, Adriana Neves; Simão, Vanessa; Merib, Josias; Carasek, Eduardo

2013-01-01

Highlights: ► Cork as a new coating for solid-phase microextraction was proposed. ► Good results were achieved, demonstrating the applicability of the cork as coating for SPME. ► The efficiency of cork fiber was very similar to commercially available fibers. -- Abstract: A new fiber for solid-phase microextraction (SPME) was prepared employing cork as a coating. The morphology and composition of the cork fiber was evaluated by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR), respectively. The proposed fiber was used for the determination of polycyclic aromatic hydrocarbons (PAHs) in river water samples by gas chromatography–selected ion monitoring–mass spectrometry (GC–SIM–MS). A central composite design was used for optimization of the variables involved in the extraction of PAHs from water samples. The optimal extraction conditions were extraction time and temperature of 60 min and 80 °C, respectively. The detection and quantification limits were 0.03 and 0.1 μg L −1 , respectively. The recovery values were between 70.2 and 103.2% and the RSD was ≤15.7 (n = 3). The linear range was 0.1–10 μg L −1 with r ≥ 0.96 and the fiber-to-fiber reproducibility showed RSD ≤ 18.6% (n = 5). The efficiency of the cork fiber was compared with commercially available fibers and good results were achieved, demonstrating the applicability and great potential of cork as a coating for SPME

Effect of Binding Components in Complex Sample Matrices on Recovery in Direct Immersion Solid-Phase Microextraction: Friends or Foe?

Science.gov (United States)

Alam, Md Nazmul; Pawliszyn, Janusz

2018-02-20

The development of matrix compatible coatings for solid-phase microextraction (SPME) has enabled direct extraction of analytes from complex sample matrices. The direct immersion (DI) mode of SPME when utilized in conjunction with such extraction phases facilitates extraction of a wide range of analytes from complex matrices without the incurrence of fouling or coating saturation. In this work, mathematical models and computational simulations were employed to investigate the effect of binding components present in complex samples on the recovery of small molecules varying in logP for extractions carried out using the direct immersion approach. The presented findings corroborate that the studied approach indeed enables the extraction of both polar and nonpolar analytes from complex matrices, provided a suitable sorbent is employed. Further results indicated that, in certain cases, the kinetics of extraction of a given analyte in its free form might be dependent on the desorption kinetics of their bound form from matrix components, which might lower total recoveries of analytes with high affinity for the matrix. However, the binding of analytes to matrix components also enables SPME to extract a balanced quantity of different logP analytes, facilitated by multiphase equilibria, with a single extraction device.

Initial Investigation of Waste Feed Delivery Tank Mixing and Sampling Issues

International Nuclear Information System (INIS)

Fort, James A.; Bamberger, Judith A.; Meyer, Perry A.; Stewart, Charles W.

2007-01-01

The Hanford tank farms contractor will deliver waste to the Waste Treatment Plant (WTP) from a staging double-shell tank. The WTP broadly classifies waste it receives in terms of 'Envelopes,' each with different limiting properties and composition ranges. Envelope A, B, and C wastes are liquids that can include up to 4% entrained solids that can be pumped directly from the staging DST without mixing. Envelope D waste contains insoluble solids and must be mixed before transfer. The mixing and sampling issues lie within Envelope D solid-liquid slurries. The question is how effectively these slurries are mixed and how representative the grab samples are that are taken immediately after mixing. This report summarizes the current state of knowledge concerning jet mixing of wastes in underground storage tanks. Waste feed sampling requirements are listed, and their apparent assumption of uniformity by lack of a requirement for sample representativeness is cited as a significant issue. The case is made that there is not an adequate technical basis to provide such a sampling regimen because not enough is known about what can be achieved in mixing and distribution of solids by use of the baseline submersible mixing pump system. A combined mixing-sampling test program is recommended to fill this gap. Historical Pacific Northwest National Laboratory project and tank farms contractor documents are used to make this case. A substantial investment and progress are being made to understand mixing issues at the WTP. A summary of the key WTP activities relevant to this project is presented in this report. The relevant aspects of the WTP mixing work, together with a previously developed scaled test strategy for determining solids suspension with submerged mixer pumps (discussed in Section 3) provide a solid foundation for developing a path forward

Gas chromatographic determination of 1,1-dimethylhydrazine in water samples by solid-phase microextraction with derivatization

Directory of Open Access Journals (Sweden)

Madi Abilev

2014-10-01

Full Text Available 1,1-Dimethylhydrazine (1,1-DMH used as a rocket fuel component is highly reactive and unstable compound. It greatly complicates its accurate and express determination in environmental samples. Goal of this work was to develop a method for its express determination in water samples based on solid-phase microextraction with preliminary derivatization. Acetone was selected as reagent for derivatization because during its reaction with 1,1-DMH, volatile and hydrophobic acetone dimethylhydrazone (ADMH was formed. It was established that fiber based on 100-micron polydimethylsiloxane provides the most efficient extraction of ADMH from water at extraction time 2 min. Optimal concentration of acetone was 30 mg/mL. The minimum time for reaction of 1,1-DMH with acetone is 10 minutes. Addition of acids and alkali reduced ADMH response that may be caused by degradation of 1,1-DMH and reduction of derivatization rate. Addition of salt allowed to increase the response of ADMH however made impossible the quantitative determination of 1,1-DMH. Dependence of ADMH response on the concentration of 1,1-DMH at optimized parameters is linear in the concentrations range of 0.1-100 mg/L and can be used for quantitative determination of 1,1-DMH in water. Detection limit of the developed method is 0.02 mg/L. Reproducibility index of the method in the whole range of concentrations did not exceed 7%, accuracy index - 15%. Developed method is simple, inexpensive, accurate, automated and can be recommended for implementation in laboratories conducting environmental monitoring in areas of rocket-carriers fall.

In-situ transmission electron microscopy of the solid-phase epitaxial growth of GaAs: sample preparation and artifact characterization

International Nuclear Information System (INIS)

Llewellyn, D.J.; Llewellyn, D.J.; Belay, K.B.; Ridgway, M.C.

1998-01-01

In-situ transmission electron microscopy (TEM) has been used to characterize the solid phase epitaxial growth of amorphized GaAs at a temperature of 260 deg C. To maximize heat transfer from the heated holder to the sample and minimize electron-irradiation induced artifacts, non-conventional methodologies were utilized for the preparation of cross-sectional samples. GaAs 3x1 mm rectangular wafers were cleaved then glued face-to-face to form a wafer stack size of 3x3 mm while maintaining the TEM region at the center. This stack was subsequently polished on the cross-section to a thickness of ∼ 200 μm. A 3 mm disc was then cut perpendicular to the cross-section using a Gatan ultrasonic cutter. The disc was polished then dimpled on both sides to a thickness of ∼ 15 μm. This was ion-beam milled at liquid nitrogen temperature to an electron-transparent layer. From a comparison of in-situ and ex-situ measurements of the recrystallization rate, the actual sample temperature during in-situ characterization was estimated to deviate by ≤ 20 deg C from that of the heated holder. The influence of electron-irradiation was found to be negligible by comparing the recrystallization rate and microstructure of irradiated and unirradiated regions of comparable thickness. Similarly, the influence of the 'thin-foil effect' was found to be negligible by comparing the recrystallization rate and microstructure of thick and thin regions, the former determined after the removal of the sample from the microscope and further ion-beam milling of tens of microns of material. In conclusion, the potential influence of artifacts during in-situ TEM can be minimized by the appropriate choice of sample preparation procedures. (authors)

Introduction of solid food to young infants.

Science.gov (United States)

Kuo, Alice A; Inkelas, Moira; Slusser, Wendelin M; Maidenberg, Molly; Halfon, Neal

2011-11-01

Timing of the first introduction of solid food during infancy may have potential effects on life-long health. To understand the characteristics that are associated with the timing of infants' initial exposure to solid foods. The 2000 National Survey of Early Childhood Health (NSECH) was a nationally representative telephone survey of 2,068 parents of children aged 4-35 months, which profiled content and quality of health care for young children. African-American and Latino families were over-sampled. Analyses in this report include bivariate tests and logistic regressions. 62% of parents reported introducing solids to their child between 4-6 months of age. African-American mothers (OR=0.5 [0.3, 0.9]), English-speaking Latino mothers (OR=0.4 [0.2, 0.7]), White mothers with more than high school education (OR=0.5 [0.2, 1.0]), and mothers who breastfed for 4 months or longer (OR=0.4 [0.3, 0.7]) were less likely to introduce solids early. Most parents (92%) of children 4-9 months of age reported that their pediatric provider had discussed introduction of solids with them since the child's birth, and provider discussion of feeding was not associated with the timing of introduction of solids. Although most parents recall discussing the introduction of solid foods with their child's physician, several subgroups of mothers introduce solid foods earlier than the AAP recommendation of 4-6 months. More effective discussion of solid food introduction linked to counseling and support of breastfeeding by the primary health care provider may reduce early introduction of solids.

Magnetic solid-phase extraction of five pyrethroids from environmental water samples followed by ultrafast liquid chromatography analysis.

Science.gov (United States)

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

2012-08-30

In this study, the polystyrene-coated magnetic nanoparticles (MNPs/PSt) were successfully prepared and characterized by Fourier transform infrared spectroscopy, transmission electron microscopy and vibrating sample magnetometry. The as-prepared MNPs/PSt were used as the adsorbent in magnetic solid phase extraction of five pyrethroids, including lambda-cyhalothrin, deltamethrin, esfenvalerate, permethrin, bifenthrin, in environmental water samples. The five pyrethroids were determined by ultra fast liquid chromatography-ultraviolet spectrometry. The influencing factors, including amount of MNPs/Pst, extraction time, pH value, type and volume of desorption solvent and desorption time, were examined and optimized. The extraction recoveries obtained with merely 50mg of MNPs/Pst were very satisfactory. The whole extraction process could be completed within 0.5h. The MNPs/PSt can be reused after an easy washing process. Thus, a simple, green, economical, time saving and effective method for pyrethroids analysis in environmental water samples was established. A high enrichment factor of 500 was achieved and the limits of detection for lambda-cyhalothrin, deltamethrin, esfenvalerate, permethrin, bifenthrin were 0.015±0.001 ng mL(-1), 0.012±0.001 ng mL(-1), 0.026±0.001 ng mL(-1), 0.020±0.001 ng mL(-1), 0.013±0.001 ng mL(-1), respectively. Recoveries obtained by analyzing spiked water samples at three concentration levels (0.100±0.001 ng mL(-1), 1.000±0.001 ng mL(-1), 10.000±0.001 ng mL(-1)) were between 78.97±8.38% and 96.05±8.38%. The standard curves for the five pyrethroids showed good linearity with the correlation coefficients in the range of 0.9994-0.9999. The intra-day and inter-day precision were satisfactory with the RSDs in the range of 2.05-5.52% and 2.73-8.38%, respectively. Copyright © 2012 Elsevier B.V. All rights reserved.

A new carbon-based magnetic material for the dispersive solid-phase extraction of UV filters from water samples before liquid chromatography-tandem mass spectrometry analysis.

Science.gov (United States)

Piovesana, Susy; Capriotti, Anna Laura; Cavaliere, Chiara; La Barbera, Giorgia; Samperi, Roberto; Zenezini Chiozzi, Riccardo; Laganà, Aldo

2017-07-01

Magnetic solid-phase extraction is one of the most promising new extraction methods for liquid samples before ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis. Several types of materials, including carbonaceous ones, have been prepared for this purpose. In this paper, for the first time, the preparation, characterization, and sorption capability of Fe 3 O 4 -graphitized carbon black (mGCB) composite toward some compounds of environmental interest were investigated. The synthesized mGCB consisted of micrometric GCB particles with 55 m 2  g -1 surface area bearing some carbonyl and hydroxyl functionalities and the surface partially decorated by Fe 3 O 4 microparticles. The prepared mGCB was firstly tested as an adsorbent for the extraction from surface water of 50 pollutants, including estrogens, perfluoroalkyl compounds, UV filters, and quinolones. The material showed good affinity to many of the tested compounds, except carboxylates and glucoronates; however, some compounds were difficult to desorb. Ten UV filters belonging to the chemical classes of benzophenones and p-aminobenzoates were selected, and parameters were optimized for the extraction of these compounds from surface water before UHPLC-MS/MS determination. Then, the method was validated in terms of linearity, trueness, intra-laboratory precision, and detection and quantification limits. In summary, the method performance (trueness, expressed as analytical recovery, 85-114%; RSD 5-15%) appears suitable for the determination of the selected compounds at the level of 10-100 ng L -1 , with detection limits in the range of 1-5 ng L -1 . Finally, the new method was compared with a published one, based on conventional solid-phase extraction with GCB, showing similar performance in real sample analysis. Graphical Abstract Workflow of the analytical method based on magnetic solid-phase extraction followed by LC-MS/MS determination.

Environmental pollution from solid wastes

International Nuclear Information System (INIS)

Jervis, R.E.; Krishnan, S.S.; Accetone, P.; Arifin, N.; Ko, M.M.C.; Nhan, C.; Nguyen, L.; Vela, L.; Yee, T.

1992-01-01

Research completed under the CRP during the past two years has encompassed several related aspects of environmental problems associated with solid wastes: assessment of major sources of toxic elements in a variety of solid waste forms, their leachability by simulated groundwater or rain/acid rain and the determination of the contribution of hospital incinerator to atmospheric releases. The summary of the findings of these investigations are given in this report. Unexpected high levels of cadmium have been found in many solid wastes. Leaching tests indicate that, in some cases, over 70% of this can be leached out into the nearby waterways. Combustibility tests indicated that 35 to 45% of it is emitted to the atmosphere during burning. This explains the increased levels of cadmium in air particulates sampled downwind from waste incinerators. Plastic items in municipal and hospital wastes were particularly elevated in Cd, Cl, Cr, Ba and Zn. Up to 1300 μg/g of Cd was found in some domestic items. By inference, Pb also is found in some common plastics but the current studies did not permit Pb determination in solid wastes, but only in aerosols. (author). 8 tabs

Comet coma sample return instrument

Science.gov (United States)

Albee, A. L.; Brownlee, Don E.; Burnett, Donald S.; Tsou, Peter; Uesugi, K. T.

1994-01-01

The sample collection technology and instrument concept for the Sample of Comet Coma Earth Return Mission (SOCCER) are described. The scientific goals of this Flyby Sample Return are to return to coma dust and volatile samples from a known comet source, which will permit accurate elemental and isotopic measurements for thousands of individual solid particles and volatiles, detailed analysis of the dust structure, morphology, and mineralogy of the intact samples, and identification of the biogenic elements or compounds in the solid and volatile samples. Having these intact samples, morphologic, petrographic, and phase structural features can be determined. Information on dust particle size, shape, and density can be ascertained by analyzing penetration holes and tracks in the capture medium. Time and spatial data of dust capture will provide understanding of the flux dynamics of the coma and the jets. Additional information will include the identification of cosmic ray tracks in the cometary grains, which can provide a particle's process history and perhaps even the age of the comet. The measurements will be made with the same equipment used for studying micrometeorites for decades past; hence, the results can be directly compared without extrapolation or modification. The data will provide a powerful and direct technique for comparing the cometary samples with all known types of meteorites and interplanetary dust. This sample collection system will provide the first sample return from a specifically identified primitive body and will allow, for the first time, a direct method of matching meteoritic materials captured on Earth with known parent bodies.

Municipal solid waste composition determination supporting the integrated solid waste management system in the island of Crete

International Nuclear Information System (INIS)

Gidarakos, E.; Havas, G.; Ntzamilis, P.

2006-01-01

A one-year survey was conducted in the greater region of Crete (located at the lower region of the Aegean Sea) for the purpose of identifying waste composition (including chemical and physical characterization), as well as any seasonal variation. The investigation was carried out repeatedly at seven landfills and one transfer station in Crete, in four phases. Each sampling phase corresponded to a season (autumn, winter, spring, summer). ASTM D5231-92(2003) standard method and RCRA Waste Sampling Draft Technical Guidance were used. Hand sorting was used for classifying the collected wastes into the following categories: plastics, paper, metals, aluminium, leather-wood-textiles-rubbers, organic wastes, non-combustibles and miscellaneous. Further analysis included proximate and ultimate analysis of combustible materials. Metals such as lead, cadmium and mercury were also investigated. The results show that there has been a significant decrease of organic wastes during the last decade due to the increase of packaging materials, as a result of a change in consumption patterns. Three main waste categories were determined: organic wastes, paper and plastics, which combined represent 76% of the total waste in Crete. Furthermore, a high fraction of glass and a seasonal variation of aluminium indicate a strong correlation of waste composition with certain human activities, such as tourism. There is also a variation between the municipal solid waste (MSW) composition in the region of Crete (2003-2004) and MSW composition suggested in the National Solid Waste Planning (2000) [National Solid Waste Planning, 2000. Completion and particularization of Common Ministerial Act 113944//1944/1997: National Solid Waste Planning, June 2000]. The results of this survey are to be utilized by the regional solid waste authorities in order to establish an integrated waste treatment site, capable of fulfilling the regional waste management demands

Municipal solid waste composition determination supporting the integrated solid waste management system in the island of Crete.

Science.gov (United States)

Gidarakos, E; Havas, G; Ntzamilis, P

2006-01-01

A one-year survey was conducted in the greater region of Crete (located at the lower region of the Aegean Sea) for the purpose of identifying waste composition (including chemical and physical characterization), as well as any seasonal variation. The investigation was carried out repeatedly at seven landfills and one transfer station in Crete, in four phases. Each sampling phase corresponded to a season (autumn, winter, spring, summer). ASTM D5231-92(2003) standard method and RCRA Waste Sampling Draft Technical Guidance were used. Hand sorting was used for classifying the collected wastes into the following categories: plastics, paper, metals, aluminium, leather-wood-textiles-rubbers, organic wastes, non-combustibles and miscellaneous. Further analysis included proximate and ultimate analysis of combustible materials. Metals such as lead, cadmium and mercury were also investigated. The results show that there has been a significant decrease of organic wastes during the last decade due to the increase of packaging materials, as a result of a change in consumption patterns. Three main waste categories were determined: organic wastes, paper and plastics, which combined represent 76% of the total waste in Crete. Furthermore, a high fraction of glass and a seasonal variation of aluminium indicate a strong correlation of waste composition with certain human activities, such as tourism. There is also a variation between the municipal solid waste (MSW) composition in the region of Crete (2003-2004) and MSW composition suggested in the National Solid Waste Planning (2000) [National Solid Waste Planning, 2000. Completion and particularization of Common Ministerial Act 113944//1944/1997: National Solid Waste Planning, June 2000]. The results of this survey are to be utilized by the regional solid waste authorities in order to establish an integrated waste treatment site, capable of fulfilling the regional waste management demands.

Automated methods for thorium determination in liquids, solids and aerosols

International Nuclear Information System (INIS)

Robertson, R.; Stuart, J.E.

1984-01-01

Methodology for determining trace thorium levels in a variety of sample types for compliance purposes was developed. Thorium in filtered water samples is concentrated by ferric hydroxide co-precipitation. Aerosols on glass-fibre, cellulose ester or teflon filters are acid digested and thorium is concentrated by lanthanum fluoride co-precipitation. Chemical separation and measurement are then done on a Technicon AAII-C auto-analyzer via TTA-solvent extraction and colorimetry using the thorium-arsenazo III colour complex. Solid samples are acid digested and thorium is concentrated and separated using lanthanum fluoride co-precipitation followed by anion-exchange chromatography. Measurement is then carried out on the autoanalyzer by direct development of the thorium-arsenazo III colour complex. Chemical yields are determined through the addition of thorium-234 tracer with assay by gamma-ray spectrometry. The sensitivities of the methods for liquids, aerosols and solids are approximately 1μg/L,0.5μg and 0.5 μg/g respectively. At thorium levels about ten times the detection limits, accuracy and reproducibility are typically +-10 percent for liquids and aerosols and +- 15 percent for solid samples

Microextraction by Packed Sorbent (MEPS and Solid-Phase Microextraction (SPME as Sample Preparation Procedures for the Metabolomic Profiling of Urine

Directory of Open Access Journals (Sweden)

Catarina Silva

2014-01-01

Full Text Available For a long time, sample preparation was unrecognized as a critical issue in the analytical methodology, thus limiting the performance that could be achieved. However, the improvement of microextraction techniques, particularly microextraction by packed sorbent (MEPS and solid-phase microextraction (SPME, completely modified this scenario by introducing unprecedented control over this process. Urine is a biological fluid that is very interesting for metabolomics studies, allowing human health and disease characterization in a minimally invasive form. In this manuscript, we will critically review the most relevant and promising works in this field, highlighting how the metabolomic profiling of urine can be an extremely valuable tool for the early diagnosis of highly prevalent diseases, such as cardiovascular, oncologic and neurodegenerative ones.

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.

Strontium mono-chloride — A new molecule for the determination of chlorine using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

Energy Technology Data Exchange (ETDEWEB)

Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Welz, Bernhard, E-mail: w.bernardo@terra.com.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Lopez, Alfredo H.D.; Gois, Jefferson S. de; Caramori, Giovanni F. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Borges, Daniel L.G.; Carasek, Eduardo [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Andrade, Jailson B. de [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil)

2014-12-01

A new method has been developed for the determination of chlorine in biological reference materials using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) of the strontium mono-chloride (SrCl) molecule and direct solid sample analysis. The use of the SrCl molecule for high-temperature MAS was not described up to now in the literature. Preliminary time-dependent density functional theory calculations of the SrCl structure were carried out in order to obtain reasonable estimates of the absorption spectrum of the target molecule. The calculations, which were carried out at BHandHLyp/def2-QZVP level of theory, proved a very accurate and inexpensive way to get information about the spectrum of the SrCl molecule, which enabled us to perform the Cl determination with good sensitivity and specificity. The molecular absorption of the SrCl molecule has been measured using the wavelength at 635.862 nm, and zirconium and palladium have been evaluated as the chemical modifiers in order to increase the sensitivity of the gaseous SrCl molecule generated in the graphite furnace. The pyrolysis and vaporization temperatures were 600 °C and 2300 °C, respectively. Accuracy and precision of the method have been evaluated using biological certified reference materials of both animal and plant origins, showing good agreement with the informed and certified values. Limit of detection and characteristic mass were 1.0 and 2.2 ng, respectively. The results found using HR-CS GF MAS were in agreement (95% confidence level) compared to those obtained by electrothermal vaporization-inductively coupled plasma mass spectrometry. - Highlights: • The spectrum of the SrCl molecule was calculated on a theoretical basis and found very close to the predicted wavelength. • It is the first time that the spectrum of the SrCl molecule is described and used analytically for the determination of Cl. • No spectral interferences were observed as the

Environment influence on the solidity of the adhesive joint

Directory of Open Access Journals (Sweden)

Vladimír Válek

2006-01-01

Full Text Available In this paper “Environment influence on the solidity of the adhesive joint” I have dealt with the utilization of the bonding metals and practising experimental laboratory tests of adhesive joints depending on different laboratory environments and anticorrosive protection of the samples.For this laboratory tests I have chosen a universal adhesive. It is a two-component epoxy adhesive with suitable conditions for bonding metals. The samples were made from steel and were produced by the standard ČSN EN 1465. After the bonding and the cure procedure the samples were exposed in H20 environment for exact intervals (parts of the samples were painted by anticorrosive painting. After the exposition I have examinated the solidity of the adhesive joint in shearing stress on the measuring instrument Zwick 050. The samples were compared with etalon that were exposed to no environment.Results of the particular measuring were described into the graphs and were recorded the break down maximum force. When the samples were broken down I have taken a photo of it, which is in the appendix.

Novel Palm Fatty Acid Functionalized Magnetite Nanoparticles for Magnetic Solid-Phase Extraction of Trace Polycyclic Aromatic Hydrocarbons from Environmental Samples.

Science.gov (United States)

Rozi, Siti Khalijah Mahmad; Nodeh, Hamid Rashidi; Kamboh, Muhammad Afzal; Manan, Ninie Suhana Abdul; Mohamad, Sharifah

2017-07-01

A novel adsorbent, palm fatty acid coated magnetic Fe 3 O 4 nanoparticles (MNP-FA) was successfully synthesized with immobilization of the palm fatty acid onto the surface of MNPs. The successful synthesis of MNP-FA was further confirmed by X-Ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and Energy dispersive X-Ray spectroscopy (EDX) analyses and water contact angle (WCA) measurement. This newly synthesized MNP-FA was applied as magnetic solid phase extraction (MSPE) adsorbent for the enrichment of polycyclic aromatic hydrocarbons (PAHs), namely fluoranthene (FLT), pyrene (Pyr), chrysene (Cry) and benzo(a)pyrene (BaP) from environmental samples prior to High Performance Liquid Chromatography- Diode Array Detector (HPLC-DAD) analysis. The MSPE method was optimized by several parameters such as amount of sorbent, desorption solvent, volume of desorption solvent, extraction time, desorption time, pH and sample volume. Under the optimized conditions, MSPE method provided a low detection limit (LOD) for FLT, Pyr, Cry and BaP in the range of 0.01-0.05 ng mL -1 . The PAHs recoveries of the spiked leachate samples ranged from 98.5% to 113.8% with the RSDs (n = 5) ranging from 3.5% to 12.2%, while for the spiked sludge samples, the recoveries ranged from 81.1% to 119.3% with the RSDs (n = 5) ranging from 3.1% to 13.6%. The recyclability study revealed that MNP-FA has excellent reusability up to five times. Chromatrographic analysis demonstrated the suitability of MNP-FA as MSPE adsorbent for the efficient extraction of PAHs from environmental samples.

Influence of foaming agents on solid thermal conductivity of foam glasses prepared from CRT panel glass

DEFF Research Database (Denmark)

Østergaard, Martin Bonderup; Petersen, Rasmus Rosenlund; König, Jakob

2017-01-01

The understanding of the thermal transport mechanism of foam glass is still lacking. The contribution of solid- and gas conduction to the total thermal conductivity remains to be reported. In many foam glasses, the solid phase consist of a mix of an amorphous and a crystalline part where foaming...... containing glass and crystalline foaming agents and amorphous samples where the foaming agents are completely dissolved in the glass structure, respectively. Results show that the samples prepared by sintering have a higher thermal conductivity than the samples prepared by melt-quenching. The thermal...... conductivities of the sintered and the melt-quenched samples represent an upper and lower limit of the solid phase thermal conductivity of foam glasses prepared with these foaming agents. The content of foaming agents dissolved in the glass structure has a major impact on the solid thermal conductivity of foam...

Development of a solid-phase microextraction-based method for sampling of persistent chlorinated hydrocarbons in an urbanized coastal environment.

Science.gov (United States)

Zeng, Eddy Y; Tsukada, David; Diehl, Dario W

2004-11-01

Solid-phase microextraction (SPME) has been used as an in situ sampling technique for a wide range of volatile organic chemicals, but SPME field sampling of nonvolatile organic pollutants has not been reported. This paper describes the development of an SPME-based sampling method employing a poly(dimethylsiloxane) (PDMS)-coated (100-microm thickness) fiber as the sorbent phase. The laboratory-calibrated PDMS-coated fibers were used to construct SPME samplers, and field tests were conducted at three coastal locations off southern California to determine the equilibrium sampling time and compare the efficacy of the SPME samplers with that of an Infiltrex 100 water pumping system (Axys Environmental Systems Ltd., Sidney, British Columbia, Canada). p,p'-DDE and o,p'-DDE were the components consistently detected in the SPME samples among 42 polychlorinated biphenyl congeners and 17 chlorinated pesticidestargeted. SPME samplers deployed attwo locations with moderate and high levels of contamination for 18 and 30 d, respectively, attained statistically identical concentrations of p,p'-DDE and o,p'-DDE. In addition, SPME samplers deployed for 23 and 43 d, respectively, at a location of low contamination also contained statistically identical concentrations of p,p'-DDE. These results indicate that equilibrium could be reached within 18 to 23 d. The concentrations of p,p'-DDE, o,p'-DDE, or p,p'-DDD obtained with the SPME samplers and the Infiltrex 100 system were virtually identical. In particular, two water column concentration profiles of p,p'-DDE and o,p'-DDE acquired by the SPME samplers at a highly contaminated site on the Palos Verdes Shelf overlapped with the profiles obtained by the Infiltrex 100 system in 1997. The field tests not only reveal the advantages of the SPME samplers compared to the Infiltrex 100 system and other integrative passive devices but also indicate the need to improve the sensitivity of the SPME-based sampling technique.

Acquisition of reproducible transmission near-infrared (NIR) spectra of solid samples with inconsistent shapes by irradiation with isotropically diffused radiation using polytetrafluoroethylene (PTFE) beads.

Science.gov (United States)

Lee, Jinah; Duy, Pham Khac; Yoon, Jihye; Chung, Hoeil

2014-06-21

A bead-incorporated transmission scheme (BITS) has been demonstrated for collecting reproducible transmission near-infrared (NIR) spectra of samples with inconsistent shapes. Isotropically diffused NIR radiation was applied around a sample and the surrounding radiation was allowed to interact homogeneously with the sample for transmission measurement. Samples were packed in 1.40 mm polytetrafluoroethylene (PTFE) beads, ideal diffusers without NIR absorption, and then transmission spectra were collected by illuminating the sample-containing beads using NIR radiation. When collimated radiation was directly applied, a small portion of the non-fully diffused radiation (NFDR) propagated through the void space of the packing and eventually degraded the reproducibility. Pre-diffused radiation was introduced by placing an additional PTFE disk in front of the packing to diminish NFDR, which produced more reproducible spectral features. The proposed scheme was evaluated by analyzing two different solid samples: density determination for individual polyethylene (PE) pellets and identification of mining locality for tourmalines. Because spectral collection was reproducible, the use of the spectrum acquired from one PE pellet was sufficient to accurately determine the density of nine other pellets with different shapes. The differentiation of tourmalines, which are even more dissimilar in appearance, according to their mining locality was also feasible with the help of the scheme.

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.)

Rapid estimate of solid volume in large tuff cores using a gas pycnometer

International Nuclear Information System (INIS)

Thies, C.; Geddis, A.M.; Guzman, A.G.

1996-09-01

A thermally insulated, rigid-volume gas pycnometer system has been developed. The pycnometer chambers have been machined from solid PVC cylinders. Two chambers confine dry high-purity helium at different pressures. A thick-walled design ensures minimal heat exchange with the surrounding environment and a constant volume system, while expansion takes place between the chambers. The internal energy of the gas is assumed constant over the expansion. The ideal gas law is used to estimate the volume of solid material sealed in one of the chambers. Temperature is monitored continuously and incorporated into the calculation of solid volume. Temperature variation between measurements is less than 0.1 degrees C. The data are used to compute grain density for oven-dried Apache Leap tuff core samples. The measured volume of solid and the sample bulk volume are used to estimate porosity and bulk density. Intrinsic permeability was estimated from the porosity and measured pore surface area and is compared to in-situ measurements by the air permeability method. The gas pycnometer accommodates large core samples (0.25 m length x 0.11 m diameter) and can measure solid volume greater than 2.20 cm 3 with less than 1% error

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

International Nuclear Information System (INIS)

Nischkauer, Winfried; Herincs, Esther; Puschenreiter, Markus; Wenzel, Walter; Limbeck, Andreas

2013-01-01

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 −1 , 0.14 μg g −1 and 0.13 μg g −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 investigated

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

Sampling and sample preparation methods for the analysis of trace elements in biological material

International Nuclear Information System (INIS)

Sansoni, B.; Iyengar, V.

1978-05-01

The authors attempt to give a most systamtic possible treatment of the sample taking and sample preparation of biological material (particularly in human medicine) for trace analysis (e.g. neutron activation analysis, atomic absorption spectrometry). Contamination and loss problems are discussed as well as the manifold problems of the different consistency of solid and liquid biological materials, as well as the stabilization of the sample material. The process of dry and wet ashing is particularly dealt with, where new methods are also described. (RB) [de

Investigating the effect of moisture protection on solid-state stability and dissolution of fenofibrate and ketoconazole solid dispersions using PXRD, HSDSC and Raman microscopy.

Science.gov (United States)

Kanaujia, Parijat; Lau, Grace; Ng, Wai Kiong; Widjaja, Effendi; Schreyer, Martin; Hanefeld, Andrea; Fischbach, Matthias; Saal, Christoph; Maio, Mario; Tan, Reginald B H

2011-09-01

Enhanced dissolution of poorly soluble active pharmaceutical ingredients (APIs) in amorphous solid dispersions often diminishes during storage due to moisture-induced re-crystallization. This study aims to investigate the influence of moisture protection on solid-state stability and dissolution profiles of melt-extruded fenofibrate (FF) and ketoconazole (KC) solid dispersions. Samples were kept in open, closed and Activ-vials(®) to control the moisture uptake under accelerated conditions. During 13-week storage, changes in API crystallinity were quantified using powder X-ray diffraction (PXRD) (Rietveld analysis) and high sensitivity differential scanning calorimetry (HSDSC) and compared with any change in dissolution profiles. Trace crystallinity was observed by Raman microscopy, which otherwise was undetected by PXRD and HSDSC. Results showed that while moisture protection was ineffective in preventing the re-crystallization of amorphous FF, KC remained X-ray amorphous despite 5% moisture uptake. Regardless of the degree of crystallinity increase in FF, the enhanced dissolution properties were similarly diminished. Moisture uptake above 10% in KC samples also led to re-crystallization and significant decrease in dissolution rates. In conclusion, eliminating moisture sorption may not be sufficient in ensuring the stability of solid dispersions. Analytical quantification of API crystallinity is crucial in detecting subtle increase in crystallinity that can diminish the enhanced dissolution properties of solid dispersions.

Natural Arsenic Pollution and Hydrochemistry of Drinking Water of an Urban Part of Iran

OpenAIRE

Mohammad Mosaferi; Mohammad Shakerkhatibi; Saeid Dastgiri; Mohammad Asghari Jafar-abadi; Alireza Khataee; Samira Sheykholeslami

2014-01-01

Natural contamination of surface and groundwater resources with arsenic is a worldwide problem. The present study aimed to investigate and report on the quality of drinking water resources with special focus on arsenic presence in an urban part of Iran. Arsenic concentrations were measured by graphite furnace atomic absorption spectroscopy (GFAAS). In both surface and groundwater samples, arsenic concentrations ranged from 6 - 61 µg/L with an average value of 39 ± 20 µg/L. Concentration of ar...

Preconcentration and determination of boron in milk, infant formula, and honey samples by solid phase extraction-electrothermal atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Lopez-Garcia, I.; Vinas, P.; Romero-Romero, R. [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia (Spain); Hernandez-Cordoba, M. [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia (Spain)], E-mail: hcordoba@um.es

2009-02-15

This work presents alternative procedures for the electrothermal atomic absorption spectrometric determination of boron in milk, infant formulas, and honey samples. Honey samples (10% m/v) were diluted in a medium containing 1% v/v HNO{sub 3} and 50% v/v H{sub 2}O{sub 2} and introduced in the atomizer. A mixture of 20 {mu}g Pd and 0.5 {mu}g Mg was used for chemical modification. Calibration was carried out using aqueous solutions prepared in the same medium, in the presence of 10% m/v sucrose. The detection limit was 2 {mu}g g{sup -1}, equivalent to three times the standard error of the estimate (s{sub y/x}) of the regression line. For both infant formulas and milk samples, due to their very low boron content, we used a procedure based on preconcentration by solid phase extraction (Amberlite IRA 743), followed by elution with 2 mol L{sup -1} hydrochloric acid. Detection limits were 0.03 {mu}g g{sup -1} for 4% m/v honey, 0.04 {mu}g g{sup -1} for 5% m/v infant formula and 0.08 {mu}g mL{sup -1} for 15% v/v cow milk. We confirmed the accuracy of the procedure by comparing the obtained results with those found via a comparable independent procedure, as well by the analysis of four certified reference materials.

Recent developments and future trends in solid phase microextraction techniques towards green analytical chemistry.

Science.gov (United States)

Spietelun, Agata; Marcinkowski, Łukasz; de la Guardia, Miguel; Namieśnik, Jacek

2013-12-20

Solid phase microextraction find increasing applications in the sample preparation step before chromatographic determination of analytes in samples with a complex composition. These techniques allow for integrating several operations, such as sample collection, extraction, analyte enrichment above the detection limit of a given measuring instrument and the isolation of analytes from sample matrix. In this work the information about novel methodological and instrumental solutions in relation to different variants of solid phase extraction techniques, solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE) and magnetic solid phase extraction (MSPE) is presented, including practical applications of these techniques and a critical discussion about their advantages and disadvantages. The proposed solutions fulfill the requirements resulting from the concept of sustainable development, and specifically from the implementation of green chemistry principles in analytical laboratories. Therefore, particular attention was paid to the description of possible uses of novel, selective stationary phases in extraction techniques, inter alia, polymeric ionic liquids, carbon nanotubes, and silica- and carbon-based sorbents. The methodological solutions, together with properly matched sampling devices for collecting analytes from samples with varying matrix composition, enable us to reduce the number of errors during the sample preparation prior to chromatographic analysis as well as to limit the negative impact of this analytical step on the natural environment and the health of laboratory employees. Copyright © 2013 Elsevier B.V. All rights reserved.

Phase transitions of amorphous solid acetone in confined geometry investigated by reflection absorption infrared spectroscopy.

Science.gov (United States)

Shin, Sunghwan; Kang, Hani; Kim, Jun Soo; Kang, Heon

2014-11-26

We investigated the phase transformations of amorphous solid acetone under confined geometry by preparing acetone films trapped in amorphous solid water (ASW) or CCl4. Reflection absorption infrared spectroscopy (RAIRS) and temperature-programmed desorption (TPD) were used to monitor the phase changes of the acetone sample with increasing temperature. An acetone film trapped in ASW shows an abrupt change in the RAIRS features of the acetone vibrational bands during heating from 80 to 100 K, which indicates the transformation of amorphous solid acetone to a molecularly aligned crystalline phase. Further heating of the sample to 140 K produces an isotropic solid phase, and eventually a fluid phase near 157 K, at which the acetone sample is probably trapped in a pressurized, superheated condition inside the ASW matrix. Inside a CCl4 matrix, amorphous solid acetone crystallizes into a different, isotropic structure at ca. 90 K. We propose that the molecularly aligned crystalline phase formed in ASW is created by heterogeneous nucleation at the acetone-water interface, with resultant crystal growth, whereas the isotropic crystalline phase in CCl4 is formed by homogeneous crystal growth starting from the bulk region of the acetone sample.

The impact of municipal solid waste disposal in Ado- Ekiti metropolis ...

African Journals Online (AJOL)

hope&shola

Soil samples from four public waste dump sites (three samples from each location at 10 m interval) and plant sample ... Solid wastes other than hazardous and radioactive material are ... Copper, for example is a micro element, it is a necessary.

Towards an accurate and precise determination of the solid-solid transition temperature of enantiotropic systems

Energy Technology Data Exchange (ETDEWEB)

Herman, Christelle, E-mail: christelle.herman@ulb.ac.b [Universite Libre de Bruxelles, Transfers, Interfaces and Processes Department, Chemical Engineering Unit, 50 Avenue Franklin D-Roosevelt, CP 165/67, 1050 Bruxelles (Belgium); Leyssens, Tom [Universite Catholique de Louvain, Institute of Condensed Matter and Nanosciences, 1 Place Louis Pasteur, 1348 Louvain-La-Neuve (Belgium); Vermylen, Valerie [UCB Pharma, 60 Allee de la Recherche, 1070 Braine l' Alleud (Belgium); Halloin, Veronique; Haut, Benoit [Universite Libre de Bruxelles, Transfers, Interfaces and Processes Department, Chemical Engineering Unit, 50 Avenue Franklin D-Roosevelt, CP 165/67, 1050 Bruxelles (Belgium)

2011-05-15

Research highlights: We test two methods to obtain the solid-solid transition temperature of Etiracetam system, showing two enantiotropically related polymorphs. The first method, based on a thermodynamic development, is sensitive to the correctness of the data required. The second method is an experimental study of the stability thermal range of each morph. We identify the nature of crystals in suspension at equilibrium through Raman analysis. The solid-solid transition temperature is found equal to 303.65 K {+-} 0.5 K. - Abstract: This paper presents two distinct methods for the determination of the solid-solid transition temperature (T{sub tr}) separating the temperature ranges of stability of two crystallographic forms, hereafter called morphs, of a same substance. The first method, based on thermodynamic calculations, consists in determining T{sub tr} as the temperature at which the Gibbs free energies of the two morphs are equal to each other. For this purpose, some thermodynamic characteristics of both morphs are required, such as the specific heat capacities, the melting temperatures and the melting enthalpies. These are obtained using the Differential Scanning Calorimetry (DSC). In the second method, T{sub tr} is determined directly by an experimental study of the temperature ranges of stability of each morph. The three main originalities of the method developed are (i) to prepare samples composed by an isomassic mixture of crystals of both morphs, (ii) to set them in a thermostated and agitated suspension, and (iii) to use an in situ Raman spectroscopic probe for the determination of the crystallographic form of the crystals in suspension at equilibrium. Both methods are applied to determine the solid-solid transition temperature of the enantiotropic system of Etiracetam, and both of its two crystallographic forms so far identified, named morph I and morph II. The first method is shown to be very sensitive to the experimental data obtained by DSC while

Towards an accurate and precise determination of the solid-solid transition temperature of enantiotropic systems

International Nuclear Information System (INIS)

Herman, Christelle; Leyssens, Tom; Vermylen, Valerie; Halloin, Veronique; Haut, Benoit

2011-01-01

Research highlights: → We test two methods to obtain the solid-solid transition temperature of Etiracetam system, showing two enantiotropically related polymorphs. → The first method, based on a thermodynamic development, is sensitive to the correctness of the data required. → The second method is an experimental study of the stability thermal range of each morph. → We identify the nature of crystals in suspension at equilibrium through Raman analysis. → The solid-solid transition temperature is found equal to 303.65 K ± 0.5 K. - Abstract: This paper presents two distinct methods for the determination of the solid-solid transition temperature (T tr ) separating the temperature ranges of stability of two crystallographic forms, hereafter called morphs, of a same substance. The first method, based on thermodynamic calculations, consists in determining T tr as the temperature at which the Gibbs free energies of the two morphs are equal to each other. For this purpose, some thermodynamic characteristics of both morphs are required, such as the specific heat capacities, the melting temperatures and the melting enthalpies. These are obtained using the Differential Scanning Calorimetry (DSC). In the second method, T tr is determined directly by an experimental study of the temperature ranges of stability of each morph. The three main originalities of the method developed are (i) to prepare samples composed by an isomassic mixture of crystals of both morphs, (ii) to set them in a thermostated and agitated suspension, and (iii) to use an in situ Raman spectroscopic probe for the determination of the crystallographic form of the crystals in suspension at equilibrium. Both methods are applied to determine the solid-solid transition temperature of the enantiotropic system of Etiracetam, and both of its two crystallographic forms so far identified, named morph I and morph II. The first method is shown to be very sensitive to the experimental data obtained by DSC

Direct determination of Cu, Mn, Pb, and Zn in beer by thermospray flame furnace atomic absorption spectrometry

International Nuclear Information System (INIS)

Nascentes, Clesia C.; Kamogawa, Marcos Y.; Fernandes, Kelly G.; Arruda, Marco A.Z.; Nogueira, Ana Rita A.; Nobrega, Joaquim A.

2005-01-01

In this work, thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) was employed for Cu, Mn, Pb, and Zn determination in beer without any sample digestion. The system was optimized and calibration was based on the analyte addition technique. A sample volume of 300 μl was introduced into the hot Ni tube at a flow-rate of 0.4 ml min -1 using 0.14 mol l -1 nitric acid solution or air as carrier. Different Brazilian beers were directly analyzed after ultrasonic degasification. Results were compared with those obtained by graphite furnace atomic absorption spectrometry (GFAAS). The detection limits obtained for Cu, Mn, Pb, and Zn in aqueous solution were 2.2, 18, 1.6, and 0.9 μg l -1 , respectively. The relative standard deviations varied from 2.7% to 7.3% (n=8) for solutions containing the analytes in the 25-50 μg l -1 range. The concentration ranges obtained for analytes in beer samples were: Cu: 38.0-155 μg l -1 ; Mn: 110-348 μg l -1 , Pb: 13.0-32.9 μg l -1 , and Zn: 52.7-226 μg l -1 . Results obtained by TS-FF-AAS and GFAAS were in agreement at a 95% confidence level. The proposed method is fast and simple, since sample digestion is not required and sensitivity can be improved without using expensive devices. The TS-FF-AAS presented suitable sensitivity for determination of Cu, Mn, Pb, and Zn in the quality control of a brewery

Highly selective solid phase extraction and preconcentration of Azathioprine with nano-sized imprinted polymer based on multivariate optimization and its trace determination in biological and pharmaceutical samples

Energy Technology Data Exchange (ETDEWEB)

Davarani, Saied Saeed Hosseiny, E-mail: ss-hosseiny@cc.sbu.ac.ir [Faculty of Chemistry, Shahid Beheshti University, G. C., P.O. Box 19839-4716, Tehran (Iran, Islamic Republic of); Rezayati zad, Zeinab [Faculty of Chemistry, Shahid Beheshti University, G. C., P.O. Box 19839-4716, Tehran (Iran, Islamic Republic of); Taheri, Ali Reza; Rahmatian, Nasrin [Islamic Azad University, Ilam Branch, Ilam (Iran, Islamic Republic of)

2017-02-01

In this research, for first time selective separation and determination of Azathioprine is demonstrated using molecularly imprinted polymer as the solid-phase extraction adsorbent, measured by spectrophotometry at λ{sub max} 286 nm. The selective molecularly imprinted polymer was produced using Azathioprine and methacrylic acid as a template molecule and monomer, respectively. A molecularly imprinted solid-phase extraction procedure was performed in column for the analyte from pharmaceutical and serum samples. The synthesized polymers were characterized by infrared spectroscopy (IR), field emission scanning electron microscopy (FESEM). In order to investigate the effect of independent variables on the extraction efficiency, the response surface methodology (RSM) based on Box–Behnken design (BBD) was employed. The analytical parameters such as precision, accuracy and linear working range were also determined in optimal experimental conditions and the proposed method was applied to analysis of Azathioprine. The linear dynamic range and limits of detection were 2.5–0.01 and 0.008 mg L{sup ‐1} respectively. The recoveries for analyte were higher than 95% and relative standard deviation values were found to be in the range of 0.83–4.15%. This method was successfully applied for the determination of Azathioprine in biological and pharmaceutical samples. - Graphical abstract: A new-nano sized imprinted polymer was synthesized and applied as sorbent in SPE in order to selective recognition, preconcentration, and determination of Azathioprine with the response surface methodology based on Box–Behnken design and was successfully investigated for the clean-up of human blood serum and pharmaceutical samples. - Highlights: • The nanosized-imprinted polymer has been synthesized by precipitation polymerization technique. • A molecularly imprinted solid-phase extraction procedure was performed for determination of Azathioprine. • The Azathioprine

Highly selective solid phase extraction and preconcentration of Azathioprine with nano-sized imprinted polymer based on multivariate optimization and its trace determination in biological and pharmaceutical samples

International Nuclear Information System (INIS)

Davarani, Saied Saeed Hosseiny; Rezayati zad, Zeinab; Taheri, Ali Reza; Rahmatian, Nasrin

2017-01-01

In this research, for first time selective separation and determination of Azathioprine is demonstrated using molecularly imprinted polymer as the solid-phase extraction adsorbent, measured by spectrophotometry at λ max 286 nm. The selective molecularly imprinted polymer was produced using Azathioprine and methacrylic acid as a template molecule and monomer, respectively. A molecularly imprinted solid-phase extraction procedure was performed in column for the analyte from pharmaceutical and serum samples. The synthesized polymers were characterized by infrared spectroscopy (IR), field emission scanning electron microscopy (FESEM). In order to investigate the effect of independent variables on the extraction efficiency, the response surface methodology (RSM) based on Box–Behnken design (BBD) was employed. The analytical parameters such as precision, accuracy and linear working range were also determined in optimal experimental conditions and the proposed method was applied to analysis of Azathioprine. The linear dynamic range and limits of detection were 2.5–0.01 and 0.008 mg L ‐1 respectively. The recoveries for analyte were higher than 95% and relative standard deviation values were found to be in the range of 0.83–4.15%. This method was successfully applied for the determination of Azathioprine in biological and pharmaceutical samples. - Graphical abstract: A new-nano sized imprinted polymer was synthesized and applied as sorbent in SPE in order to selective recognition, preconcentration, and determination of Azathioprine with the response surface methodology based on Box–Behnken design and was successfully investigated for the clean-up of human blood serum and pharmaceutical samples. - Highlights: • The nanosized-imprinted polymer has been synthesized by precipitation polymerization technique. • A molecularly imprinted solid-phase extraction procedure was performed for determination of Azathioprine. • The Azathioprine-molecular imprinting

Portable Solid Phase Micro-Extraction Coupled with Ion Mobility Spectrometry System for On-Site Analysis of Chemical Warfare Agents and Simulants in Water Samples

Science.gov (United States)

Yang, Liu; Han, Qiang; Cao, Shuya; Yang, Jie; Yang, Junchao; Ding, Mingyu

2014-01-01

On-site analysis is an efficient approach to facilitate analysis at the location of the system under investigation as it can result in more accurate, more precise and quickly available analytical data. In our work, a novel self-made thermal desorption based interface was fabricated to couple solid-phase microextraction with ion mobility spectrometry for on-site water analysis. The portable interface can be connected with the front-end of an ion mobility spectrometer directly without other modifications. The analytical performance was evaluated via the extraction of chemical warfare agents and simulants in water samples. Several parameters including ionic strength and extraction time have been investigated in detail. The application of the developed method afforded satisfactory recoveries ranging from 72.9% to 114.4% when applied to the analysis of real water samples. PMID:25384006

DNP-enhanced solid-state NMR spectroscopy of active pharmaceutical ingredients.

Science.gov (United States)

Zhao, Li; Pinon, Arthur C; Emsley, Lyndon; Rossini, Aaron J

2017-11-28

Solid-state NMR spectroscopy has become a valuable tool for the characterization of both pure and formulated active pharmaceutical ingredients (APIs). However, NMR generally suffers from poor sensitivity that often restricts NMR experiments to nuclei with favorable properties, concentrated samples, and acquisition of one-dimensional (1D) NMR spectra. Here, we review how dynamic nuclear polarization (DNP) can be applied to routinely enhance the sensitivity of solid-state NMR experiments by one to two orders of magnitude for both pure and formulated APIs. Sample preparation protocols for relayed DNP experiments and experiments on directly doped APIs are detailed. Numerical spin diffusion models illustrate the dependence of relayed DNP enhancements on the relaxation properties and particle size of the solids and can be used for particle size determination when the other factors are known. We then describe the advanced solid-state NMR experiments that have been enabled by DNP and how they provide unique insight into the molecular and macroscopic structure of APIs. For example, with large sensitivity gains provided by DNP, natural isotopic abundance, 13 C- 13 C double-quantum single-quantum homonuclear correlation NMR spectra of pure APIs can be routinely acquired. DNP also enables solid-state NMR experiments with unreceptive quadrupolar nuclei such as 2 H, 14 N, and 35 Cl that are commonly found in APIs. Applications of DNP-enhanced solid-state NMR spectroscopy for the molecular level characterization of low API load formulations such as commercial tablets and amorphous solid dispersions are described. Future perspectives for DNP-enhanced solid-state NMR experiments on APIs are briefly discussed. Copyright © 2017 John Wiley & Sons, Ltd.

Microwave assisted solid phase extraction for separation preconcentration sulfamethoxazole in wastewater using tyre based activated carbon as solid phase material prior to spectrophotometric determination

Science.gov (United States)

Mogolodi Dimpe, K.; Mpupa, Anele; Nomngongo, Philiswa N.

2018-01-01

This work was chiefly encouraged by the continuous consumption of antibiotics which eventually pose harmful effects on animals and human beings when present in water systems. In this study, the activated carbon (AC) was used as a solid phase material for the removal of sulfamethoxazole (SMX) in wastewater samples. The microwave assisted solid phase extraction (MASPE) as a sample extraction method was employed to better extract SMX in water samples and finally the analysis of SMX was done by the UV-Vis spectrophotometer. The microwave assisted solid phase extraction method was optimized using a two-level fractional factorial design by evaluating parameters such as pH, mass of adsorbent (MA), extraction time (ET), eluent ratio (ER) and microwave power (MP). Under optimized conditions, the limit of detection (LOD) and limit of quantification (LOQ) were 0.5 μg L- 1 and 1.7 μg L- 1, respectively, and intraday and interday precision expressed in terms of relative standard deviation were > 6%.The maximum adsorption capacity was 138 mg g- 1 for SMX and the adsorbent could be reused eight times. Lastly, the MASPE method was applied for the removal of SMX in wastewater samples collected from a domestic wastewater treatment plant (WWTP) and river water.

Ultra-sensitive speciation analysis of mercury by CE-ICP-MS together with field-amplified sample stacking injection and dispersive solid-phase extraction.

Science.gov (United States)

Chen, YiQuan; Cheng, Xian; Mo, Fan; Huang, LiMei; Wu, Zujian; Wu, Yongning; Xu, LiangJun; Fu, FengFu

2016-04-01

A simple dispersive solid-phase extraction (DSPE) used to extract and preconcentrate ultra-trace MeHg, EtHg and Hg(2+) from water sample, and a sensitive method for the simultaneous analysis of MeHg, EtHg and Hg(2+) by using capillary electrophoresis-inductively coupled plasma mass spectrometry (CE-ICP-MS) with field-amplified sample stacking injection (FASI) were first reported in this study. The DSPE used thiol cotton particles as adsorbent, and is simple and effective. It can be used to extract and preconcentrate ultra-trace mercury compounds in water samples within 30 min with a satisfied recovery and no mercury species alteration during the process. The FASI enhanced the sensitivity of CE-ICP-MS with 25-fold, 29-fold and 27-fold for MeHg, EtHg and Hg(2+) , respectively. Using FASI-CE-ICP-MS together with DSPE, we have successfully determined ultra-trace MeHg, EtHg and Hg(2+) in tap water with a limits of quantification (LOQs) of 0.26-0.45 pg/mL, an RSD (n = 3) mercury. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

SOLIDS PRECIPITATION EVENT IN MCU CAUSAL ANALYSIS AND RECOMMENDATIONS FROM SOLIDS RECOVERY TEAM

Energy Technology Data Exchange (ETDEWEB)

Garrison, A.; Aponte, C.

2014-08-15

A process upset occurred in the Modular Caustic-Side Solvent Extraction Unit (MCU) facility on April 6th, 2014. During recovery efforts, a significant amount of solids were found in the Salt Solution Feed Tank (SSFT), Salt Solution Receipt Tanks (SSRTs), two extraction contactors, and scrub contactors. The solids were identified by Savannah River National Laboratory (SRNL) as primarily sodium oxalate and sodium alumina silicate (NAS) with the presence of some aluminum hydroxide. NAS solids have been present in the SSFT since simulant runs during cold chemical startup of MCU in 2007, and have not hindered operations since that time. During the process upset in April 2014, the oxalate solids partially blocked the aqueous outlet of the extraction contactors, causing salt solution to exit through the contactor organic outlet to the scrub contactors with the organic phase. This salt solution overwhelmed the scrub contactors and passed with the organic phase to the strip section of MCU. The partially reversed flow of salt solution resulted in a Strip Effluent (SE) stream that was high in Isopar™ L, pH and sodium. The primary cause of the excessive solids accumulation in the SSRTs and SSFT at MCU is attributed to an increase in the frequency of oxalic acid cleaning of the 512-S primary filter. Agitation in the SSRTs at MCU in response to cold weather likely provided the primary mechanism to transfer the solids to the contactors. Sources of the sodium oxalate solids are attributed to the oxalic acid cleaning solution used to clean the primary filter at the Actinide Removal Process (ARP) filtration at 512-S, as well as precipitation from the salt batch feed, which is at or near oxalate saturation. The Solids Recovery Team was formed to determine the cause of the solids formation and develop recommendations to prevent or mitigate this event in the future. A total of 53 recommendations were generated. These recommendations were organized into 4 focus areas: • Improve

Drop-on-demand sample introduction system coupled with the flowing atmospheric-pressure afterglow for direct molecular analysis of complex liquid microvolume samples.

Science.gov (United States)

Schaper, J Niklas; Pfeuffer, Kevin P; Shelley, Jacob T; Bings, Nicolas H; Hieftje, Gary M

2012-11-06

One of the fastest developing fields in analytical spectrochemistry in recent years is ambient desorption/ionization mass spectrometry (ADI-MS). This burgeoning interest has been due to the demonstrated advantages of the method: simple mass spectra, little or no sample preparation, and applicability to samples in the solid, liquid, or gaseous state. One such ADI-MS source, the flowing atmospheric-pressure afterglow (FAPA), is capable of direct analysis of solids just by aiming the source at the solid surface and sampling the produced ions into a mass spectrometer. However, direct introduction of significant volumes of liquid samples into this source has not been possible, as solvent loads can quench the afterglow and, thus, the formation of reagent ions. As a result, the analysis of liquid samples is preferably carried out by analyzing dried residues or by desorbing small amounts of liquid samples directly from the liquid surface. In the former case, reproducibility of sample introduction is crucial if quantitative results are desired. In the present study, introduction of liquid samples as very small droplets helps overcome the issues of sample positioning and reduced levels of solvent intake. A recently developed "drop-on-demand" (DOD) aerosol generator is capable of reproducibly producing very small volumes of liquid (∼17 pL). In this paper, the coupling of FAPA-MS and DOD is reported and applications are suggested. Analytes representing different classes of substances were tested and limits of detections were determined. Matrix tolerance was investigated for drugs of abuse and their metabolites by analyzing raw urine samples and quantification without the use of internal standards. Limits of detection below 2 μg/mL, without sample pretreatment, were obtained.

Activated carbon modified with 4-(8-hydroxyquinoline-azo)benzamidine for selective solid-phase extraction and preconcentration of trace lead from environmental samples

International Nuclear Information System (INIS)

Tian, H.; Chang, X.; Hu, Z.; Yang, K.; He, Q.; Zhang, L.; Tu, Z.

2010-01-01

Activated carbon was chemically modified with 4-(8-hydroxyquinoline-azo)benzamidine and used for separation and preconcentration of trace amounts of Pb(II) in environmental samples by solid-phase extraction prior to the measurement by inductively coupled plasma atomic emission spectrometry. The effects of pH, shaking time, eluent concentration and volume, sample flow rate and potential interfering ions were studied. Under the optimum conditions, the enrichment factor was 100, the detection limits is 0. 43 ng mL -1 , and the relative standard deviations are <2. 1% (n = 8). The adsorption capacity of the sorbent is 53. 58 mg of lead(II) per gram of the material. The sorbent was successfully applied to the preconcentration of trace Pb(II) in the reference materials GBW 08301 (river sediment) and GBW 08302 (Tibet soil). The recovery of lead(II) from Yellow river water, Huangshui water, and tap water is in range of 99. 3-101. 6%. (author)

Towards sustainable solid waste management: Investigating household participation in solid waste management

Science.gov (United States)

Akil, A. M.; Ho, C. S.

2014-02-01

The aim of this paper is to assess the readiness of Iskandar Malaysia community to accept solid waste recycling. The research is based on quantitative research design and descriptive survey of the households at Iskandar Malaysia using the stratified sampling method for a sample of 670. The survey was conducted using a structured questionnaire that covered two basic principles; a) recycling knowledge; b) willingness to recycle. Data was analysed using the SPSS to carry out statistical analysis. The finding shows households' knowledge towards the solid waste recycling is good and positive. However, finding also shows that respondents have incomprehensive knowledge on the method of disposal as more than 50% of householders only recycle papers and textiles. Most of the households agreed to participate in the activities of the separation of waste if the facility will be made available at their kerbside. Therefore, it is recommended that government should provide more in-depth knowledge by intensifying the awareness of the households in the recycling programs. In term of urban planning and management, the location of recycling facility can be analysing by using GIS. This is important to understand the catchment area of each neighbourhood or precinct to ensure effective household participation.

Laser Tweezer Controlled Solid Immersion Lens for High Resolution Imaging in Microfluidic and Biological Samples

National Research Council Canada - National Science Library

Birkbeck, Aaron L; Zlatanovic, Sanja; Ozkan, Mihrimah; Esener, Sadik C

2005-01-01

...). Up to now, solid immersion lens imaging systems have relied upon cantilever-mounted SILs that are difficult to integrate into microfluidic systems and require an extra alignment step with external optics...

Novel polyamide-based nanofibers prepared by electrospinning technique for headspace solid-phase microextraction of phenol and chlorophenols from environmental samples

International Nuclear Information System (INIS)

Bagheri, Habib; Aghakhani, Ali; Baghernejad, Masoud; Akbarinejad, Alireza

2012-01-01

A novel solid phase microextraction (SPME) fiber was fabricated by electrospinning method in which a polymeric solution was converted to nanofibers using high voltages. A thin stainless steel wire was coated by the network of polymeric nanofibers. The polymeric nanofiber coating on the wire was mechanically stable due to the fine and continuous nanofibers formation around the wire with a three dimensional structure. Polyamide (nylon 6), due to its suitable characteristics was used to prepare the unbreakable SPME nanofiber. The scanning electron microscopy (SEM) images of this new coating showed a diameter range of 100–200 nm for polyamide nanofibers with a homogeneous and porous surface structure. The extraction efficiency of new coating was investigated for headspace solid-phase microextraction (HS-SPME) of some environmentally important chlorophenols from aqueous samples followed by gas chromatography–mass spectrometry (GC–MS) analysis. Effect of different parameters influencing the extraction efficiency including extraction temperature, extraction time, ionic strength and polyamide amount were investigated and optimized. In order to improve the chromatographic behavior of phenolic compounds, all the analytes were derivatized prior to the extraction process using basic acetic anhydride. The detection limits of the method under optimized conditions were in the range of 2–10 ng L −1 . The relative standard deviations (RSD) (n = 3) at the concentration level of 1.7–6.7 ng mL −1 were obtained between 1 and 7.4%. The calibration curves of chlorophenols showed linearity in the range of 27–1330 ng L −1 for phenol and monochlorophenols and 7–1000 ng L −1 for dichloro and trichlorophenols. Also, the proposed method was successfully applied to the extraction of phenol and chlorophenols from real water samples and relative recoveries were between 84 and 98% for all the selected analytes except for 2,4,6 tricholophenol which was between 72 and 74%.

Solid Phase Microextraction and Related Techniques for Drugs in Biological Samples

OpenAIRE

Moein, Mohammad Mahdi; Said, Rana; Bassyouni, Fatma; Abdel-Rehim, Mohamed

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 o...

Solid-phase reductive amination for glycomic analysis.

Science.gov (United States)

Jiang, Kuan; Zhu, He; Xiao, Cong; Liu, Ding; Edmunds, Garrett; Wen, Liuqing; Ma, Cheng; Li, Jing; Wang, Peng George

2017-04-15

Reductive amination is an indispensable method for glycomic analysis, as it tremendously facilitates glycan characterization and quantification by coupling functional tags at the reducing ends of glycans. However, traditional in-solution derivatization based approach for the preparation of reductively aminated glycans is quite tedious and time-consuming. Here, a simpler and more efficient strategy termed solid-phase reductive amination was investigated. The general concept underlying this new approach is to streamline glycan extraction, derivatization, and purification on non-porous graphitized carbon sorbents. Neutral and sialylated standard glycans were utilized to test the feasibility of the solid-phase method. As results, almost complete labeling of those glycans with four common labels of aniline, 2-aminobenzamide (2-AB), 2-aminobenzoic acid (2-AA) and 2-amino-N-(2-aminoethyl)-benzamide (AEAB) was obtained, and negligible desialylation occurred during sample preparation. The labeled glycans derived from glycoproteins showed excellent reproducibility in high performance liquid chromatography (HPLC) and matrix assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) analysis. Direct comparisons based on fluorescent absorbance and relative quantification using isotopic labeling demonstrated that the solid-phase strategy enabled 20-30% increase in sample recovery. In short, the solid-phase strategy is simple, reproducible, efficient, and sensitive for glycan analysis. This method was also successfully applied for N-glycan profiling of HEK 293 cells with MALDI-TOF MS, showing its attractive application in the high-throughput analysis of mammalian glycome. Published by Elsevier B.V.

Perturbation of nuclear spin polarizations in solid state NMR of nitroxide-doped samples by magic-angle spinning without microwaves

Energy Technology Data Exchange (ETDEWEB)

Thurber, Kent R., E-mail: thurberk@niddk.nih.gov; Tycko, Robert [Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases, National Institutes of Health, Bethesda, Maryland 20892-0520 (United States)

2014-05-14

We report solid state {sup 13}C and {sup 1}H nuclear magnetic resonance (NMR) experiments with magic-angle spinning (MAS) on frozen solutions containing nitroxide-based paramagnetic dopants that indicate significant perturbations of nuclear spin polarizations without microwave irradiation. At temperatures near 25 K, {sup 1}H and cross-polarized {sup 13}C NMR signals from {sup 15}N,{sup 13}C-labeled L-alanine in trinitroxide-doped glycerol/water are reduced by factors as large as six compared to signals from samples without nitroxide doping. Without MAS or at temperatures near 100 K, differences between signals with and without nitroxide doping are much smaller. We attribute most of the reduction of NMR signals under MAS near 25 K to nuclear spin depolarization through the cross-effect dynamic nuclear polarization mechanism, in which three-spin flips drive nuclear polarizations toward equilibrium with spin polarization differences between electron pairs. When T{sub 1e} is sufficiently long relative to the MAS rotation period, the distribution of electron spin polarization across the nitroxide electron paramagnetic resonance lineshape can be very different from the corresponding distribution in a static sample at thermal equilibrium, leading to the observed effects. We describe three-spin and 3000-spin calculations that qualitatively reproduce the experimental observations.

Perturbation of nuclear spin polarizations in solid state NMR of nitroxide-doped samples by magic-angle spinning without microwaves

International Nuclear Information System (INIS)

Thurber, Kent R.; Tycko, Robert

2014-01-01

We report solid state 13 C and 1 H nuclear magnetic resonance (NMR) experiments with magic-angle spinning (MAS) on frozen solutions containing nitroxide-based paramagnetic dopants that indicate significant perturbations of nuclear spin polarizations without microwave irradiation. At temperatures near 25 K, 1 H and cross-polarized 13 C NMR signals from 15 N, 13 C-labeled L-alanine in trinitroxide-doped glycerol/water are reduced by factors as large as six compared to signals from samples without nitroxide doping. Without MAS or at temperatures near 100 K, differences between signals with and without nitroxide doping are much smaller. We attribute most of the reduction of NMR signals under MAS near 25 K to nuclear spin depolarization through the cross-effect dynamic nuclear polarization mechanism, in which three-spin flips drive nuclear polarizations toward equilibrium with spin polarization differences between electron pairs. When T 1e is sufficiently long relative to the MAS rotation period, the distribution of electron spin polarization across the nitroxide electron paramagnetic resonance lineshape can be very different from the corresponding distribution in a static sample at thermal equilibrium, leading to the observed effects. We describe three-spin and 3000-spin calculations that qualitatively reproduce the experimental observations

Perturbation of nuclear spin polarizations in solid state NMR of nitroxide-doped samples by magic-angle spinning without microwaves.

Science.gov (United States)

Thurber, Kent R; Tycko, Robert

2014-05-14

We report solid state (13)C and (1)H nuclear magnetic resonance (NMR) experiments with magic-angle spinning (MAS) on frozen solutions containing nitroxide-based paramagnetic dopants that indicate significant perturbations of nuclear spin polarizations without microwave irradiation. At temperatures near 25 K, (1)H and cross-polarized (13)C NMR signals from (15)N,(13)C-labeled L-alanine in trinitroxide-doped glycerol/water are reduced by factors as large as six compared to signals from samples without nitroxide doping. Without MAS or at temperatures near 100 K, differences between signals with and without nitroxide doping are much smaller. We attribute most of the reduction of NMR signals under MAS near 25 K to nuclear spin depolarization through the cross-effect dynamic nuclear polarization mechanism, in which three-spin flips drive nuclear polarizations toward equilibrium with spin polarization differences between electron pairs. When T1e is sufficiently long relative to the MAS rotation period, the distribution of electron spin polarization across the nitroxide electron paramagnetic resonance lineshape can be very different from the corresponding distribution in a static sample at thermal equilibrium, leading to the observed effects. We describe three-spin and 3000-spin calculations that qualitatively reproduce the experimental observations.

Mass, energy and material balances of SRF production process. Part 3: solid recovered fuel produced from municipal solid waste.

Science.gov (United States)

Nasrullah, Muhammad; Vainikka, Pasi; Hannula, Janne; Hurme, Markku; Kärki, Janne

2015-02-01

This is the third and final part of the three-part article written to describe the mass, energy and material balances of the solid recovered fuel production process produced from various types of waste streams through mechanical treatment. This article focused the production of solid recovered fuel from municipal solid waste. The stream of municipal solid waste used here as an input waste material to produce solid recovered fuel is energy waste collected from households of municipality. This article presents the mass, energy and material balances of the solid recovered fuel production process. These balances are based on the proximate as well as the ultimate analysis and the composition determination of various streams of material produced in a solid recovered fuel production plant. All the process streams are sampled and treated according to CEN standard methods for solid recovered fuel. The results of the mass balance of the solid recovered fuel production process showed that 72% of the input waste material was recovered in the form of solid recovered fuel; 2.6% as ferrous metal, 0.4% as non-ferrous metal, 11% was sorted as rejects material, 12% as fine faction and 2% as heavy fraction. The energy balance of the solid recovered fuel production process showed that 86% of the total input energy content of input waste material was recovered in the form of solid recovered fuel. The remaining percentage (14%) of the input energy was split into the streams of reject material, fine fraction and heavy fraction. The material balances of this process showed that mass fraction of paper and cardboard, plastic (soft) and wood recovered in the solid recovered fuel stream was 88%, 85% and 90%, respectively, of their input mass. A high mass fraction of rubber material, plastic (PVC-plastic) and inert (stone/rock and glass particles) was found in the reject material stream. © The Author(s) 2014.