Applications of mass spectrometry in the trace element analysis of biological materials

International Nuclear Information System (INIS)

Moens, L.

1997-01-01

The importance of mass spectrometry for the analysis of biological material is illustrated by reviewing the different mass spectrometric methods applied and describing some typical applications published recently. Though atomic absorption spectrometry is used in the majority of analyses of biological material, most mass spectrometric methods have been used to some extent for trace element determination in biomedical research. The relative importance of the different methods is estimated by reviewing recent research papers. It is striking that especially inductively coupled plasma mass spectrometry is increasingly being applied, partly because the method can be used on-line after chromatographic separation, in speciation studies. Mass spectrometric methods prove to offer unique possibilities in stable isotope tracer studies and for this purpose also experimentally demanding methods such as thermal ionization mass spectrometry and accelerator mass spectrometry are frequently used. (orig.)

Fast sequential multi-element determination of major and minor elements in environmental samples and drinking waters by high-resolution continuum source flame atomic absorption spectrometry.

Science.gov (United States)

Gómez-Nieto, Beatriz; Gismera, Ma Jesús; Sevilla, Ma Teresa; Procopio, Jesús R

2015-01-07

The fast sequential multi-element determination of 11 elements present at different concentration levels in environmental samples and drinking waters has been investigated using high-resolution continuum source flame atomic absorption spectrometry. The main lines for Cu (324.754 nm), Zn (213.857 nm), Cd (228.802 nm), Ni (232.003 nm) and Pb (217.001 nm), main and secondary absorption lines for Mn (279.482 and 279.827 nm), Fe (248.327, 248.514 and 302.064 nm) and Ca (422.673 and 239.856 nm), secondary lines with different sensitivities for Na (589.592 and 330.237 nm) and K (769.897 and 404.414 nm) and a secondary line for Mg (202.582 nm) have been chosen to perform the analysis. A flow injection system has been used for sample introduction so sample consumption has been reduced up to less than 1 mL per element, measured in triplicate. Furthermore, the use of multiplets for Fe and the side pixel registration approach for Mg have been studied in order to reduce sensitivity and extend the linear working range. The figures of merit have been calculated and the proposed method was applied to determine these elements in a pine needles reference material (SRM 1575a), drinking and natural waters and soil extracts. Recoveries of analytes added at different concentration levels to water samples and extracts of soils were within 88-115% interval. In this way, the fast sequential multi-element determination of major and minor elements can be carried out, in triplicate, with successful results without requiring additional dilutions of samples or several different strategies for sample preparation using about 8-9 mL of sample. Copyright © 2014 Elsevier B.V. All rights reserved.

Application of dot matrix LCD in multi-element portable X-ray fluorescence spectrometry The LCD is stated for Liquid Crystal Display

CERN Document Server

Lin Yan Chang; Lai Wan Chang; Zhou Si Chun

2002-01-01

Dot matrix LCD based on T6963C is a low power supply module. It needs no complex interface circuits connecting with MCU. Application in text and graphics is easy. Application of this LCD in multi-element portable XRF spectrometry is show. How to use it in Chinese, pull-down menu, spectrum and how to design the interface circuits with embedded computer are shown as well

Validation of multi-element isotope dilution ICPMS for the analysis of basalts

Energy Technology Data Exchange (ETDEWEB)

Willbold, M.; Jochum, K.P.; Raczek, I.; Amini, M.A.; Stoll, B.; Hofmann, A.W. [Max-Planck-Institut fuer Chemie, Mainz (Germany)

2003-09-01

In this study we have validated a newly developed multi-element isotope dilution (ID) ICPMS method for the simultaneous analysis of up to 12 trace elements in geological samples. By evaluating the analytical uncertainty of individual components using certified reference materials we have quantified the overall analytical uncertainty of the multi-element ID ICPMS method at 1-2%. Individual components include sampling/weighing, purity of reagents, purity of spike solutions, calibration of spikes, determination of isotopic ratios, instrumental sources of error, correction of mass discrimination effect, values of constants, and operator bias. We have used the ID-determined trace elements for internal standardization to improve indirectly the analysis of 14 other (mainly mono-isotopic trace elements) by external calibration. The overall analytical uncertainty for those data is about 2-3%. In addition, we have analyzed USGS and MPI-DING geological reference materials (BHVO-1, BHVO-2, KL2-G, ML3B-G) to quantify the overall bias of the measurement procedure. Trace element analysis of geological reference materials yielded results that agree mostly within about 2-3% relative to the reference values. Since these results match the conclusions obtained by the investigation of the overall analytical uncertainty, we take this as a measure for the validity of multi-element ID ICPMS. (orig.)

The Determination of Composite Elements in Zircaloy-2 by X-Ray Fluorescence and Emission Spectrometry Method

International Nuclear Information System (INIS)

Dian Anggraini; Rosika Kriswarini; Yusuf N

2007-01-01

Analysis of composing elements in zircaloy-2 has been done by Emission Spectrometry method and X-Ray Fluorescence (XRF). The aim of the analysis is to verify conformity between composing elements in zircaloy-2 and the material certificate. Spectrometry Emission method has higher sensitivity in element determination of a material than that of XRF method, so can be estimated that emission spectrometry method has higher accuracy than that of XRF method. The result of qualitative analysis by Emission Spectrometry indicate that the composing elements in zircaloy-2 were Sn, Cr and Ni. However, the qualitative analysis result by XRF method indicated that the composing elements in zircaloy 2 were Sn, Cr, Ni and Fe. Fe element can not be analysed by Emission Spectrometry method because Emission Spectrometer did not equipped with Fe detector. The quantitative analysis result of the composing elements in the material with both methods showed that Sn, Cr and Ni concentration of zircaloy 2 existed in concentration ranges of the material certificate. Result of statistical test (F and t-test) of analysis result of both methods can be used for analyzing composing elements in zircaloy 2. Emission Spectrometry method was more sensitive and accurate for determining Cr and Ni element in zircaloy 2 than that of emission Spectrometry method but both methods had same accuracy. The precision of measurement of Sn, Cr and Ni element using XRF method was better than that of Emission spectrometry method. (author)

Simultaneous multi-element analysis of some edible pulses using neutron activation analysis

International Nuclear Information System (INIS)

El-Sweify, F.H.; Metwally, E.; Abdel-Khalik, H.

2007-01-01

This paper comprises the application of instrumental neutron activation analysis (INAA) for multi-element determination in some edible pulse samples. These edible pulses are usually daily used in the Egyptian kitchen. These were: anise, cumin, coriander, caraway, black cumin, white kidney bean, lupine, lentil, chickpea, broad bean, peanut, almond, and fenugreek. The pulses have been analyzed as dehulled pulses, in the case of legume and oil pulses with simultaneous analysis of their respective skins. The determined elements were: Ce, Co, Cr, Cs, Eu, Fe, Hf, Rb, Sb, Sc, Sr, Th and Zn. The element content in the dehulled pulses and their respective skins has been compared. Some elements were major or minor elements where others were trace elements. Standard reference materials were used to assure quality control, accuracy and precision of the technique. (author)

Application of a microwave-based desolvation system for multi-elemental analysis of wine by inductively coupled plasma based techniques

Energy Technology Data Exchange (ETDEWEB)

Grindlay, Guillermo [Department of Analytical Chemistry, Nutrition and Food Sciences, University of Alicante, P.O. Box 99, 03080 Alicante (Spain)], E-mail: guillermo.grindlay@ua.es; Mora, Juan; Maestre, Salvador; Gras, Luis [Department of Analytical Chemistry, Nutrition and Food Sciences, University of Alicante, P.O. Box 99, 03080 Alicante (Spain)

2008-11-23

Elemental wine analysis is often required from a nutritional, toxicological, origin and authenticity point of view. Inductively coupled plasma based techniques are usually employed for this analysis because of their multi-elemental capabilities and good limits of detection. However, the accurate analysis of wine samples strongly depends on their matrix composition (i.e. salts, ethanol, organic acids) since they lead to both spectral and non-spectral interferences. To mitigate ethanol (up to 10% w/w) related matrix effects in inductively coupled plasma atomic emission spectrometry (ICP-AES), a microwave-based desolvation system (MWDS) can be successfully employed. This finding suggests that the MWDS could be employed for elemental wine analysis. The goal of this work is to evaluate the applicability of the MWDS for elemental wine analysis in ICP-AES and inductively coupled plasma mass spectrometry (ICP-MS). For the sake of comparison a conventional sample introduction system (i.e. pneumatic nebulizer attached to a spray chamber) was employed. Matrix effects, precision, accuracy and analysis throughput have been selected as comparison criteria. For ICP-AES measurements, wine samples can be directly analyzed without any sample treatment (i.e. sample dilution or digestion) using pure aqueous standards although internal standardization (IS) (i.e. Sc) is required. The behaviour of the MWDS operating with organic solutions in ICP-MS has been characterized for the first time. In this technique the MWDS has shown its efficiency to mitigate ethanol related matrix effects up to concentrations of 1% (w/w). Therefore, wine samples must be diluted to reduce the ethanol concentration up to this value. The results obtained have shown that the MWDS is a powerful device for the elemental analysis of wine samples in both ICP-AES and ICP-MS. In general, the MWDS has some attractive advantages for elemental wine analysis when compared to a conventional sample introduction system such

Application of a microwave-based desolvation system for multi-elemental analysis of wine by inductively coupled plasma based techniques

International Nuclear Information System (INIS)

Grindlay, Guillermo; Mora, Juan; Maestre, Salvador; Gras, Luis

2008-01-01

Elemental wine analysis is often required from a nutritional, toxicological, origin and authenticity point of view. Inductively coupled plasma based techniques are usually employed for this analysis because of their multi-elemental capabilities and good limits of detection. However, the accurate analysis of wine samples strongly depends on their matrix composition (i.e. salts, ethanol, organic acids) since they lead to both spectral and non-spectral interferences. To mitigate ethanol (up to 10% w/w) related matrix effects in inductively coupled plasma atomic emission spectrometry (ICP-AES), a microwave-based desolvation system (MWDS) can be successfully employed. This finding suggests that the MWDS could be employed for elemental wine analysis. The goal of this work is to evaluate the applicability of the MWDS for elemental wine analysis in ICP-AES and inductively coupled plasma mass spectrometry (ICP-MS). For the sake of comparison a conventional sample introduction system (i.e. pneumatic nebulizer attached to a spray chamber) was employed. Matrix effects, precision, accuracy and analysis throughput have been selected as comparison criteria. For ICP-AES measurements, wine samples can be directly analyzed without any sample treatment (i.e. sample dilution or digestion) using pure aqueous standards although internal standardization (IS) (i.e. Sc) is required. The behaviour of the MWDS operating with organic solutions in ICP-MS has been characterized for the first time. In this technique the MWDS has shown its efficiency to mitigate ethanol related matrix effects up to concentrations of 1% (w/w). Therefore, wine samples must be diluted to reduce the ethanol concentration up to this value. The results obtained have shown that the MWDS is a powerful device for the elemental analysis of wine samples in both ICP-AES and ICP-MS. In general, the MWDS has some attractive advantages for elemental wine analysis when compared to a conventional sample introduction system such

Multi-elemental determination of trace elements in deep seawater by inductively coupled plasma mass spectrometry with resin preconcentration

International Nuclear Information System (INIS)

Sumida, Takashi; Nakazato, Tetsuya; Tao, Hiroaki

2003-01-01

A miniaturized column (ca. 3 mm i.d., 40 mm length), packed with a chelating resin (0.2 g) with iminodiacetic acid groups (Muromac A-1), was tested for the preconcentration of trace elements in seawater. After preconcentration, the column was washed with ammonium acetate buffer (pH 5.5) and water to remove the major elements, such as Ca and Mg, and was then eluted with 4 ml of 2 mol l -1 nitric acid. Twenty-six trace elements were determined by inductively coupled plasma mass spectrometry and inductively coupled plasma emission spectrometry. The necessary volume of the seawater sample was only 200 ml. The recoveries for most of the elements tested were over 90%, although those for Al, V and Th were around 70%. The trueness and precision were evaluated by analyzing a standard reference material of seawater (NASS-4, NRC Canada). The observed values obtained with the present method showed good agreement with the certified values. The present method was also applied to deep seawater samples collected at Muroto, Japan. A difference in the rare earth element pattern, especially the Ce anomaly, between the deep seawater sample and the surface seawater sample was observed, as well as the differences of the concentrations of many trace elements. (author)

Multi-element trace analysis of solid samples using one-photon two-step RIMS

International Nuclear Information System (INIS)

Telle, H. H.; Abraham, C. J.; Jones, O. R.; Krustev, T.

1998-01-01

In this study we have investigated the feasibility of multi-element analysis using a simple 1+1 photo-excitation/photo-ionization scheme. Although such schemes are usually far from ideal for optimum resonance ionization, they are the approach of choice if one wishes to maintain a simple, easy-to-operate laser set-up which is potentially suitable for routine analysis. In addition, we only made use of the second-harmonic tuning range of a single dye. While this limits the range of elements which are accessible in the 1+1 RIS scheme it further adds to the simplicity and allows for automation of sequential multi-element analysis

Infinite elements for soil-structure interaction analysis in multi-layered halfspaces

International Nuclear Information System (INIS)

Yun, Chung Bang; Kim, Jae Min; Yang, Shin Chu

1994-01-01

This paper presents the theoretical aspects of a computer code (KIESSI) for soil-structure interaction analysis in a multi-layered halfspace using infinite elements. The shape functions of the infinite elements are derived from approximate expressions of the analytical solutions. Three different infinite elements are developed. They are the horizontal, the vertical and the comer infinite elements (HIE, VIE and CIE). Numerical example analyses are presented for demonstrating the effectiveness of the proposed infinite elements

A computer programme for use in the development of multi-element x-ray-fluorescence methods of analysis

International Nuclear Information System (INIS)

Wall, G.J.

1985-01-01

A computer programme (written in BASIC) is described for the evaluation of spectral-line intensities in X-ray-fluorescence spectrometry. The programme is designed to assist the analyst while he is developing new analytical methods, because it facilitates the selection of the following evaluation parameters: calculation models, spectral-line correction factors, calibration curves, calibration ranges, and point deletions. In addition, the programme enables the analyst to undertake routine calculations of data from multi-element analyses in which variable data-reduction parameters are used for each element

Neutron activation spectrometry and neutron activation analysis in analytical geochemistry

International Nuclear Information System (INIS)

Dulski, P.; Moeller, P.

1975-07-01

The present report is to show the geochemists who are interested in neutron activation spectrometry (NAS) and neutron activation analysis (NAA) which analytical possibilities these methods offer him. As a review of these analytical possibilities, a lieterature compolation is given which is subdivided into two groups: 1) rock (basic, intermediary, acid, sediments, soils and nuds, diverse minerals, tectites, meteorites and lunar material). 2) ore (Al, Au, Be, Cr, Cu, Mn, Mo, Fe, Pb, Pt, Sn, Ti, W, Zn, Zr, U and phosphate ore, polymetallic ores, fluorite, monazite and diverse ores). The applied methods as well as the determinable elements in the given materials can be got from the tables. On the whole, the literature evaluation carried out makes it clear that neutron activation spectrometry is a very useful multi-element method for the analysis of rocks. The analysis of ores, however, is subjected to great limitations. As rock analysis is very frequently of importance in prospecting for ore deposits, the NAS proves to be extremely useful for this very field of application. (orig./LH) [de

Analysis of trace elements by means of accelerator secondary ion mass spectrometry

International Nuclear Information System (INIS)

Ender, R.M.

1997-01-01

The analysis of material composition and trace element concentration is of increasing interest primarily in semiconductor technology but also in metallurgy, geology, biology and medicine. At present, Secondary Ion Mass Spectrometry (SIMS) is in many respects the best technique to provide 3-dimensional information on the distribution of trace elements with concentrations below 1 ppm. However, due to the presence of molecular ions the detectability of many trace elements it restricted because of molecular mass interferences. In addition, detectors used in SIMS have a background counting rate of 0.1-1 Hz, which further limits trace element analysis. In Accelerator Mass Spectrometry (AMS) long-lived radionuclides are detected free of molecular interferences and detector background at isotopic ratios as low as 10 -15 . Moreover, isobaric interferences can be reduced as well. In order to benefit from these advantages a combination of SIMS and AMS (Accelerator SIMS) has been proposed almost 20 years ago, but no facility has ever been fully developed. It has been the aim of this work to add a new sputtering chamber for AMS measurements of ultrapure semiconductor material to the existing PSI/ETH AMS facility. To fulfill the requirements of material analysis, an UHV chamber with special precautions against contamination has been built and adapted to the existing AMS setup. For sputtering, a commercial Cs gun with an ExB filter and a 1 o beam bend for neutral particle suppression is used to obtain a pure Cs ion beam. The gun is equipped with different apertures for varying the diameter of the beam spot. With the integrated scanning unit the 10 keV Cs beam can be rastered over approximately 1 mm 2 . This allows different applications such as bulk analysis, depth profiling and imaging. The secondary ion extraction is matched to the ion optical and geometrical requirements of the existing accelerator mass spectrometer. (author) figs., tabs., 67 refs

The element analysis of high purity beryllium by method of laser mass-spectrometry

International Nuclear Information System (INIS)

Virich, V.D.; Kisel', O.V.; Kovtun, K.V.; Pugachev, N.S.; Yakobson, L.A.

2003-01-01

The operation is devoted to examination of a possibility of the analysis of element composition pure and high purity model of a beryllium is model by a method of laser mass spectrometry. The advantages of a method in a part of finding of a small amount of admixtures in comparison with other modes of the analysis are exhibited. The possibility of quantitative definition of a content in beryllium samples of gas-making admixtures-C,N,O surveyed

Determination of trace elements in soy milk using ICP atomic emission spectrometry

International Nuclear Information System (INIS)

Tanaka, Satoko; Chayama, Kenji

2009-01-01

The present study investigated the optimal method for the multi-element quantification of 9 elements in soy milk: calcium, copper, iron, potassium, magnesium, manganese, sodium, phosphorus, and zinc. Results obtained using ICP atomic emission spectrometry were compared with those obtained by atomic absorption spectrometry, which is the standard method. The same sample was measured using both ICP atomic emission spectrometry and atomic absorption spectrometry. The percentage of minerals recovered by ICP atomic emission spectrometry ranged from 99.3% to 102%, which was equivalent to that by atomic absorption spectrometry. Therefore, a good result with standard deviation was obtained. The mineral contents of 16 samples of commercially-available soy milk products were measured. The Cu content was significantly proportional to the amount of soybean solids (P < 0.001). Moreover, although relation-ships did not attain statistical significance, the consents of Fe, Zn, K, Mg and P were proportional to the amount of soybean solids, and were highest in soy milk, followed by prepared soy milk and so milk beverage. The Ca content of modified soy milk was significantly higher than that of soy milk and soy milk-based beverages (P < 0.001). Furthermore, the Na content in soy milk was significantly lower. (author)

Multi-element analysis, bioavailability and fractionation of herbal tea products

Energy Technology Data Exchange (ETDEWEB)

Szymczycha-Madeja, Anna; Welna, Maja; Zyrnicki, Wieslaw, E-mail: anna.szymczycha@pwr.wroc.pl [Wroclaw University of Technology, Chemistry Department, Analytical Chemistry Division, Wroclaw (Poland)

2013-05-15

Herbal teas (Mentha piperitae foliumand mixture Marticaria chamomilla flos with Lavandula officinalis flos) were compared considering the total contents of micro (Al, Ba, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Sr, Ti, V) and macro (C, H, N, S, Ca, Mg, P) elements, bioavailability and fractionation. Different methods (inductively coupled plasma optical emission spectrometry (ICP OES), Fourier transform infrared spectroscopy (FTIR) and CHNS elemental analysis) were applied. The microwave-assisted digestion procedure was found to be more effective than the hot-plate heating for the wet acid digestion of tea. The application of the modified BCR (Community Bureau of Reference) sequential extraction procedure exhibited differences in the concentrations of metal bound to reducible and oxidizable fractions. The accuracy of method was verified by analysis of certified reference material INCT-TL{sup -1} Tea Leaves. The daily intake of all elements from the analyzed herbal tea infusion did not exceed the maximum permissible levels and does not constitute health risk. (author)

Multi-element analysis, bioavailability and fractionation of herbal tea products

International Nuclear Information System (INIS)

Szymczycha-Madeja, Anna; Welna, Maja; Zyrnicki, Wieslaw

2013-01-01

Herbal teas (Mentha piperitae foliumand mixture Marticaria chamomilla flos with Lavandula officinalis flos) were compared considering the total contents of micro (Al, Ba, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Sr, Ti, V) and macro (C, H, N, S, Ca, Mg, P) elements, bioavailability and fractionation. Different methods (inductively coupled plasma optical emission spectrometry (ICP OES), Fourier transform infrared spectroscopy (FTIR) and CHNS elemental analysis) were applied. The microwave-assisted digestion procedure was found to be more effective than the hot-plate heating for the wet acid digestion of tea. The application of the modified BCR (Community Bureau of Reference) sequential extraction procedure exhibited differences in the concentrations of metal bound to reducible and oxidizable fractions. The accuracy of method was verified by analysis of certified reference material INCT-TL -1 Tea Leaves. The daily intake of all elements from the analyzed herbal tea infusion did not exceed the maximum permissible levels and does not constitute health risk. (author)

Elemental analysis using instrumental neutron activation analysis and inductively coupled plasma atomic emission spectrometry: a comparative study

International Nuclear Information System (INIS)

Chung, Yong Sam; Choi, Kwang Soon; Moon, Jong Hwa; Kim, Sun Ha; Lim, Jong Myoung; Kim, Young Jin; Quraishi, Shamshad Begum

2003-05-01

Elemental analyses for certified reference materials were carried out using instrumental neutron activation analysis and inductively coupled plasma-atomic emission spectrometry. Five Certified Reference Materials (CRM) were selected for the study on comparative analysis of environmental samples. The CRM are Soil (NIST SRM 2709), Coal fly ash (NIST SRM 1633a), urban dust (NIST SRM 1649a) and air particulate on filter media (NIST SRM 2783 and human hair (GBW 09101)

Paradigms in isotope dilution mass spectrometry for elemental speciation analysis

International Nuclear Information System (INIS)

Meija, Juris; Mester, Zoltan

2008-01-01

Isotope dilution mass spectrometry currently stands out as the method providing results with unchallenged precision and accuracy in elemental speciation. However, recent history of isotope dilution mass spectrometry has shown that the extent to which this primary ratio measurement method can deliver accurate results is still subject of active research. In this review, we will summarize the fundamental prerequisites behind isotope dilution mass spectrometry and discuss their practical limits of validity and effects on the accuracy of the obtained results. This review is not to be viewed as a critique of isotope dilution; rather its purpose is to highlight the lesser studied aspects that will ensure and elevate current supremacy of the results obtained from this method

Multi-element neutron activation analysis and solution of classification problems using multidimensional statistics

International Nuclear Information System (INIS)

Vaganov, P.A.; Kol'tsov, A.A.; Kulikov, V.D.; Mejer, V.A.

1983-01-01

The multi-element instrumental neutron activation analysis of samples of mountain rocks (sandstones, aleurolites and shales of one of gold deposits) is performed. The spectra of irradiated samples are measured by Ge(Li) detector of the volume of 35 mm 3 . The content of 22 chemical elements is determined in each sample. The results of analysis serve as reliable basis for multi-dimensional statistic information processing, they constitute the basis for the generalized characteristics of rocks which brings about the solution of classification problem for rocks of different deposits

Elemental analysis of air particulate samples in Jakarta area by x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Yumiarti; Yusuf, M.; Mellawati, June; Menry, Yulizon; Surtipanti S

1998-01-01

Determination of elements in air particulate samples collected from Jakarta, especially from industrial area Pulo Gadung, also from residence, office, and recreation sites had been carried out. The samples collected periodically from August through December 1996. The elements were analyzed by X-ray fluorescence spectrometry method. Quantitative and qualitative analyses were done using QXAS AXIL (Quantitative X-ray Analysis System of x-ray Spectra by Iterative Least squares fitting) and QAES (Quantitative Analyses of Environmental Samples) package program. Results of the analyses showed that the content of heavy metal elements in air particulate samples from all areas studied were still below the maximum permissible concentration. (authors)

Fully automated dissolution and separation methods for inductively coupled plasma atomic emission spectrometry rock analysis. Application to the determination of rare earth elements

International Nuclear Information System (INIS)

Govindaraju, K.; Mevelle, G.

1987-01-01

In rock analysis laboratories, sample preparation is a serious problem, or even an enormous bottleneck. Because this laboratory is production-oriented, this problem was attacked by automating progressively, different steps in rock analysis for major, minor and trace elements. This effort has been considerably eased by the fact that all sample preparation schemes in this laboratory for the past three decades have been based on an initial lithium borate fusion of rock samples and all analytical methods based on multi-element atomic emission spectrometry, with switch-over from solid analysis by arc/spark excitation to solution analysis by plasma excitation in 1974. The sample preparation steps which have been automated are: weighing of samples and fluxes, lithium borate fusion, dissolution and dilution of fusion products and ion-exchange separation of difficult trace elements such as rare earth elements (REE). During 1985 and 1986, these different unit operations have been assembled together as peripheral units in the form of a workstation, called LabRobStation. A travelling robot is the master of LabRobStation, with all peripheral units at its reach in 10 m 2 workspace. As an example of real application, the automated determination of REE, based on more than 8000 samples analysed during 1982 and 1986, is presented. (author)

Macro elemental analysis of food samples by nuclear analytical technique

Science.gov (United States)

Syahfitri, W. Y. N.; Kurniawati, S.; Adventini, N.; Damastuti, E.; Lestiani, D. D.

2017-06-01

Energy-dispersive X-ray fluorescence (EDXRF) spectrometry is a non-destructive, rapid, multi elemental, accurate, and environment friendly analysis compared with other detection methods. Thus, EDXRF spectrometry is applicable for food inspection. The macro elements calcium and potassium constitute important nutrients required by the human body for optimal physiological functions. Therefore, the determination of Ca and K content in various foods needs to be done. The aim of this work is to demonstrate the applicability of EDXRF for food analysis. The analytical performance of non-destructive EDXRF was compared with other analytical techniques; neutron activation analysis and atomic absorption spectrometry. Comparison of methods performed as cross checking results of the analysis and to overcome the limitations of the three methods. Analysis results showed that Ca found in food using EDXRF and AAS were not significantly different with p-value 0.9687, whereas p-value of K between EDXRF and NAA is 0.6575. The correlation between those results was also examined. The Pearson correlations for Ca and K were 0.9871 and 0.9558, respectively. Method validation using SRM NIST 1548a Typical Diet was also applied. The results showed good agreement between methods; therefore EDXRF method can be used as an alternative method for the determination of Ca and K in food samples.

Analysis of oil shale and oil shale products for certain minor elements

International Nuclear Information System (INIS)

Dickman, P.T.; Purdy, M.; Doerges, J.E.; Ryan, V.A.; Poulson, R.E.

1977-01-01

The University of Wyoming was contracted by the Department of Energy's Laramie Energy Research Center (LERC) to develop rapid, inexpensive, and simple methods of quantitative and qualitative elemental analysis for products used and generated in the simulated in-situ retorting of oil shale. Alpha particle spectrometry was used to determine the radioisotope content of the aqueous retort products. Alpha particles are mono-energetic and the spectrometry method employed had very low background levels (1 count per 2000 seconds). These factors allow for both the quantitative and qualitative analysis of natural radioisotopes at the 1 ppm level. Sample preparation does not require any chemical treatment. Energy dispersive x-ray fluorescence (XRF) was used for the multi-element analysis of the retort products. The XRF, integrated with a mini-computer, allows rapid analysis of several elements in multiple samples. XRF samples require minimal amounts of preparation and analytical results are highly reproducible. This paper presents the methods developed and preliminary analytical results from oil shale by-products. Results from the analysis of oil shale rocks are not yet ready for presentation

Minimally-invasive Laser Ablation Inductively Coupled Plasma Mass Spectrometry analysis of model ancient copper alloys

Energy Technology Data Exchange (ETDEWEB)

Walaszek, Damian [University of Warsaw, Faculty of Chemistry, Biological and Chemical Research Centre, Żwirki i Wigury 101, 02-089 Warszawa (Poland); Laboratory for Analytical Chemistry, Swiss Federal Laboratories for Materials Science and Technology, Überlandstrasse 129, CH-8600 Dübendorf (Switzerland); Senn, Marianne; Wichser, Adrian [Laboratory for Analytical Chemistry, Swiss Federal Laboratories for Materials Science and Technology, Überlandstrasse 129, CH-8600 Dübendorf (Switzerland); Faller, Markus [Laboratory for Jointing Technology and Corrosion, Swiss Federal Laboratories for Materials Science and Technology, Überlandstrasse 129, CH-8600 Dübendorf (Switzerland); Wagner, Barbara; Bulska, Ewa [University of Warsaw, Faculty of Chemistry, Biological and Chemical Research Centre, Żwirki i Wigury 101, 02-089 Warszawa (Poland); Ulrich, Andrea [Laboratory for Analytical Chemistry, Swiss Federal Laboratories for Materials Science and Technology, Überlandstrasse 129, CH-8600 Dübendorf (Switzerland)

2014-09-01

This work describes an evaluation of a strategy for multi-elemental analysis of typical ancient bronzes (copper, lead bronze and tin bronze) by means of laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS).The samples originating from archeological experiments on ancient metal smelting processes using direct reduction in a ‘bloomery’ furnace as well as historical casting techniques were investigated with the use of the previously proposed analytical procedure, including metallurgical observation and preliminary visual estimation of the homogeneity of the samples. The results of LA-ICPMS analysis were compared to the results of bulk composition obtained by X-ray fluorescence spectrometry (XRF) and by inductively coupled plasma mass spectrometry (ICPMS) after acid digestion. These results were coherent for most of the elements confirming the usefulness of the proposed analytical procedure, however the reliability of the quantitative information about the content of the most heterogeneously distributed elements was also discussed in more detail. - Highlights: • The previously proposed procedure was evaluated by analysis of model copper alloys. • The LA-ICPMS results were comparable to the obtained by means of XRF and ICPMS. • LA-ICPMS results indicated the usefulness of the proposed analytical procedure.

Determination of trace elements in Katana (Japanese sword) by neutron activation analysis with multidimensional γ-ray spectrometry

International Nuclear Information System (INIS)

Okada, Y.; Hirai, S.; Ohya, S.; Kimura, Atsushi; Hatsukawa, Yuichi; Toh, Yosuke; Koizumi, Mitsuo; Oshima, Masumi

2006-01-01

In this study, we tried to measure trace elements (As and Sb) in Katana (Japanese swords) by multidimensional γ-ray spectrometry method (GEMINI-II) and conventional counting method for neutron activation analysis (NAA). The determined values by GEMINI-II and conventional counting were in good agreement with. Using the multidimensional γ-ray spectrometry (GEMINI-II) to determine As and Sb was improved by 7 times and 10 times compared with the conventional counting method. (author)

Application of delayed X-ray spectrometry to the analysis of some rare earth elements

International Nuclear Information System (INIS)

Pillay, A.E.; Mboweni, R.C.M.

1991-01-01

The capabilities of delayed x-ray spectrometry preceded by isotope-source thermal neutron activation for the specific determination of some rare earth elements (Sm, Eu, Dy, Ho) in small powdered samples was evaluated. The feasibility study relied heavily on the low-energy sensitivity of the detector used. Detection of the delayed x-rays was achieved with a 100-mm 2 Ge detector with the ability to produce optimum photopeak-to-noise ratios. The rare earth elements were chosen on the basis of their inherent favourable nuclear properties for producing a practicable x-ray yield and on the demand for their analysis. Analytical results are presented over a range of concentrations for the elements of interest and the potential of the technique for application to their general routine analysis is discussed. Interferences from the sample matrix can be suppressed to an extent that makes the method almost independent of the matrix. This and other features make the technique a strong rival to conventional activation analysis. (author)

Development of realtime monitoring technology for laser photoreaction product - Development of glow discharge-mass spectrometry (GD-MS) hybrid techniques for trace analysis of refractory elements

Energy Technology Data Exchange (ETDEWEB)

Lee, Sang Chun [Kyungnam University, Masan (Korea); Kim, Ha Suck [Seoul National University, Seoul (Korea); Kim, Hyo Jin [Dongduk Women' s University, Seoul (Korea)

2000-04-01

This research is focusing on development of hybrid techniques of glow discharge-mass spectrometry for the trace analysis of refractory elements. At first, we developed a glow discharge(GD) ionization cell and its characteristics was investigated. The new GD cell was designed based on direct current hollow cathode glow discharge and it is used for quadrupole mass analyzer and time-of-flight mass analyzer. Currently, GD-quadrupole mass spectrometry is working for the analysis of refractory elements. The experimental results show relatively good for trace analysis. In addition, ion mobile spectrometry using plasma and liquid discharge technique were investigated for the analysis of refractory elements and both techniques need more investigation to deduce the their usefulness. 30 refs., 67 figs., 4 tabs. (Author)

Controlled Dissolution of Surface Layers for Elemental Analysis by Inductively Coupled Plasma-Mass Spectrometry

Energy Technology Data Exchange (ETDEWEB)

Lorge, Susan Elizabeth [Iowa State Univ., Ames, IA (United States)

2007-01-01

Determining the composition of thin layers is increasingly important for a variety of industrial materials such as adhesives, coatings and microelectronics. Secondary ion mass spectrometry (SIMS), Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), glow discharge optical emission spectroscopy (GDOES), glow discharge mass spectrometry (GDMS), and laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) are some of the techniques that are currently employed for the direct analysis of the sample surface. Although these techniques do not suffer from the contamination problems that often plague sample dissolution studies, they do require matrix matched standards for quantification. Often, these standards are not readily available. Despite the costs of clean hoods, Teflon pipette tips and bottles, and pure acids, partial sample dissolution is the primary method used in the semiconductor industry to quantify surface impurities. Specifically, vapor phase decomposition (VPD) coupled to ICP-MS or total reflection x-ray fluorescence (TXRF) provides elemental information from the top most surface layers at detection sensitivities in the 10⁷-10¹⁰atoms/cm² range. The ability to quantify with standard solutions is a main advantage of these techniques. Li and Houk applied a VPD-like technique to steel. The signal ratio of trace element to matrix element was used for quantification. Although controlled dissolution concentrations determined for some of the dissolved elements agreed with the certified values, concentrations determined for refractory elements (Ti, Nb and Ta) were too low. LA-ICP-MS and scanning electron microscopy (SEM) measurements indicated that carbide grains distributed throughout the matrix were high in these refractory elements. These elements dissolved at a slower rate than the matrix element, Fe. If the analyte element is not removed at a rate similar to the matrix element a true

Optimal acid digestion for multi-element analysis of different waste matrices

DEFF Research Database (Denmark)

Götze, Ramona; Astrup, Thomas Fruergaard

of the distinct waste materials and recyclables. The purpose of this study is to evaluate the performance of different standardized microwave assisted acid digestion methods on waste samples and subsequent multi-element analysis. Six acid digestion methods were applied on a Paper & Cardboard and Composite waste...

Provenance Establishment of Stingless Bee Honey Using Multi-element Analysis in Combination with Chemometrics Techniques.

Science.gov (United States)

Shadan, Aidil Fahmi; Mahat, Naji A; Wan Ibrahim, Wan Aini; Ariffin, Zaiton; Ismail, Dzulkiflee

2018-01-01

As consumption of stingless bee honey has been gaining popularity in many countries including Malaysia, ability to identify accurately its geographical origin proves pertinent for investigating fraudulent activities for consumer protection. Because a chemical signature can be location-specific, multi-element distribution patterns may prove useful for provenancing such product. Using the inductively coupled-plasma optical emission spectrometer as well as principal component analysis (PCA) and linear discriminant analysis (LDA), the distributions of multi-elements in stingless bee honey collected at four different geographical locations (North, West, East, and South) in Johor, Malaysia, were investigated. While cross-validation using PCA demonstrated 87.0% correct classification rate, the same was improved (96.2%) with the use of LDA, indicating that discrimination was possible for the different geographical regions. Therefore, utilization of multi-element analysis coupled with chemometrics techniques for assigning the provenance of stingless bee honeys for forensic applications is supported. © 2017 American Academy of Forensic Sciences.

Multi-element determination in environmental samples by mass spectrometric isotope dilution analysis using thermal ionization. Pt. 2

International Nuclear Information System (INIS)

Hilpert, K.; Waidmann, E.

1988-01-01

An analytical procedure for the multi-element analysis of the elements Fe, Ni, Cu, Zn, Ga, Rb, Sr, Cd, Ba, Tl, and Pb in pine needles by mass spectrometric isotope dilution analysis using thermal ionization has been reported in Part I of this paper. This procedure is now transferred to the non-vegetable material 'Oyster Tissue' (Standard Reference Material 1566, National Bureau of Standards, USA). By a modification of the analytical procedure, it was possible to determine Cr in this material in addition to the aforementioned elements. No concentrations are certified for the elements Ga, Ba and Tl analyzed in this work. The concentrations of the remaining elements obtained by the multi-element analysis agree well with those certified. (orig.)

Analysis of organic compounds by secondary neutral mass spectrometry (SNMS) and secondary ion mass spectrometry (SIMS)

International Nuclear Information System (INIS)

Ewinger, H.P.

1993-05-01

This study is about the use of secondary neutral mass spectrometry (SNMS) and secondary ion mass spectrometry (SIMS) as analytical techniques with depth resolution in determining organic components in environmental solid microparticles. The first application of plasma SNMS to organic compounds revealed the spectra to be composed mainly of signals from the atoms of all participating elements, such as C, H, O, N, S, P, and Cl. In addition, signals produced by multi-atomic clusters can be detected, such as CH, C 2 , CH 2 , C 2 H, and C 3 , as well as signals indicating the presence of organic compounds with hetero elements, such as OH, NH, and CN. Their intensity decreases very markedly with increasing numbers of atoms. Among the signals from bi-atomic clusters, those coming from elements with large mass differences are most intense. The use of plasma SNMS with organic compounds has shown that, except for spurious chemical reactions induced by ion bombardment and photodesorption by the photons of the plasma, it is possible to analyze with resolution in depth, elements of organic solids. A more detailed molecular characterization of organic compounds is possible by means of SIMS on the basis of multi-atomic fragments and by comparison with suitable signal patterns. (orig./BBR) [de

A provenance study of iron archaeological artefacts by Inductively Coupled Plasma-Mass Spectrometry multi-elemental analysis

International Nuclear Information System (INIS)

Desaulty, Anne-Marie; Mariet, Clarisse; Dillmann, Philippe; Joron, Jean Louis; Fluzin, Philippe

2008-01-01

Raw materials and wastes (i.e. ore, slag and laitier) from ironmaking archaeological sites have been analyzed in order to understand the behavior of the trace elements in the ancient ironmaking processes and to find the significant-most elements to characterize an iron making region. The ICP-MS (Inductively Coupled Plasma Mass Spectrometry) appears to be an excellent technique for this type of studies. The comparison between the ICP-MS results obtained with the Standard Addition method and the INAA (Instrumental Neutron Activation Analyses) results proved that Sc, Co, (Ni), Rb, Cs, Ba, La, Ce, Sm, Eu, Yb, Hf, Th, U contents in the ores, slag and laitiers, and Co and Ni contents in the cast iron can be successfully determined by ICP-MS after wet acid digestion (low detection limits, good sensitivity and precision). By using significant trace element pairs (Yb/Ce, Ce/Th, La/Sc, U/Th, Nb/Y) present in the ores, laitiers and slag, it is possible to discriminate different French ironmaking regions as the Pays de Bray, Lorraine and Pays d'Ouche. These results open the way to further studies on the provenance of iron objects. The comparison between the ICP-MS results obtained with the Standard Calibration Curves method and the INAA results shows that matrices rich in iron, affect the ICP-MS analyses by suppressing the analytes signal. Further studies are necessary to improve understanding matrix effects

Can laser-ionisation time-of-flight mass spectrometry be a promising alternative to laser ablation/inductively-coupled plasma mass spectrometry and glow discharge mass spectrometry for the elemental analysis of solids?

NARCIS (Netherlands)

Sysoev, AA; Sysoev, AA

2002-01-01

At the beginning of the age of laser-ionisation mass spectrometry (LIMS) increasing numbers of publications were observed. However, later the method began to run into obstacles associated with poor reproducibility of analysis and large variations in elemental sensitivities so that the wide interest

Study of radionuclide and element characterization of Angola marine sediment using low background gamma spectrometry and instrumental neutron activation analysis techniques

International Nuclear Information System (INIS)

Teixeira, M.C.P.; Vuong Huu Tan; Truong Y; Ho Manh Dung; Le Nhu Sieu; Cao Dong Vu; Nguyen Thanh Binh

2007-01-01

The concentrations of radionuclides and chemical elements in Angola marine sediment samples were determined by using low background gamma (LBG) spectrometry and instrumental neutron activation analysis (INAA). The combination of radionuclide and elemental concentration values yielded synergy in the validation of analytical data and identification of sediment sources modeled by multivariate factor analysis. Varimax rotation factor analysis based on the elemental concentrations revealed five sources contributed to the sediment composition, i.e. crustal, sea-salt, industrial, coal-related and Se-related sources. (author)

Trace Element Analysis of Minerals in Magmatic-Hydrothermal Ores by Laser Ablation Inductively-Coupled Plasma Mass Spectrometry: Approaches and Opportunities

Directory of Open Access Journals (Sweden)

Nigel Cook

2016-10-01

Full Text Available Laser ablation inductively-coupled plasma mass spectrometry (LA-ICP-MS has rapidly established itself as the method of choice for generation of multi-element datasets for specific minerals, with broad applications in Earth science. Variation in absolute concentrations of different trace elements within common, widely distributed phases, such as pyrite, iron-oxides (magnetite and hematite, and key accessory minerals, such as apatite and titanite, can be particularly valuable for understanding processes of ore formation, and when trace element distributions vary systematically within a mineral system, for a vector approach in mineral exploration. LA-ICP-MS trace element data can assist in element deportment and geometallurgical studies, providing proof of which minerals host key elements of economic relevance, or elements that are deleterious to various metallurgical processes. This contribution reviews recent advances in LA-ICP-MS methodology, reference standards, the application of the method to new mineral matrices, outstanding analytical uncertainties that impact on the quality and usefulness of trace element data, and future applications of the technique. We illustrate how data interpretation is highly dependent on an adequate understanding of prevailing mineral textures, geological history, and in some cases, crystal structure.

Non destructive multi elemental analysis using prompt gamma neutron activation analysis techniques: Preliminary results for concrete sample

Energy Technology Data Exchange (ETDEWEB)

Dahing, Lahasen Normanshah [School of Applied Physics, Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor, Malaysia and Malaysian Nuclear Agency (Nuklear Malaysia), Bangi 43000, Kajang (Malaysia); Yahya, Redzuan [School of Applied Physics, Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor (Malaysia); Yahya, Roslan; Hassan, Hearie [Malaysian Nuclear Agency (Nuklear Malaysia), Bangi 43000, Kajang (Malaysia)

2014-09-03

In this study, principle of prompt gamma neutron activation analysis has been used as a technique to determine the elements in the sample. The system consists of collimated isotopic neutron source, Cf-252 with HPGe detector and Multichannel Analysis (MCA). Concrete with size of 10×10×10 cm{sup 3} and 15×15×15 cm{sup 3} were analysed as sample. When neutrons enter and interact with elements in the concrete, the neutron capture reaction will occur and produce characteristic prompt gamma ray of the elements. The preliminary result of this study demonstrate the major element in the concrete was determined such as Si, Mg, Ca, Al, Fe and H as well as others element, such as Cl by analysis the gamma ray lines respectively. The results obtained were compared with NAA and XRF techniques as a part of reference and validation. The potential and the capability of neutron induced prompt gamma as tool for multi elemental analysis qualitatively to identify the elements present in the concrete sample discussed.

ISMAS international discussion meet on elemental mass spectrometry in health and environmental sciences

International Nuclear Information System (INIS)

Aggarwal, S.K.; Jaison, P.G.; Telmore, V.M.

2011-04-01

Mass spectrometry is an indispensable analytical tool associated with almost all branches of science including biology, chemistry, earth sciences, nuclear science, physics, etc. The technique holds tremendous potential owing to its high sensitivity, selectivity and its ability to measure small changes in the isotopic abundances of different elements. Innovations in mass spectrometry instrumentation are further widening the scope by making it possible to handle very large bio-molecules and polymers. New techniques for mass analysis, novel designs for ionization and developments in electronic accessories have contributed to elevate mass spectrometry to a position of prime importance in research. Development in mass spectrometry has revolutionized the study of micro-nutrient metabolism, of biologically active compounds and for drug discovery in pharmaceutical research. Elemental mass spectrometry is making major contributions to food toxicology, food forensics, and study of metabolism of nutrient minerals including Fe, Zn, Ca, Cu and Se. The area of speciation analysis using hyphenated techniques as well as electro-spray ionization have undergone a phenomenal evolution and development in the recent past. Impressive progress in mass spectrometry towards lower detection limits, higher resolution and molecule-specific detection at trace levels in complex matrices allows new frontiers to be crossed. Papers relevant to INIS are indexed separately

Precision and Accuracy of k0-NAA Method for Analysis of Multi Elements in Reference Samples

International Nuclear Information System (INIS)

Sri-Wardani

2004-01-01

Accuracy and precision of k 0 -NAA method could determine in the analysis of multi elements contained in reference samples. The analyzed results of multi elements in SRM 1633b sample were obtained with optimum results in bias of 20% but it is in a good accuracy and precision. The analyzed results of As, Cd and Zn in CCQM-P29 rice flour sample were obtained with very good result in bias of 0.5 - 5.6%. (author)

Assessment of elemental pollution in soil of Islamabad city using instrumental neutron activation analysis and atomic absorption spectrometry techniques

International Nuclear Information System (INIS)

Daud, M.; Wasim, M.; Khalid, N.; Zaidi, J.H.; Iqbal, J.

2009-01-01

The soil samples of nine different sites in Islamabad were studied for their elemental composition. Instrumental neutron activation analysis and atomic absorption spectrometry were employed and 33 elements were determined. The acquired data were analyzed using descriptive statistics, principal component analysis, cluster analysis, pollution level index and enrichment factor. A perusal of results shows a distribution of elemental concentration in two major groups, one along the highway and the other in industrial area of Islamabad. The soil along the highway sites was found to be relatively less polluted than at the sites in the industrial area. The enrichment factor indicates the presence of As, Pb, Sb, Se and Sn at higher levels. The method validation was done by analyzing IAEA reference materials SL-1 (lake sediment) and S7 (soil). (orig.)

Derivative flame atomic absorption spectrometry and its application in trace analysis

International Nuclear Information System (INIS)

Sun, H. W.; Li, L. Q.

2005-01-01

Flame atomic absorption spectrometry is an accepted and widely used method for the determination of trace elements in a great variety of samples. But its sensitivity doesn't meet the demands of trace and ultra-trace analysis for some samples. The derivative signal processing technique, with a very high capability for enhancing sensitivity, was developed for flame atomic absorption spectrometry. The signal models of conventional flame atomic absorption spectrometry are described. The equations of derivative signals are established for flame atomic absorption spectrometry, flow injection atomic absorption spectrometry (FI-FAAS) and atom trapping flame atomic absorption spectrometry (AT-FAAS). The principle and performance of the derivative atomic absorption spectrometry are evaluated. The derivative technique based on determination of variation rate of signal intensity with time (dl/dt) is different from the derivative spectrophotometry based on determination of variation rate of signal intensity with wavelength (dl/dhλ). Derivative flame atomic absorption spectrometry has higher sensitivity, lower detection limits and better accuracy. It has been applied to the direct determination of trace elements without preconcentration. If the derivative technique was combined with several preconcentration techniques, the sensitivity would be enhanced further for ultra-trace analysis with good linearity. The applications of derivative flame atomic absorption spectroscopy are reviewed for trace element analysis in biological, pharmaceutical, environmental and food samples

Evaluation of pressed powders and thin section standards for multi-elemental analysis by conventional and micro-PIXE analysis

International Nuclear Information System (INIS)

Homma-Takeda, Shino; Iso, Hiroyuki; Ito, Masaki

2010-01-01

For multi-elemental analysis, various standards are used to quantify the elements consists of environmental and biological samples. In this paper two different configuration standards, pressed powders and thin section standards, were assessed for their purpose as standards by conventional and micro-PIXE analysis. Homogeneity of manganese, iron, zinc (Zn), copper and yttrium added to pressed powder standard materials were validated and the relative standard deviation (RSD) of the X-ray intensity of the standards was 2 area and the metal concentration was acceptable. (author)

Application of PCA-LDA method to determine the geographical origin of tea based on determination of stable isotopes and multi-elements

International Nuclear Information System (INIS)

Yuan Yuwei; Zhang Yongzhi; Yang Guiling; Zhang Zhiheng; Fu Haiyan; Han Wenyan; Li Shufang

2013-01-01

The ratio of stable isotope and concentration of multi-element in tea was determinated with isotope ratio mass spectrometry (IRMS) and inductively coupled plasma mass spectrometry (ICP-MS). Pattern recognition techniques with principal component analysis (PCA) and linear discriminant analysis (LDA) were used to classify the geographical origins of tea from Fujian, Shandong and Zhejiang province, and Yuyao, Jinhua and Xihu region of Zhejiang. The results showed the values of δ"1"5N, δ"1"3C, δD, δ"1"8O and the ratios of "2"0"6Pb/"2"0"7Pb, "2"0"8Pb/"2"0"6Pb and "8"7Sr/"8"6Sr in tea samples were different from different origins. There was also large variable for the concentrations of 27 mineral elements, such as Li, Be, Na and so on, with a specific character of origin. The method of PCA could be used to classify the geographical origin of tea from different origins but with a cross in the scatter plot. However, PCA combining with LDA could gave correct assignation percentages of 99% for the tea samples among Fujian, Shandong and Zhejiang provinces, and 87% for the tea samples among Yuyao, Jinhua and Xihu region of Zhejiang. These results revealed that it was possible and feasible to classify the geographical origin of tea by the method of PCA-LDA based on the determination of isotopes and multi-elements. (authors)

Multi-elemental profile of some Brazilian make-up products by instrumental neutron activation analysis

Energy Technology Data Exchange (ETDEWEB)

Dalmazio, Ilza; Menezes, Maria Angela de B.C., E-mail: id@cdtn.b, E-mail: menezes@cdtn.b [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil). Servico de Reator e Tecnicas Analiticas. Lab. de Ativacao Neutronica

2011-07-01

Recent works have shown that analysis in cosmetics and beauty products from the European and Asian markets indicate the presence of U, Th and rare earths besides other trace elements. Considering these previous findings and health issues, it would be valuable to obtain information on elements in cosmetics available in the Brazilian market. The purpose of this study was to acquire a multi-elemental profile of some Brazilian make-up products of diverse brands. Samples of eye shadow, liquid base, facial concealer, lipstick, and compact face powder were analyzed applying neutron activation analysis, k{sub 0}-standardization method at CDTN/CNEN, using the TRIGA Mark I IPR-R1 research reactor. Concentrations of more than 30 elements in samples are presented and it was found elements included in Brazilian National Health Surveillance Agency prohibitive list, rare earths, Th and U in a minimum of two cosmetic samples. (author)

Multi-elemental profile of some Brazilian make-up products by instrumental neutron activation analysis

International Nuclear Information System (INIS)

Dalmazio, Ilza; Menezes, Maria Angela de B.C.

2011-01-01

Recent works have shown that analysis in cosmetics and beauty products from the European and Asian markets indicate the presence of U, Th and rare earths besides other trace elements. Considering these previous findings and health issues, it would be valuable to obtain information on elements in cosmetics available in the Brazilian market. The purpose of this study was to acquire a multi-elemental profile of some Brazilian make-up products of diverse brands. Samples of eye shadow, liquid base, facial concealer, lipstick, and compact face powder were analyzed applying neutron activation analysis, k 0 -standardization method at CDTN/CNEN, using the TRIGA Mark I IPR-R1 research reactor. Concentrations of more than 30 elements in samples are presented and it was found elements included in Brazilian National Health Surveillance Agency prohibitive list, rare earths, Th and U in a minimum of two cosmetic samples. (author)

[Rapid determination of major and trace elements in the salt lake clay minerals by X-ray fluorescence spectrometry].

Science.gov (United States)

Wang, Xiao-Huan; Meng, Qing-Fen; Dong, Ya-Ping; Chen, Mei-Da; Li, Wu

2010-03-01

A rapid multi-element analysis method for clay mineral samples was described. This method utilized a polarized wave-length dispersive X-ray fluorescence spectrometer--Axios PW4400, which had a maximum tube power of 4 000 watts. The method was developed for the determination of As, Mn, Co, Cu, Cr, Dy, Ga, Mo, P, Pb, Rb, S, Sr, Ni, ,Cs, Ta, Th, Ti, U, V, Y, Zn, Zr, MgO, K2O, Na2O, CaO, Fe2O3, Al2O3, SiO2 and so on. Thirty elements in clay mineral species were measured by X-ray fluorescence spectrometry with pressed powder pellets. Spectral interferences, in particular the indirect interferences of each element, were studied. A method to distinguish the interference between each other periodic elements in element periodic table was put forward. The measuring conditions and existence were mainly investigated, and the selected background position as well as corrected spectral overlap for the trace elements were also discussed. It was found that the indirect spectral overlap line was the same important as direct spectral overlap line. Due to inducing the effect of indirect spectral overlap, some elements jlike Bi, Sn, W which do not need analysis were also added to the elements channel. The relative standard deviation (RSD) was in the range of 0.01% to 5.45% except three elements Mo, Cs and Ta. The detection limits, precisions and accuracies for most elements using this method can meet the requirements of sample analysis in clay mineral species.

Elemental and isotopic characterization of Japanese and Philippine polished rice samples using instrumental neutron activation analysis and isotope ratio mass spectrometry

International Nuclear Information System (INIS)

Pabroa, Preciosa Corazon B.; Sucgang, Raymond J.; Mendoza, Norman dS.; Ebihara, Mitsuru

2011-01-01

Rice is a staple food for most Asian countries such as the Philippines and Japan and as such its elemental and isotopic content are of interest to the consumers. Its elemental content may reflect the macro nutrient reduction during milling or probable toxic elements uptake. Three Japanese and four Philippine polished rice samples in his study mostly came from rice bought from supermarkets.These rice samples were washed, dried and ground to fine powder. Instrumental neutron activation analysis (INAA), a very sensitive non-destructive multi-element analytical technique, was used for the elemental analysis of the samples and isotope-ratio mass spectrometry (IRMS) was used to obtain the isotopic signatures of the samples. Results show that compared with the unpolished rice standard NIES CRM10b, the polished Japanese and Philippine rice sampled show reduced concentrations of elements by as much as 1/3 to 1/10 of Mg, Mn, K and Na. Levels of Ca and Zn are not greatly affected. Arsenic is found in all the Japanese rice tested at an average concentration of 0.103 μg/g and three out of four of the Philippine rice at an average concentration of 0.070 μg/g. Arsenic contamination may have been introduced from the fertilizer used in rice fields. Higher levels of Br are seen in two of the Philippine rice at 14 and 34 μg/g with the most probable source being the pesticide methyl bromide. Isotopic ratio of ae 13 C show signature of a C3 plant with possible narrow distinguishable signature of Japanese rice within -27.5 to -28.5 while Philippine rice within -29 to -30. More rice samples will be analyzed to gain better understanding of isotopic signatures to distinguish inter-varietal and/or geographical differences. Elemental composition of soil samples of rice samples sources will be determined for better understanding of uptake mechanisms. (author)

Analysis of Trace Elements in Rat Bronchoalveolar Lavage Fluid by Inductively Coupled Plasma Mass Spectrometry.

Science.gov (United States)

Qamar, Wajhul; Al-Ghadeer, Abdul Rahman; Ali, Raisuddin; Abuelizz, Hatem A

2017-08-01

The main objective was to determine the elemental profile of the lung lining fluid of rats which are used as model animals in various experiments. Lung lining fluid elemental constitution obtained after bronchoalveolar lavage fluid (BALF) was analyzed by inductively coupled plasma mass spectrometry (ICP-MS) to determine the biological trace elements along with calcium and magnesium. BALF was collected from healthy rats using a tracheal cannula. However, cells in BALF were counted to monitor any underlying inflammatory lung condition. Cell free BALF samples were processed and analyzed for the elements including magnesium (Mg), calcium (Ca), chromium (Cr), manganese (Mn), iron (Fe), nickel (Ni), copper (Cu), zinc (Zn), selenium (Se), bromine (Br), and iodine (I). In view of this, calcium concentration was the highest (6318.08 ± 3094.3 μg/L) and copper concentration was the lowest (0.89 ± 0.21 μg/L). The detected elements, from high to low concentration, include Ca > Mg > Fe > Br > I > Cr > Ni > Zn > Mn > Se > Cu. Pearson's correlation analysis revealed no significant correlation between cell count and concentration of any of the element detected in BALF. Correlation analysis also revealed significant positive correlation among Fe, I, Cr, Ni, and Mn. Ca was found to be correlated negatively with Cu and positively with Se. Br and Mg found to be positively correlated with each other. Zn remained the only element that was not found to be correlated with any of the elements in the rat BALF.

Analysis of selected elements in tobacco by wavelength dispersive X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Martin, J.M.

1988-01-01

A rapid method for the determination of 16 elements in tobacco by wavelength dispersive X-ray fluorescence spectrometry has been developed. The method is accurate and precise, and requires only 9 min per sample for quantitation. Sample preparation consists of placing a portion of dried, ground tobacco in a sample cup, and pressing at 25 tons pressure to make a compressed pellet. This pellet is then automatically analyzed by X-ray fluorescence for 16 elements. The results are stored on a computer disk for future recall and report generation. The elements are: Al, Br, Ca, Cl, Cu, Fe, K, Mg, Mn, Na, P, S, Si, Sr, Ti and Zn

Imaging of elements in leaves of tobacco by solid sampling–electrothermal vaporization–inductively coupled plasma-optical emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Masson, Pierre, E-mail: masson@bordeaux.inra.fr

2014-12-01

Plants take up and store elements according to the environment in which they are growing. Because plants are at the base of the food chain, the determination of essential elements or toxic elements in plant materials is of importance. However, it is assumed that the element content determined on selected tissues may provide more specific information than that derived from the whole plant analysis. In this work, we assessed the feasibility of solid sampling–electrothermal vaporization–inductively coupled plasma-optical emission spectrometry analyses for quantitative imaging of Cd and Mg in plant leaves. Leaves of tobacco (Nicotiana tabacum) were selected to be used as samples. To produce a two dimensional image, sections cut from leaf samples were analyzed. Cellulose doped with multi-element solution standards was used as calibration samples. Two certified reference materials (NIST SRM 1547 Peach Leaves and NIST SRM 1573a Tomato leaves) were used to verify the accuracy of measurements with good agreement between the measured concentrations and the certified values. Quantitative imaging revealed the inhomogeneous distribution of the selected elements. Excess of Cd and Mg tended to be focused on peripheral regions and the tip of the leaf.

Multi Elemental Study Using Prompt Gamma Technique

International Nuclear Information System (INIS)

Normanshah Dahing; Muhamad Samudi Yasir; Normanshah Dahing; Hanafi Ithnin; Mohd Fitri Abdul Rahman; Hearie Hassan

2016-01-01

In this study, principle of prompt gamma neutron activation analysis has been used as a technique to determine the elements in the sample. The system consists of collimated isotopic neutron source, Cf-252 with HPGe detector and Multichannel Analysis (MCA). Concrete with size of 10x10x10 cm 3 and 15x15x15 cm 3 were analysed as sample. When neutrons enter and interact with elements in the concrete, the neutron capture reaction will occur and produce characteristic prompt gamma ray of the elements. The preliminary result of this study demonstrate the major element in the concrete was determined such as Si, Mg, Ca, Al, Fe and H as well as others element, such as Cl by analysis the gamma ray lines respectively. The results obtained were compared with computer simulation, NAA and XRF as a part of reference and validation. The potential and the capability of neutron induced prompt gamma as tool for multi elemental analysis qualitatively to identify the elements present in the concrete sample discussed. (author)

NanoSIMS multi-element imaging reveals internalisation and nucleolar targeting for a highly-charged polynuclear platinum compound.

Science.gov (United States)

Wedlock, Louise E; Kilburn, Matt R; Liu, Rong; Shaw, Jeremy A; Berners-Price, Susan J; Farrell, Nicholas P

2013-08-11

Simultaneous multi-element imaging using NanoSIMS (nano-scale secondary ion mass spectrometry), exploiting the novel combination of (195)Pt and (15)N in platinum-am(m)ine antitumour drugs, provides information on the internalisation and subcellular localisation of both metal and ligands, and allows identification of ligand exchange.

[Rapid multi-elemental analysis on four precious Tibetan medicines based on LIBS technique].

Science.gov (United States)

Liu, Xiao-na; Shi, Xin-yuan; Jia, Shuai-yun; Zhao, Na; Wu, Zhi-sheng; Qiao, Yan-jiang

2015-06-01

The laser-induced breakdown spectroscopy (LIBS) was applied to perform a qualitative elementary analysis on four precious Tibetan medicines, i. e. Renqing Mangjue, Renqing Changjue, 25-herb coral pills and 25-herb pearl pills. The specific spectra of the four Tibetan medicines were established. In the experiment, Nd: YAG and 1 064 nm-baseband pulse laser were adopted to collect the spectra. A laser beam focused on the surface of the samples to generate plasma. Its spectral signal was detected by using spectrograph. Based on the National Institute of Standard and Technology (NIST) database, LIBS spectral lines were indentified. The four Tibetan medicines mainly included Ca, Na, K, Mg and other elements and C-N molecular band. Specifically, Fe was detected in Renqing Changjue and 25-herb pearl pills; heavy mental elements Hg and Cu were shown in Renqing Mangjue and Renqing Changjue; Ag was found in Renqing Changjue. The results demonstrated that LIBS is a reliable and rapid multi-element analysis on the four Tibetan medicines. With Real-time, rapid and nondestructive advantages, LIBS has a wide application prospect in the element analysis on ethnic medicines.

Direct analysis of samples by mass spectrometry: From elements to bio-molecules using laser ablation inductively couple plasma mass spectrometry and laser desorption/ionization mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Perdian, David C. [Iowa State Univ., Ames, IA (United States)

2009-01-01

Mass spectrometric methods that are able to analyze solid samples or biological materials with little or no sample preparation are invaluable to science as well as society. Fundamental research that has discovered experimental and instrumental parameters that inhibit fractionation effects that occur during the quantification of elemental species in solid samples by laser ablation inductively coupled plasma mass spectrometry is described. Research that determines the effectiveness of novel laser desorption/ionization mass spectrometric methods for the molecular analysis of biological tissues at atmospheric pressure and at high spatial resolution is also described. A spatial resolution is achieved that is able to analyze samples at the single cell level.

Multi trace element analysis of dry biological materials by neutron activation analysis including a chemical group separation

International Nuclear Information System (INIS)

Weers, C.A.

1980-07-01

Multi-element analysis of dry biological material by neutron activation analysis has to include radiochemical separation. The evaporation process is described in terms of the half-volume. The pretreatment of the samples and the development of the destruction-evaporation apparatus are described. The successive adsorption steps with active charcoal, Al 2 O 3 and coprecipitation with Fe(OH) 3 are described. Results obtained for standard reference materials are summarized. (G.T.H.)

Accuracy and Precision in Elemental Analysis of Environmental Samples using Inductively Coupled Plasma-Atomic Emission Spectrometry

International Nuclear Information System (INIS)

Quraishi, Shamsad Begum; Chung, Yong-Sam; Choi, Kwang Soon

2005-01-01

Inductively Coupled Plasma-Atomic Emission Spectrometry followed by micro-wave digestion have been performed on different environmental Certified Reference Materials (CRMs). Analytical results show that accuracy and precision in ICP-AES analysis were acceptable and satisfactory in case of soil and hair CRM samples. The relative error of most of the elements in these two CRMs is within 10% with few exceptions and coefficient of variation is also less than 10%. Z-score as an analytical performance was also within the acceptable range (±2). ICP-AES was found as an inadequate method for Air Filter CRM due to incomplete dissolution, low concentration of elements and very low mass of the sample. However, real air filter sample could have been analyzed with high accuracy and precision by increasing sample mass during collection. (author)

Multi-element quantification of ancient/historic glasses by laser ablation inductively coupled plasma mass spectrometry using sum normalization calibration

International Nuclear Information System (INIS)

Elteren, Johannes T. van; Tennent, Norman H.; Selih, Vid S.

2009-01-01

Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) for quantitative analysis of ancient/historic glasses is subject to calibration issues which have been addressed in this work. Since ancient/historic glasses have widely ranging matrix compositions, a complementary analysis by an alternative method is generally employed to determine at least one major element which can be used as an internal standard. We demonstrate that such a complementary analysis is unnecessary using a so-called sum normalization calibration technique (mathematically formulated) by simultaneous measurement of 54 elements and normalizing them to 100% [w/w] based on their corresponding oxide concentrations. The crux of this approach is that by assuming a random internal standard concentration of a particular major oxide, e.g. SiO 2 , the normalization algorithm varies the internal standard concentration until the cumulated concentrations of all 54 elemental oxides reach 100% [w/w]. The fact that 54 elements are measured simultaneously predetermines the laser ablation mode to rastering. Nine glass standards, some replicating historic compositions, were used for calibration. The linearity of the calibration graphs (forced through the origin) represented by the relative standard deviations in the slope were between 0.1 and 6.6% using SiO 2 as an internal standard. This allows high-accuracy determination of elemental oxides as confirmed by good agreement between found and reported values for major and minor elemental oxides in some synthetic glasses with typical medieval composition (European Science Foundation 151 and 158). Also for trace elemental concentrations of lanthanides in a reference glass (P and H Developments Ltd. DLH7, a base glass composition with nominally 75 μg g -1 elements added) accurate data were obtained. Interferences from polyatomic species and doubly charged species on the masses of trace elements are possible, depending on the base composition of the

Characterisation of nuclear fuel samples by quadrupole and multi-collector inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Wernli, Beath; Guenther-Leopold, Ines; Kobler Waldis, Judith; Kopajtic, Zlatan

2003-01-01

The characterisation of nuclear fuel cycle materials for trace and minor metallic constituents is of great interest for the nuclear industry and safeguard officials. The main objective of various international programmes dealing with postirradiation examinations is to improve the knowledge of the inventories of actinides, fission and spallation products in spent nuclear fuels. The low detection limits for a large number of elements combined with the ability to analyse the isotopic composition of the elements have established inductively coupled plasma mass spectrometry (ICP-MS) as a powerful multi-element technique in diverse analytical applications for the characterisation of nuclear materials. Because numerous isobaric overlaps restrict the direct determination of many fission products by mass spectrometry, extensive chemical separations are required for these elements. In order to simplify this sample preparation procedure, a high performance liquid chromatography system (HPLC) was online coupled to the mass spectrometer. Since about 10 years a quadrupole based ICP-MS (Q-ICP-MS) combined with an HPLC is used within the Hot Laboratory of the Paul Scherrer Institut for different applications on nuclear fuel samples. Since May 2003 also a new multi-collector ICP-MS (MC-ICP-MS) is used for the mass spectrometric characterisation of nuclear fuel samples, especially for the precise determination of the isotopic vectors of fission products and actinides. Therefore, two complementary analytical systems are now available in the group of 'Isotope and Wet Analytical Chemistry'. A comparison of the analytical performance of both systems (with and without an online coupled HPLC system) for the determination of the isotopic composition and the elemental concentration of different nuclides in nuclear fuel samples, the advantages and limitations of both techniques, the accuracy and precision of the results and typical applications for both methods will be discussed in the

Application of slurry nebulization to trace elemental analysis of some biological samples by inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Mochizuki, T.; Sakashita, A.; Iwata, H.; Ishibashi, Y.; Gunji, N.

1991-01-01

The application of slurry nebulization/inductively coupled plasma mass spectrometry (ICP-MS) to trace elemental analysis of biological samples has been investigated. Three standard samples of the National Institute of Standards and Technology (NIST) were dispersed in 1% aqueous Triton X-100 solution by grinding with a planetary micronizing mill. The resulting slurries were nebulized into an ICP without any additional treatments. The 1% (m/v) slurry of the NIST bovine liver showed no significant influence on cone blockage and signal suppression/enhancement. Detection limit, precision and accuracy were discussed for the determination of 24 elements of interest in bovine liver, rice flour and pine needles. Detection limits ranged from 0.0001 μg g -1 for U to 0.52 μg g -1 for Zn at the effective integrating time of 10 s. For high mass elements, low blank values were obtained, yielding excellent limits ( -1 ). Acceptable accuracy and precision were obtained for most of the elements in the NIST bovine liver and rice flour, even for the volatile elements, such as As, Se and Br. However, relatively poor accuracy was obtained for the analysis of pine needles. (orig.)

XRF and TXRF techniques for multi-element determination of trace elements in whole blood and human hair samples

International Nuclear Information System (INIS)

Khuder, A.; Karjou, J.; Sawan, M.Kh.; Bakir, M.A.

2007-01-01

XRF and TXRF were established as useful techniques for multi-element analysis of whole blood and human head hair samples. Direct-XRF with different collimation units and different X-ray excitation modes was successfully used for the determination of S, P, K, Ca, Fe, and Br elements in blood samples and K, Ca, Mn, Fe elements in human hair samples. Direct analysis by TXRF was used for the determination of Rb and Sr in digested blood and human hair samples, respectively, while, the co-precipitation method using APDC for TXRF analysis was used for the determination of Ni, Cu, Zn, and Pb elements in both matrices. As a result, the improved XRF and TXRF methods were applied for multi-element determination of elements in whole blood and human hair samples in non-occupational exposed population living in Damascus city. The mean concentrations of analyzed elements in both matrices were on the reported range values for non-occupational population in other countries. (author)

XRF and TXRF techniques for multi-element determination of trace elements in whole blood and human hair samples

International Nuclear Information System (INIS)

Khuder, A.; Karjou, J.; Sawan, M.Kh.; Bakir, M.A.

2008-01-01

XRF and TXRF were established as useful techniques for multi-element analysis of whole blood and human head hair samples. Direct-XRF with different collimation units and different X-ray excitation modes was successfully used for the determination of S, P, K, Ca, Fe, and Br elements in blood samples and K, Ca, Mn, Fe elements in human hair samples. Direct analysis by TXRF was used for the determination of Rb and Sr in digested blood and human hair samples, respectively, while, the co-precipitation method using APDC for TXRF analysis was used for the determination of Ni, Cu, Zn, and Pb elements in both matrices. As a result, the improved XRF and TXRF methods were applied for multi-element determination of elements in whole blood and human hair samples in non-occupational exposed population living in Damascus city. The mean concentrations of analyzed elements in both matrices were on the reported range values for non-occupational population in other countries. (author)

Gas chromatography/plasma spectrometry - an important analytical tool for elemental speciation studies

International Nuclear Information System (INIS)

Wuilloud, Jorgelina C.A.; Wuilloud, Rodolfo G.; Vonderheide, Anne P.; Caruso, Joseph A.

2004-01-01

In this review, a full discussion and update of the state-of-the-art of gas chromatography (GC) coupled to all known plasma spectrometers is presented. A brief introductive discussion of the advantages and disadvantages of GC-plasma interfaces, as well as types of plasmas and mass spectrometers, is given. The plasma-based techniques covered include inductively coupled plasma mass spectrometry (ICP-MS) microwave-induced plasma optical emission spectrometry (MIP-OES), and inductively coupled plasma optical emission spectrometry (ICP-OES). Also, different variants of plasma sources, such as low power plasmas and glow discharge (GD) sources, are described and compared with respect to their capabilities in elemental speciation. Recent advances and alternative mass analyzers (collision/reaction cell; time-of-flight; double-focusing sector field) are also mentioned. Different aspects of the GC-plasma coupling are discussed with particular attention to the applications of these hyphenated techniques to the analysis of elemental species. Additionally, classical and modern sample preparation methods, including extraction and/or preconcentration and derivatization reactions, are presented and evaluated

Multi-element analysis of crude-oil samples by 14.6 MeV neutron activation

International Nuclear Information System (INIS)

Cam, N.F.; Cigeroglu, F.; Erduran, M.N.

1997-01-01

The instrumental neutron activation technique, using the SAMEST T-400 neutron generator with 14.6 MeV neutrons produced from 3 H(d,n) 4 He reaction, is demonstrated for multi-element analysis of Saudi-Arabian crude-oil samples. The system parameters for the absolute method (e.g., the counting solid-angle, intrinsic efficiency of the γ-ray detector, effective neutron flux, activation cross sections, etc.)were determined and the results of elemental concentrations were presented with the corrections for all possible interferences having been carefully considered. (author)

Advances in low atomic number element analysis by wavelength dispersive x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Vrebos, B.

1996-01-01

Traditionally, the analysis of low atomic number has been a chal1enging task for wavelength dispersive x-ray fluorescence spectrometry. Among the most important factors influencing analysis of the low atomic number elements (from Z=11 downwards) are the fluorescence yield, absorption and the dispersion. The effect of each of these factors on the overall performance will be illustrated. The long wavelengths involved (longer than I nm) used to pose severe problems concerning the monochromator used. Early instruments relied on lead stearate or Blodgett Langmuir soap films for the diffraction of the characteristic radiation. Nowadays, synthetic multilayers are commonly used. The performance of these multilayers is determined by the reflectivity, the resolution and the absorption of the characteristic radiation to be diffracted. These parameters can be optimised by adequately selecting the composition of the materials involved. The sensitivity of the modem instruments is sufficient to allow quantitative analysis. However, this aspect of WDS XRF is still met with considerable scepticism. Examples of quantitative analysis will be given to illustrate the current capability

[Study on the determination of 14 inorganic elements in coffee by inductively coupled plasma mass spectrometry].

Science.gov (United States)

Nie, Xi-Du; Fu, Liang

2013-07-01

Samples of coffee were digested by microwave digestion, and inorganic elements amounts of Na, Mg, P, Ca, Cr, Mn, Fe, Co, Cu, Zn, As, Se, Mo and Pb in sample solutions were determined by inductively coupled plasma mass spectrometry (ICP-MS). HNO3 + H2O2 was used to achieve the complete decomposition of the organic matrix in a closed-vessel microwave oven. The working parameters of the instrument were optimized. The results showed that the relative standard deviation (RSD) was less than 3.84% for all the elements, and the recovery was found to be 92.00% -106.52% by adding standard recovery experiment. This method was simple, sensitive and precise and can perform simultaneous multi-elements determination of coffee, which could satisfy the sample examination request and provide scientific rationale for determining inorganic elements of coffee.

Application of alpha spectrometry to the discovery of new elements by heavy-ion-beam bombardment

International Nuclear Information System (INIS)

Nitschke, J.M.

1983-05-01

Starting with polonium in 1898, α-spectrometry has played a decisive role in the discovery of new, heavy elements. For even-even nuclei, α-spectra have proved simple to interpret and exhibit systematic trends that allow extrapolation to unknown isotopes. The early discovery of the natural α-decay series led to the very powerful method of genetically linking the decay of new elements to the well-established α-emission of daughter and granddaughter nuclei. This technique has been used for all recent discoveries of new elements including Z = 109. Up to mendelevium (Z = 101), thin samples suitable for α-spectrometry were prepared by chemical methods. With the advent of heavy-ion accelerators new sample preparation methods emerged. These were based on the large momentum transfer associated with heavy-ion reactions, which produced energetic target recoils that, when ejected from the target, could be thermalized in He gas. Subsequent electrical deposition or a He-jet technique yielded samples that were not only thin enough for α-spectroscopy, but also for α- and #betta#-recoil experiments. Many variations of these methods have been developed and are discussed. For the synthesis of element 106 an aerosol-based recoil transport technique was devised. In the most recent experiments, α-spectrometry has been coupled with the magnetic analysis of the recoils. The time from production to analysis of an isotope has thereby been reduced to 10 - 6 s; while it was 10 - 1 to 10 0 s for He-jets and 10 1 to 10 3 s for rapid chemical separations. Experiments are now in progress to synthesize super heavy elements (SHE) and to analyze them with these latest techniques. Again, α-spectrometry will play a major role since the expected signature for the decay of a SHE is a sequence of α-decays followed by spontaneous fission

Plant trait detection with multi-scale spectrometry

Science.gov (United States)

Gamon, J. A.; Wang, R.

2017-12-01

Proximal and remote sensing using imaging spectrometry offers new opportunities for detecting plant traits, with benefits for phenotyping, productivity estimation, stress detection, and biodiversity studies. Using proximal and airborne spectrometry, we evaluated variation in plant optical properties at various spatial and spectral scales with the goal of identifying optimal scales for distinguishing plant traits related to photosynthetic function. Using directed approaches based on physiological vegetation indices, and statistical approaches based on spectral information content, we explored alternate ways of distinguishing plant traits with imaging spectrometry. With both leaf traits and canopy structure contributing to the signals, results exhibit a strong scale dependence. Our results demonstrate the benefits of multi-scale experimental approaches within a clear conceptual framework when applying remote sensing methods to plant trait detection for phenotyping, productivity, and biodiversity studies.

Investigations on the direct introduction of cigarette smoke for trace elements analysis by inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Chang, Michael J.; Naworal, John D.; Walker, Kathleen; Connell, Chris T.

2003-01-01

Direct introduction of mainstream cigarette smoke into an inductively coupled plasma mass spectrometry (ICP-MS) has been investigated with respect to its feasibility for on-line analysis of trace elements. An automated apparatus was designed and built interfacing a smoking machine with an ICP-MS for smoke generation, collection, injection and analysis. Major and minor elements present in the particulate phase and the gas phase of mainstream cigarette smoke of 2R4F reference cigarettes have been qualitatively identified by examination of their full mass spectra. This method provides a rapid-screening analysis of the transfer of trace elements into mainstream smoke during cigarette combustion. A full suite of elements present in the whole cigarette smoke has been identified, including As, B, Ba, Br, Cd, Cl, Cs, Cu, Hg, I, K, Li, Mn, Na, Pb, Rb, Sb, Sn, Tl and Zn. Of these elements, the major portions of B, Ba, Cs, Cu, K, Li, Mn, Na, Pb, Rb, Sn, Tl and Zn are present in the particulate phase, whereas the major portion of Hg is present in the gas phase. As, Br, Cd, Cl, I and Sb exist in a distribution between the gas phase and the particulate phase. Depending on the element, the precision of measurement ranges from 5 to 25% in terms of relative standard deviation of peak height and peak area, based on the fourth puff of 2R4F mainstream cigarette smoke analyzed in five smoking replicates

Rare earth elements determined in Antarctic ice by inductively coupled plasma-Time of flight, quadrupole and sector field-mass spectrometry: An inter-comparison study

International Nuclear Information System (INIS)

Dick, D.; Wegner, A.; Gabrielli, P.; Ruth, U.; Barbante, C.; Kriews, M.

2008-01-01

Inductively coupled plasma mass spectrometry (ICP-MS) is a suitable tool for multi-element analysis at low concentration levels. Rare earth element (REE) determinations in standard reference materials and small volumes of molten ice core samples from Antarctica have been performed with an ICP-time of flight-MS (ICP-TOF-MS) system. Recovery rates for REE in e.g. SPS-SW1 amounted to ∼103%, and the relative standard deviations were 3.4% for replicate analysis at REE concentrations in the lower ng L -1 range. Analyses of REE concentrations in Antarctic ice core samples showed that the ICP-TOF-MS technique meets the demands of restricted sample mass. The data obtained are in good agreement with ICP-Quadrupole-MS (ICP-Q-MS) and ICP-Sector Field-MS (ICP-SF-MS) results. The ICP-TOF-MS system determines accurately and precisely REE concentrations exceeding 5 ng L -1 while between 0.5 and 5 ng L -1 accuracy and precision are element dependent

Computational complexity and memory usage for multi-frontal direct solvers used in p finite element analysis

KAUST Repository

Calo, Victor M.; Collier, Nathan; Pardo, David; Paszyński, Maciej R.

2011-01-01

The multi-frontal direct solver is the state of the art for the direct solution of linear systems. This paper provides computational complexity and memory usage estimates for the application of the multi-frontal direct solver algorithm on linear systems resulting from p finite elements. Specifically we provide the estimates for systems resulting from C0 polynomial spaces spanned by B-splines. The structured grid and uniform polynomial order used in isogeometric meshes simplifies the analysis.

Computational complexity and memory usage for multi-frontal direct solvers used in p finite element analysis

KAUST Repository

Calo, Victor M.

2011-05-14

The multi-frontal direct solver is the state of the art for the direct solution of linear systems. This paper provides computational complexity and memory usage estimates for the application of the multi-frontal direct solver algorithm on linear systems resulting from p finite elements. Specifically we provide the estimates for systems resulting from C0 polynomial spaces spanned by B-splines. The structured grid and uniform polynomial order used in isogeometric meshes simplifies the analysis.

Multi-constituent determination and fingerprint analysis of Scutellaria indica L. using ultra high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

Science.gov (United States)

Liang, Xianrui; Zhao, Cui; Su, Weike

2015-11-01

An ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry method integrating multi-constituent determination and fingerprint analysis has been established for quality assessment and control of Scutellaria indica L. The optimized method possesses the advantages of speediness, efficiency, and allows multi-constituents determination and fingerprint analysis in one chromatographic run within 11 min. 36 compounds were detected, and 23 of them were unequivocally identified or tentatively assigned. The established fingerprint method was applied to the analysis of ten S. indica samples from different geographic locations. The quality assessment was achieved by using principal component analysis. The proposed method is useful and reliable for the characterization of multi-constituents in a complex chemical system and the overall quality assessment of S. indica. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

use of x-ray fluorescence spectrometry to determine trace elements ...

African Journals Online (AJOL)

NIJOTECH

Abstract. This paper deals with application of X-ray fluorescence spectrometry for the detection of trace elements in graphic. An X-ray spectrometer was constructed and used to carry out measurements on graphite spheres impregnated with different chemical elements. The intensities of the lines of these trace elements, ...

Optimization of trace elements determination (Arsenic and chromium) in blood and serum of human by electrothermal atomic absorption spectrometry

International Nuclear Information System (INIS)

Ahmadi Faghih, M. A.; Aflaki, F.

2003-01-01

Trace elements play an important role in the bio physiology of cells by affecting their growth and contributions to various biological processes such as wound healing. Determination of toxic trace elements in biological fluids is an important subject of interest for toxicological purposes. Increasing the concentration of these elements in the blood levels, cause serious diseases in patients. Recently instrumental analysis procedures such as atomic absorption spectrometry have been used in clinical measurements for determination of many toxic trace elements in the biological samples. In this paper we are reporting the study of various methods of blood and serum samples preparation for determining the toxic trace elements of Arsenic and Chromium. The measurement of this elements performed by using electrothermal atomic absorption spectrometry. The best and reliable results for Chromium analysis was achieved by injection of diluted serum samples, where the samples were diluted with H CI 0.1N. In Arsenic analysis, the best results obtained by extraction with aqueous solution of TCA. For determining all of these elements the RSD% was less than 5%

Multi-element analyses of Vietnamese environmental samples for radiation protection

International Nuclear Information System (INIS)

Mai, T.H.; Nguyen, T.B.; Nguyen, T.N.; Yoshida, S.

2005-01-01

The Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) were used for measuring 8 major and 27 trace elements in food and soil samples collected in Vietnam. The concentration of elements in food samples was different from different locations and also from different food groups. Depth profiles of the elements were discussed for soil samples. (author)

Simultaneous multi-element determination in different seed samples of Dodonaea viscosa hopseed using instrumental neutron activation analysis

International Nuclear Information System (INIS)

El-Sweify, Fatma H.; El-Amir, Mahmoud A.; Mostafa, Mohamed; Ramadan, Hala E.; Rashad, Ghada M.

2016-01-01

Instrumental neutron activation analysis technique (INAA) was applied for nondestructive multi-element analysis of seed samples of the plant Dodonaea viscosa hopseed. This plant is distributed all over Egypt, because of its suitable properties. The samples were collected from some bushes grown at different sites in some governorates, in July of each year during the period from 2004 to 2011. The determined elements are: Co, Cs, Eu, Fe, Hg, Ni, Rb, Sc, Se, Sr and Zn, under the chosen irradiation and cooling times. The content of some elements has been compared with data obtained from previous work on analysis of various kinds of seeds. The influence of some parameters on the determined elemental content is discussed. Standard reference materials IAEA-155 and IAEA-V-10 were used to assure quality control, accuracy and precision of the technique.

Simultaneous multi-element determination in different seed samples of Dodonaea viscosa hopseed using instrumental neutron activation analysis

Energy Technology Data Exchange (ETDEWEB)

El-Sweify, Fatma H.; El-Amir, Mahmoud A.; Mostafa, Mohamed; Ramadan, Hala E.; Rashad, Ghada M. [Atomic Energy Authority, Cairo (Egypt). Hot Lab. Center

2016-07-01

Instrumental neutron activation analysis technique (INAA) was applied for nondestructive multi-element analysis of seed samples of the plant Dodonaea viscosa hopseed. This plant is distributed all over Egypt, because of its suitable properties. The samples were collected from some bushes grown at different sites in some governorates, in July of each year during the period from 2004 to 2011. The determined elements are: Co, Cs, Eu, Fe, Hg, Ni, Rb, Sc, Se, Sr and Zn, under the chosen irradiation and cooling times. The content of some elements has been compared with data obtained from previous work on analysis of various kinds of seeds. The influence of some parameters on the determined elemental content is discussed. Standard reference materials IAEA-155 and IAEA-V-10 were used to assure quality control, accuracy and precision of the technique.

Determination of the rare earth elements in marine pore waters and associated sediments

International Nuclear Information System (INIS)

Kennedy, H.; Elderfield, H.

Accurate and precise determinations of natural levels of rare earth elements (R.E.E.) in sea water and pore water are highly reliant upon the size and variability of the analytical blank, the method for determining the yield, and, to a lesser extent, the inherent precision of the instrument used. Isotope dilution mass spectrometry (IDMS) together with ultra-clean room techniques has been successfully used in the determinations of rare earth elements in pore waters. Simultaneous multi-element analysis by inductively coupled plasma atomic emission spectrometry (ICP) provides an alternative to IDMS for a rapid determination of R.E.E. in sediments. (author)

Multi-element analysis of small biological samples

International Nuclear Information System (INIS)

Rokita, E.; Cafmeyer, J.; Maenhaut, W.

1983-01-01

A method combining PIXE and INAA was developed to determine the elemental composition of small biological samples. The method needs virtually no sample preparation and less than 1 mg is sufficient for the analysis. The method was used for determining up to 18 elements in leaves taken from Cracow Herbaceous. The factors which influence the elemental composition of leaves and the possible use of leaves as an environmental pollution indicator are discussed

Resonance ionization mass spectrometry of ion beam sputtered neutrals for element- and isotope-selective analysis of plutonium in micro-particles

Energy Technology Data Exchange (ETDEWEB)

Erdmann, N. [Institute for Transuranium Elements, European Commission Joint Research Centre, Karlsruhe (Germany); Kratz, J.V.; Trautmann, N. [Johannes Gutenberg-University Mainz, Institute of Nuclear Chemistry, Mainz (Germany); Passler, G. [Johannes Gutenberg-University Mainz, Institute of Physics, Mainz (Germany)

2009-11-15

Micro-particles containing actinides are of interest for risk assessments of contaminated areas, nuclear forensic analyses, and IAEA as well as Euratom safeguards programs. For their analysis, secondary ion mass spectrometry (SIMS) has been established as the state-of-the-art standard technique. In the case of actinide mixtures within the particles, however, SIMS suffers from isobaric interferences (e.g., {sup 238}U/{sup 238}Pu, {sup 241}Am/{sup 241}Pu). This can be eliminated by applying resonance ionization mass spectrometry which is based on stepwise resonant excitation and ionization of atoms with laser light, followed by mass spectrometric detection of the produced ions, combining high elemental selectivity with the analysis of isotopic compositions. This paper describes the instrumental modifications for coupling a commercial time-of-flight (TOF)-SIMS apparatus with three-step resonant post-ionization of the sputtered neutrals using a high-repetition-rate (kHz) Nd:YAG laser pumped tunable titanium:sapphire laser system. Spatially resolved ion images obtained from actinide-containing particles in TOF-SIMS mode demonstrate the capability for isotopic and spatial resolution. Results from three-step resonant post-ionization of bulk Gd and Pu samples successfully demonstrate the high elemental selectivity of this process. (orig.)

Application of the multi-element analysis by X-fluorescence and neutron activation to the characterization of an archaeological site

International Nuclear Information System (INIS)

Rossini, I.

1991-06-01

The first part of this thesis is about possible analysis methods (XRF, PIXE, INAA, laser fluorimetry, and ICP), applied to Uranium, Thorium and Rubidium assays in archaeological clays and potteries. The best results have been obtained with Neutron Activation technics. The second part is about the multi-element analysis of quarries and about the research by statistical treatment of correlations between the element concentrations and the sampling sites (excavations, quarries)

Multi-element probabilistic collocation method in high dimensions

International Nuclear Information System (INIS)

Foo, Jasmine; Karniadakis, George Em

2010-01-01

We combine multi-element polynomial chaos with analysis of variance (ANOVA) functional decomposition to enhance the convergence rate of polynomial chaos in high dimensions and in problems with low stochastic regularity. Specifically, we employ the multi-element probabilistic collocation method MEPCM and so we refer to the new method as MEPCM-A. We investigate the dependence of the convergence of MEPCM-A on two decomposition parameters, the polynomial order μ and the effective dimension ν, with ν<< N, and N the nominal dimension. Numerical tests for multi-dimensional integration and for stochastic elliptic problems suggest that ν≥μ for monotonic convergence of the method. We also employ MEPCM-A to obtain error bars for the piezometric head at the Hanford nuclear waste site under stochastic hydraulic conductivity conditions. Finally, we compare the cost of MEPCM-A against Monte Carlo in several hundred dimensions, and we find MEPCM-A to be more efficient for up to 600 dimensions for a specific multi-dimensional integration problem involving a discontinuous function.

Trace-element analysis of uranium ores by x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Coetzee, P.P.; De Villiers, W.v Z.

1985-01-01

The determination of seventeen trace elements (As, Ba, Co, Cr, Cu, Mo, Nb, Ni, Pb, Sr, Th, U, V, Y, Zn, and Zr) in uranium ores by x-ray fluorescence spectrometry was investigated. For the elements with analyte lines in the vicinity of the U-L lines, large overlap corrections were necessary and only a few completely interference-free background positions were available. Consequently, the Feather and Willis method was used for determining the background intensity at the peak positions as well as mass absorption coefficients. As a result of the presence of the U-L absorption edges, both primary and secondary mass absorption coefficients had to be used for matrix corrections. Furthermore, it was observed that the background intensity in the region of the uranium lines increased with increasing uranium content of the sample, instead of the expected decrease due to the increasing mass absorption coefficient. This was attributed to the scattering of uranium lines in the spectrometer chamber. A method was developed to correct the measured intensities for this effect. The contribution from the scattering of uranium lines to the measured intensity at the various 20 positions was determined on samples with different uranium concentrations and for which the mass absorption coefficients and concentrations of the various elements were known

Multi-element neutron activation analysis of biological tissues: contribution to the study of trace element accumulation as a function of aging

International Nuclear Information System (INIS)

Gaudry, Andre.

1975-01-01

The accumulation of trace elements in various organs as a function of age was studied in rats, in connection with tissue aging phenomena. Part one reviews the various methods available to develop a programme of simultaneous multi-element analysis in biological matrices. Part two studies the precision and accuracy offered by neutron activation analysis. Special attention is paid to the problem of sample contamination by the silica glass irradiation supports. The possible causes of this effect are mentioned and a procedure limiting its harmful influence is proposed. Part three defines the restrictions introduced by the use of a method to separate the activable matrix. The fourth and last chapter describes the development of a multielement chemical separation system, designed to work semi-automatically for the simultaneous treatment of three samples and a standard in a shielded cell of small dimensions. The principles of a multi-comparator calibration where a knowledge of certain conventional but imprecise nuclear data is unnecessary owing to an experimental expedient are outlined briefly. Finally the separation method is tried out on various biological samples, including a reference (bovine liver SRM1577-NBS), and some results are given [fr

Wear And Tear Determination By Trace Multi-Element Analysis Of An Unused And Used Lubricant Oil Using Instrumental Neutron Activation Analysis

International Nuclear Information System (INIS)

Adeyemo, D.J.

2004-01-01

Instrumental neutron activation analysis technique using the Imperial College Centre consort M. K. II nuclear reactor was utilized for the determination of: As, Ba Ca CI, Co, Cr, Cu, Fe, K, Mn, Mo, Na Ni, Rb, Sb, Se, Ti, V, and Zn, in an imported and used car lubricant oil. The wear of the oil lubricated parts of the car engine was monitored by establishing a correlation between the results obtained in the analysis. The result obtained from the analysis of the unused and then used samples on a low performing oil leaking four stroke car engine showed an increase on all the elements determined except for Se and Rb. The precision for the multi-element analysis is less than 12% for most of the elements. The accuracy of the measurement is also validated by the result obtained from the analysis of NBS-SRM1635 (sub-bituminous) coal standard for the elements. The results obtained indicate that analysis of unused and used lubricant oil samples can aid in locating defects in engine parts and hence facilitated maintenance procedures

Isotope analysis of micro metal particles by adopting laser-ablation mass spectrometry

International Nuclear Information System (INIS)

Song, Kyu Seok; Ha, Young Kyung; Han, Sun Ho; Park, Yong Joon; Kim, Won Ho

2005-01-01

The isotope analysis of microparticles in environmental samples as well as laboratory samples is an important task. A special concern is necessary in particle analysis of swipe samples. Micro particles are normally analyzed either by dissolving particles in the solvents and adopting conventional analytical methods or direct analysis method such as a laser-ablation ICP mass spectrometry (LA-ICP-MS), SIMS, and SNMS (sputtered neutral mass spectrometry). But the LA-ICPMS uses large amount of samples because normally laser beam is tightly focused on the target particle for the complete ablation. The SIMS and SNMS utilize ion beams for the generation of sample ions from the particle. But the number of ions generated by an ion beam is less than 5% of the total generated particles in SIMS. The SNMS is also an excellent analytical technique for particle analysis, however, ion beam and frequency tunable laser system are required for the analysis. Recently a direct analysis of elements as well as isotopes by using laser-ablation is recognized one of the most efficient detection technology for particle samples. The laser-ablation mass spectrometry requires only one laser source without frequency tuneability with no sample pretreatment. Therefore this technique is one of the simplest analysis techniques for solid samples as well as particles. In this study as a part of the development of the new isotope analysis techniques for particles samples, a direct laser-ablation is adopted with mass spectrometry. Zinc and gadolinium were chosen as target samples, since these elements have isotopes with minor abundance (0.62% for Zn, and 0.2% for Gd). The preliminary result indicates that isotopes of these two elements are analyzed within 10% of natural abundance with good mass resolution by using direct laser-ablation mass spectrometry

Comparison of neutron activation analysis with other instrumental methods for elemental analysis of airborne particulate matter

International Nuclear Information System (INIS)

Regge, P. de; Lievens, F.; Delespaul, I.; Monsecour, M.

1976-01-01

A comparison of instrumental methods, including neutron activation analysis, X-ray fluorescence spectrometry, atomic absorption spectrometry and emission spectrometry, for the analysis of heavy metals in airborne particulate matter is described. The merits and drawbacks of each method for the routine analysis of a large number of samples are discussed. The sample preparation technique, calibration and statistical data relevant to each method are given. Concordant results are obtained by the different methods for Co, Cu, Ni, Pb and Zn. Less good agreement is obtained for Fe, Mn and V. The results are not in agreement for the elements Cd and Cr. Using data obtained on the dust sample distributed by Euratom-ISPRA within the framework of an interlaboratory comparison, the accuracy of each method for the various elements is estimated. Neutron activation analysis was found to be the most sensitive and accurate of the non-destructive analysis methods. Only atomic absorption spectrometry has a comparable sensitivity, but requires considerable preparation work. X-ray fluorescence spectrometry is less sensitive and shows biases for Cr and V. Automatic emission spectrometry with simultaneous measurement of the beam intensities by photomultipliers is the fastest and most economical technique, though at the expense of some precision and sensitivity. (author)

Multi-element fingerprinting as a tool in origin authentication of four east China marine species.

Science.gov (United States)

Guo, Lipan; Gong, Like; Yu, Yanlei; Zhang, Hong

2013-12-01

The contents of 25 elements in 4 types of commercial marine species from the East China Sea were determined by inductively coupled plasma mass spectrometry and atomic absorption spectrometry. The elemental composition was used to differentiate marine species according to geographical origin by multivariate statistical analysis. The results showed that principal component analysis could distinguish samples from different areas and reveal the elements which played the most important role in origin diversity. The established models by partial least squares discriminant analysis (PLS-DA) and by probabilistic neural network (PNN) can both precisely predict the origin of the marine species. Further study indicated that PLS-DA and PNN were efficacious in regional discrimination. The models from these 2 statistical methods, with an accuracy of 97.92% and 100%, respectively, could both distinguish samples from different areas without the need for species differentiation. © 2013 Institute of Food Technologists®

Development of the multitracer technology for a simultaneous multi-elemental analysis and its evolution in RI-beam factory project

International Nuclear Information System (INIS)

Enomoto, Shuichi

2003-01-01

This review describes the method to produce the multitracer, its biobehavior, its application for environmental sciences, Nuclear Energy Fundamentals Crossover Research (for upgrading multitracer production technology, and development of the automatic chemical separation units and of the simultaneous imaging apparatus for multi gamma-ray nuclides), and Inst. of Physical and Chemical Research (RIKEN) RI-beam factory project. The multitracer technology is an efficient (i.e., many information's are available through one experimentation) tracer technique for studying the physical, chemical and biological behavior of elements with use of their multiple radioisotopes produced by accelerators like RIKEN ring cyclotron and of computer/semiconductor detector for their individual gamma-ray spectrometry. The multitracer elements are produced in their carrier-free forms by irradiation of the target element with the heavy particle (up to Ta, in RIKEN cyclotron) and by resultant nuclear fragmentation of the target. The multitracer through nuclear fragmentation and/or fission with an automated separation apparatus will be sophisticatedly supplied in future. GREI (gamma-ray emission imaging) is under investigation. The RI-beam factory project aims to irradiate/accelerate the radioisotope, which is expected to give novel knowledge's in biology like metabolic physiology. (N.I.)

Quantitating subcellular metabolism with multi-isotope imaging mass spectrometry

OpenAIRE

Steinhauser, Matthew L.; Bailey, Andrew; Senyo, Samuel E.; Guillermier, Christelle; Perlstein, Todd S.; Gould, Alex P.; Lee, Richard T.; Lechene, Claude P.

2012-01-01

Mass spectrometry with stable isotope labels has been seminal in discovering the dynamic state of living matter 1,2 but is limited to bulk tissues or cells. We developed multi-isotope imaging mass spectrometry (MIMS) that allowed us to view and measure stable isotope incorporation with sub-micron resolution 3,4 . Here we apply MIMS to diverse organisms, including Drosophila, mice, and humans. We test the “immortal strand hypothesis,” which predicts that during asymmetric stem cell division ch...

Analysis of metal-laden water via portable X-ray fluorescence spectrometry

Science.gov (United States)

Pearson, Delaina; Weindorf, David C.; Chakraborty, Somsubhra; Li, Bin; Koch, Jaco; Van Deventer, Piet; de Wet, Jandre; Kusi, Nana Yaw

2018-06-01

A rapid method for in-situ elemental composition analysis of metal-laden water would be indispensable for studying polluted water. Current analytical lab methods to determine water quality include flame atomic absorption spectrometry (FAAS), atomic absorption spectrophotometry (AAS), electrothermal atomic absorption spectrometry (EAAS), and inductively coupled plasma (ICP) spectroscopy. However only two field methods, colorimetry and absorptiometry, exist for elemental analysis of water. Portable X-ray fluorescence (PXRF) spectrometry is an effective method for elemental analysis of soil, sediment, and other matrices. However, the accuracy of PXRF is known to be affected while scanning moisture-laden soil samples. This study sought to statistically establish PXRF's predictive ability for various elements in water at different concentrations relative to inductively coupled plasma atomic emission spectroscopy (ICP-AES). A total of 390 metal-laden water samples collected from leaching columns of mine tailings in South Africa were analyzed via PXRF and ICP-AES. The PXRF showed differential effectiveness in elemental quantification. For the collected water samples, the best relationships between ICP and PXRF elemental data were obtained for K and Cu (R2 = 0.92). However, when scanning ICP calibration solutions with elements in isolation, PXRF results indicated near perfect agreement; Ca, K, Fe, Cu and Pb produced an R2 of 0.99 while Zn and Mn produced an R2 of 1.00. The utilization of multiple PXRF (stacked) beams produced stronger correlation to ICP relative to the use of a single beam in isolation. The results of this study demonstrated the PXRF's ability to satisfactorily predict the composition of metal-laden water as reported by ICP for several elements. Additionally this study indicated the need for a "Water Mode" calibration for the PXRF and demonstrates the potential of PXRF for future study of polluted or contaminated waters.

A review of modern instrumental methods of elemental analysis of petroleum related material. Part 2

International Nuclear Information System (INIS)

Nadkarni, R.A.

1991-01-01

In this paper a review is presented of the state of the art in elemental analysis of petroleum-related materials (crude oil, gasoline, additives, and lubricants) using modern instrumental analysis techniques. The major instrumental techniques used for elemental analysis of petroleum products include atomic absorption spectrometry (both with flame and with graphite furnace atomizer), inductively coupled plasma atomic emission spectrometry, ion chromatography, microelemental methods, neutron activation, spark source mass spectrometry, and x-ray fluorescence. Each of these techniques is compared for its advantages, disadvantages, and typical applications in the petroleum field

Determination of trace elements in ground water by two preconcentration methods using atomic absorption spectrometry

International Nuclear Information System (INIS)

Elhag, A. Y.

2004-01-01

This is a comparative study between two different methods of preconcentration done to separate the trace elements cadmium, nickel. chromium, manganese, copper, zinc, and lead in drinking (ground) water samples taken from different locations in Gezira State, central Sudan (the map); these methods are (coprecipitation) with aluminium hydroxide and by Ammonium Pyrrolidine Dithiocarbamate (APDC) using Methyl Isobutyl Ketone (MIBK) as an organic solvent; and subsequent analysis by Atomic Absorption Spectrometry (AAS) for both methods. The result of comparison showed the superiority of the (APDC) coprecipitation method over the aluminium hydroxide coprecipitation method in the total percentage recoveries of the studied trace elements in drinking (ground) water samples, such results confirm previous studies. This study also involves direct analysis of these water samples by atomic absorption spectrometry to determine the concentrations of trace elements Cadmium, Nickel, Chromium, Manganese, Copper, Zinc and Lead and compare it to the corresponding guide line values described by the World Health Organization and the maximum concentrations of trace elements in drinking water permitted by the Sudanese Standards and Metrology Organizations (SSMO), where the concentrations of some elements in some samples were found to be different than the described values by both of the organizations. The study includes a trial to throw light on the effect of the proximity of the water samples sources to the Blue Nile river on its trace elements concentrations; no relation was proved to exist in that respect.(Author)

Multi-ingredients determination and fingerprint analysis of leaves from Ilex latifolia using ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

Science.gov (United States)

Fan, Chunlin; Deng, Jiewei; Yang, Yunyun; Liu, Junshan; Wang, Ying; Zhang, Xiaoqi; Fai, Kuokchiu; Zhang, Qingwen; Ye, Wencai

2013-10-01

An ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS) method integrating multi-ingredients determination and fingerprint analysis has been established for quality assessment and control of leaves from Ilex latifolia. The method possesses the advantages of speediness, efficiency, accuracy, and allows the multi-ingredients determination and fingerprint analysis in one chromatographic run within 13min. Multi-ingredients determination was performed based on the extracted ion chromatograms of the exact pseudo-molecular ions (with a 0.01Da window), and fingerprint analysis was performed based on the base peak chromatograms, obtained by negative-ion electrospray ionization QTOF-MS. The method validation results demonstrated our developed method possessing desirable specificity, linearity, precision and accuracy. The method was utilized to analyze 22 I. latifolia samples from different origins. The quality assessment was achieved by using both similarity analysis (SA) and principal component analysis (PCA), and the results from SA were consistent with those from PCA. Our experimental results demonstrate that the strategy integrated multi-ingredients determination and fingerprint analysis using UPLC-QTOF-MS technique is a useful approach for rapid pharmaceutical analysis, with promising prospects for the differentiation of origin, the determination of authenticity, and the overall quality assessment of herbal medicines. Copyright © 2013 Elsevier B.V. All rights reserved.

TXRF, PIXE and EDXRF: a first step towards normalization of x-ray spectrometry for chemical analysis

International Nuclear Information System (INIS)

Barreiros, M.A.; Costa, M.M.; Palha, M.; Pinheiro, T.; Araujo, M.F.; Silva, R.C. da

2000-01-01

Nowadays, many research studies rely on analytical measurements to which x-ray spectrometry techniques are particularly adequate. Because they are multi-elemental, versatile, fast and can reach low detection limits they are often applied to environmental and biomedical studies. Besides, they are able to provide reliable and accurate results. As also occurs with other analytical procedures, the quality assurance for non-routine analysis in R and D laboratories, is much less well established. when compared with routine analytical work. Thus, it is of foremost importance, to set the major quality parameters that significantly affect the quality of results. In addition, there is a need to apply the new concepts of trace ability and uncertainty to these techniques. This work reports on the reliability of TXRF, PIXE and EDXRF measurements by evaluating the uncertainty and trace ability for elemental analysis. The set of experimental and statistical procedures used to ensure the quality of results relative to the proposed objectives, as well as the methods applied to estimate the uncertainties will be presented and discussed. The sample preparation procedures, analytical calibration and spectral evaluation will be the parameters examined in this inter-laboratory study. The sample preparation procedures comprise pressure acid digestion and pelletizing for solid samples. The internal quality control for analytical calibration and spectral analysis is performed using certified reference materials and standard solutions. The goal of this work is to present a first step towards normalization of x-ray spectrometry techniques for chemical analysis. (author)

Analysis of eight argonne premium coal samples by X-ray fluorescence spectrometry

Science.gov (United States)

Evans, J.R.; Sellers, G.A.; Johnson, R.G.; Vivit, D.V.; Kent, J.

1990-01-01

X-ray fluorescence spectrometric methods were used in the analysis of eight Argonne Premium Coal Samples. Trace elements (Cr, Ni, Cu, Zn, Rb, Sr, Y, Zr, Nb, Ba, La, and Ce) in coal ash were determined by energy-dispersive X-ray fluorescence spectrometry; major elements (Na, Mg, Al, Si, P, S, K, Ca, Ti, Mn, and Fe) in coal ash and trace elements (Cl and P) in whole coal were determined by wavelength-dispersive X-ray fluorescence spectrometry. The results of this study will be used in a geochemical database compiled for these materials from various analytical techniques. The experimental XRF methods and procedures used to determine these major and trace elements are described.

Traceability of Opuntia ficus-indica L. Miller by ICP-MS multi-element profile and chemometric approach.

Science.gov (United States)

Mottese, Antonio Francesco; Naccari, Clara; Vadalà, Rossella; Bua, Giuseppe Daniel; Bartolomeo, Giovanni; Rando, Rossana; Cicero, Nicola; Dugo, Giacomo

2018-01-01

Opuntia ficus-indica L. Miller fruits, particularly 'Ficodindia dell'Etna' of Biancavilla (POD), 'Fico d'india tradizionale di Roccapalumba' with protected brand and samples from an experimental field in Pezzolo (Sicily) were analyzed by inductively coupled plasma mass spectrometry in order to determine the multi-element profile. A multivariate chemometric approach, specifically principal component analysis (PCA), was applied to individuate how mineral elements may represent a marker of geographic origin, which would be useful for traceability. PCA has allowed us to verify that the geographical origin of prickly pear fruits is significantly influenced by trace element content, and the results found in Biancavilla PDO samples were linked to the geological composition of this volcanic areas. It was observed that two principal components accounted for 72.03% of the total variance in the data and, in more detail, PC1 explains 45.51% and PC2 26.52%, respectively. This study demonstrated that PCA is an integrated tool for the traceability of food products and, at the same time, a useful method of authentication of typical local fruits such as prickly pear. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Inorganic trace analysis by laser ionization mass spectrometry

International Nuclear Information System (INIS)

Becker, S.; Dietze, H.J.

1991-01-01

Among the different spectrometric techniques for trace analysis Laser Ionization Mass Spectrometry (LIMS) is well established as a trace analytic method with a wide coverage. In the LIMS the sample material is evaporated and ionized by means of a focused pulsed laser beam in a laser microplasma, which is formed in the spot area of the irradiated sample. All chemical elements in the sample materials are evaporated and ionized in the laser plasma. The formed ions are separated according to mass and energy by a time-of-flight, quadrupole or double focusing mass spectrometer. In this review the characteristics and analytical features, some recent developments, and applications of laser ionization mass spectrometry in inorganic trace analysis are described. (orig.)

Laser ionization mass spectrometry in inorganic trace analysis

International Nuclear Information System (INIS)

Becker, J.S.; Dietze, H.J.

1992-01-01

Among the different spectrometric techniques for trace analysis Laser Ionization Mass Spectrometry (LIMS) is well established as a trace analytical method. With the LIMS technique the sample material is evaporated and ionized by means of a focused pulsed laser in a laser microplasma, which is formed in the spot area of the irradiated sample. All chemical elements in the sample materials are evaporated and ionized in the laser plasma. The ions formed are separated according to their mass and energy by a time-of-flight, quadrupole or double focusing mass spectrometer. In this review the characteristics and analytical features, some recent developments and applications of laser ionization mass spectrometry in inorganic trace analysis are described. (orig.)

Burnup determination of power reactor fuel elements by gamma spectrometry; Determination par spectrometrie {gamma} du taux d'irradiation des elements combustibles des reacteurs de puissance

Energy Technology Data Exchange (ETDEWEB)

Robin, M; Jastrzeb, M; Boisliveau, S; Boyer, R; Vidal, R [Commissariat a l' Energie Atomique, Fontenay-aux-Roses (France). Centre d' Etudes Nucleaires

1969-07-01

This report describes a method for determining by {gamma} spectrometry the burn up and the specific power of fuel elements irradiated in power reactors. The energy spectrum of {gamma} rays emitted by fission products is measured by means of a simple equipment using a sodium iodide detector and a multichannel analyzer. In order to extract from the spectrum a quantity proportional to the burn up, it is necessary to: - isolate an activity specific of one emitter,- give the same importance to fissions in uranium and plutonium - take into account the radioactive decay during and after irradiation. One hundred fuel elements were studied and burn up values obtained by {gamma} spectrometry are compared to results given by chemical analyses. Preliminary measurements show that the accuracy of the results is greatly increased by the use of a germanium detector, due to its good resolution. (authors) [French] Ce rapport expose une methode de determination par spectrometrie {gamma} du taux d'irradiation et de la puissance specifique des elements combustibles irradies dans les reacteurs de puissance. Une installation simple utilisant un detecteur d'iodure de sodium et un selecteur multicanaux mesure le spectre en energie du rayonnement {gamma} emis par les produits de fission. Afin d'extraire du spectre une quantite proportionnelle au taux de combustion, il faut: - isoler une activite specifique a un emetteur, - donner la meme importance aux fissions survenues dans l'uranium et le plutonium, - prendre en compte la decroissance radioactive pendant et apres l'irradiation. Les mesures ont porte sur une centaine d'elements combustibles et les taux de combustion obtenus par spectrometrie {gamma} sont compares aux resultats des analyses chimiques. Des mesures preliminaires montrent que l'utilisation d'un detecteur de germanium augmente considerablement la precision des resultats, en raison de son excellente resolution. (auteurs)

The chemical speciation and analysis of trace elements in sediment with Neutron Activation Analytical method(NAA) and atomic mass spectrometry

International Nuclear Information System (INIS)

Nam, Sang-Ho; Kim, Jae-Jin; Chung, Yong-Sam; Kim, Sun-Ha

2003-01-01

In this research, first of all, the analytical methods for the determination of major elements in sediment have been developed with ICP-MS (Inductively Coupled Plasma Mass Spectrometry). The analytical results of major elements (Al, Ca, K, Fe, Mg) with Cool ICP-MS were much better than those with normal ICP-MS. The analytical results were compared with those of NAA (Neutron Activation Analysis). NAA were a little superior to ICP-MS for the determination of major elements in sediment as a non-destructive trace analytical trace analytical method. The analytical methods for the determination of minor elements (Cr, Ce, U, Co, Pb, As, Se) have been also developed with ICP-MS. The analytical results by standard calibration curve with ICP-MS were not accurate due to the matrix interferences. Thus, the internal standard method was applied, then the analytical results for minor elements with ICP-MS were greatly improved. The analytical results obtained by ICP-MS were compared with those obtained by NAA. It showed that the two analytical methods have great capabilities for the determination of minor elements in sediments. Accordingly, the NAA will plan an important role in analysis of environment sample with complex matrix. ICP-MS also will play an important role because it has a great capability for the determination of Pb that could not be determined by NAA

The determination of the C, N, O and trace element content of Triticum aestivum by activation analysis, X-ray excitation and mass spectrometry

International Nuclear Information System (INIS)

Leonhardt, J.W.; Dahn, E.; Dietze, H.J.; Freyer, K.; Geisler, M.; Hartmann, G.; Jung, K.; Schelhorn, H.

1979-01-01

The results of determinations of the C, N, O and trace element content of grains, sprouts and leaves of Triticum aestivum by means of various methods of activation analysis, X-ray excitation and mass spectrometry are presented. The C and O contents were determined by X-ray excitation; the O, N, P and Si contents were measured by NAA with 14-MeV neutrons, and the trace elements were determined by NAA with thermal neutrons. A mass-spectrometric survey analysis confirmed the results obtained by NAA. The use of neutron-induced nuclear reactions together with autoradiography enabled a representative picture to be formed of the spatial distribution in two dimensions of 14 N in biological specimens. (author)

Atomic spectrometry methods for wine analysis: A critical evaluation and discussion of recent applications

Energy Technology Data Exchange (ETDEWEB)

Grindlay, Guillermo, E-mail: guillermo.grindlay@ua.es [Department of Analytical Chemistry, Nutrition and Food Sciences, University of Alicante, PO Box 99, 03080 Alicante (Spain); Mora, Juan; Gras, Luis [Department of Analytical Chemistry, Nutrition and Food Sciences, University of Alicante, PO Box 99, 03080 Alicante (Spain); Loos-Vollebregt, Margaretha T.C. de [Delft University of Technology, Faculty of Applied Sciences, Analytical Biotechnology, Julianalaan 67, 2628 BC Delft (Netherlands)

2011-04-08

The analysis of wine is of great importance since wine components strongly determine its stability, organoleptic or nutrition characteristics. In addition, wine analysis is also important to prevent fraud and to assess toxicological issues. Among the different analytical techniques described in the literature, atomic spectrometry has been traditionally employed for elemental wine analysis due to its simplicity and good analytical figures of merit. The scope of this review is to summarize the main advantages and drawbacks of various atomic spectrometry techniques for elemental wine analysis. Special attention is paid to interferences (i.e. matrix effects) affecting the analysis as well as the strategies available to mitigate them. Finally, latest studies about wine speciation are briefly discussed.

Atomic spectrometry methods for wine analysis: A critical evaluation and discussion of recent applications

International Nuclear Information System (INIS)

Grindlay, Guillermo; Mora, Juan; Gras, Luis; Loos-Vollebregt, Margaretha T.C. de

2011-01-01

The analysis of wine is of great importance since wine components strongly determine its stability, organoleptic or nutrition characteristics. In addition, wine analysis is also important to prevent fraud and to assess toxicological issues. Among the different analytical techniques described in the literature, atomic spectrometry has been traditionally employed for elemental wine analysis due to its simplicity and good analytical figures of merit. The scope of this review is to summarize the main advantages and drawbacks of various atomic spectrometry techniques for elemental wine analysis. Special attention is paid to interferences (i.e. matrix effects) affecting the analysis as well as the strategies available to mitigate them. Finally, latest studies about wine speciation are briefly discussed.

Analysis of some metallic elements and metalloids composition and relationships in parasol mushroom Macrolepiota procera.

Science.gov (United States)

Falandysz, Jerzy; Sapkota, Atindra; Dryżałowska, Anna; Mędyk, Małgorzata; Feng, Xinbin

2017-06-01

The aim of the study was to characterise the multi-elemental composition and associations between a group of 32 elements and 16 rare earth elements collected by mycelium from growing substrates and accumulated in fruiting bodies of Macrolepiota procera from 16 sites from the lowland areas of Poland. The elements were quantified by inductively coupled plasma quadrupole mass spectrometry using validated method. The correlation matrix obtained from a possible 48 × 16 data matrix has been used to examine if any association exits between 48 elements in mushrooms foraged from 16 sampling localizations by multivariate approach using principal component (PC) analysis. The model could explain up to 93% variability by eight factors for which an eigenvalue value was ≥1. Absolute values of the correlation coefficient were above 0.72 (significance at p < 0.05) for 43 elements. From a point of view by consumer, the absolute content of Cd, Hg, Pb in caps of M. procera collected from background (unpolluted) areas could be considered elevated while sporadic/occasional ingestion of this mushroom is considered safe. The multivariate functional analysis revealed on associated accumulation of many elements in this mushroom. M. procera seem to possess some features of a bio-indicative species for anthropogenic Pb but also for some geogenic metals.

Alternative approaches to correct interferences in the determination of boron in shrimps by electrothermal atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Pasias, I.N.; Pappa, Ch.; Katsarou, V.; Thomaidis, N.S., E-mail: ntho@chem.uoa.gr; Piperaki, E.A.

2014-02-01

The aim of this study is to propose alternative techniques and methods in combination with the classical chemical modification to correct the major matrix interferences in the determination of boron in shrimps. The performance of an internal standard (Ge) for the determination of boron by the simultaneous multi-element atomic absorption spectrometry was tested. The use of internal standardization increased the recovery from 85.9% to 101% and allowed a simple correction of errors during sampling preparation and heating process. Furthermore, a new preparation procedure based on the use of citric acid during digestion and dilution steps improved the sensitivity of the method and decreased the limit of detection. Finally, a comparative study between the simultaneous multi-element atomic absorption spectrometry with a longitudinal Zeeman-effect background correction system, equipped with a transversely-heated graphite atomizer and the single element atomic absorption spectrometry with a D{sub 2} background correction system, equipped with an end-heated graphite atomizer was undertaken to investigate the different behavior of boron in both techniques. Different chemical modifiers for the determination of boron were tested with both techniques. Ni-citric acid and Ca were the optimal chemical modifiers when simultaneous multi-element atomic absorption spectrometry and single-element atomic absorption spectrometry were used, respectively. By using the single-element atomic absorption spectrometry, the calculated characteristic mass was 220 pg and the calculated limit of detection was 370 μg/kg. On the contrary, with simultaneous multi-element atomic absorption spectrometry, the characteristic mass was 2200 pg and the limit of detection was 5.5 mg/kg. - Highlights: • New approaches were developed to cope with interferences of B determination by ETAAS • Ge was used as internal standard for the determination of B by simultaneous ETAAS • Citric acid was used during

Elemental labelling combined with liquid chromatography inductively coupled plasma mass spectrometry for quantification of biomolecules: A review

International Nuclear Information System (INIS)

Kretschy, Daniela; Koellensperger, Gunda; Hann, Stephan

2012-01-01

Highlights: ► Survey of bio-analytical approaches utilizing biomolecule labelling. ► Detailed discussion of methodology and chemistry of elemental labelling. ► Biomedical and bio-analytical applications of elemental labelling. ► FI-ICP-MS and LC–ICP-MS for quantification of elemental labelled biomolecules. ► Review of selected applications. - Abstract: This article reviews novel quantification concepts where elemental labelling is combined with flow injection inductively coupled plasma mass spectrometry (FI-ICP-MS) or liquid chromatography inductively coupled plasma mass spectrometry (LC–ICP-MS), and employed for quantification of biomolecules such as proteins, peptides and related molecules in challenging sample matrices. In the first sections an overview on general aspects of biomolecule quantification, as well as of labelling will be presented emphasizing the potential, which lies in such methodological approaches. In this context, ICP-MS as detector provides high sensitivity, selectivity and robustness in biological samples and offers the capability for multiplexing and isotope dilution mass spectrometry (IDMS). Fundamental methodology of elemental labelling will be highlighted and analytical, as well as biomedical applications will be presented. A special focus will lie on established applications underlining benefits and bottlenecks of such approaches for the implementation in real life analysis. Key research made in this field will be summarized and a perspective for future developments including sophisticated and innovative applications will given.

Determination of aluminium, scandium and rare earth elements by emission flame spectrometry

International Nuclear Information System (INIS)

Otruba, V.; Sommer, L.

1989-01-01

Emission spectrometry in nitrous oxide-acetylene flames in combination with a highly resolving double monochromator and sensitive detecting system enables simple, sensitive and selective determinations of aluminium, scandium and all rare earth elements with exception of cerium in complicated matrices. Calibration plots are linear for a large concentration interval (≤ 100 μgxml -1 ), detection limits are in ngxml -1 level and RSD does not exceed 3% on the optimal concentration level of the particular element. The determination of Al, Sc, Eu and Yb showed particular advantages as to methods using ICP-spectrometry. (orig.)

Detailed Modeling and Irreversible Transfer Process Analysis of a Multi-Element Thermoelectric Generator System

Science.gov (United States)

Xiao, Heng; Gou, Xiaolong; Yang, Suwen

2011-05-01

Thermoelectric (TE) power generation technology, due to its several advantages, is becoming a noteworthy research direction. Many researchers conduct their performance analysis and optimization of TE devices and related applications based on the generalized thermoelectric energy balance equations. These generalized TE equations involve the internal irreversibility of Joule heating inside the thermoelectric device and heat leakage through the thermoelectric couple leg. However, it is assumed that the thermoelectric generator (TEG) is thermally isolated from the surroundings except for the heat flows at the cold and hot junctions. Since the thermoelectric generator is a multi-element device in practice, being composed of many fundamental TE couple legs, the effect of heat transfer between the TE couple leg and the ambient environment is not negligible. In this paper, based on basic theories of thermoelectric power generation and thermal science, detailed modeling of a thermoelectric generator taking account of the phenomenon of energy loss from the TE couple leg is reported. The revised generalized thermoelectric energy balance equations considering the effect of heat transfer between the TE couple leg and the ambient environment have been derived. Furthermore, characteristics of a multi-element thermoelectric generator with irreversibility have been investigated on the basis of the new derived TE equations. In the present investigation, second-law-based thermodynamic analysis (exergy analysis) has been applied to the irreversible heat transfer process in particular. It is found that the existence of the irreversible heat convection process causes a large loss of heat exergy in the TEG system, and using thermoelectric generators for low-grade waste heat recovery has promising potential. The results of irreversibility analysis, especially irreversible effects on generator system performance, based on the system model established in detail have guiding significance for

Quantitative imaging of subcellular metabolism with stable isotopes and multi-isotope imaging mass spectrometry

Science.gov (United States)

Steinhauser, Matthew L.; Lechene, Claude P.

2014-01-01

Multi-isotope imaging mass spectrometry (MIMS) is the quantitative imaging of stable isotope labels in cells with a new type of secondary ion mass spectrometer (NanoSIMS). The power of the methodology is attributable to (i) the immense advantage of using non-toxic stable isotope labels, (ii) high resolution imaging that approaches the resolution of usual transmission electron microscopy and (iii) the precise quantification of label down to 1 part-per-million and spanning several orders of magnitude. Here we review the basic elements of MIMS and describe new applications of MIMS to the quantitative study of metabolic processes including protein and nucleic acid synthesis in model organisms ranging from microbes to humans. PMID:23660233

Atomic spectrometry methods for wine analysis: a critical evaluation and discussion of recent applications.

Science.gov (United States)

Grindlay, Guillermo; Mora, Juan; Gras, Luis; de Loos-Vollebregt, Margaretha T C

2011-04-08

The analysis of wine is of great importance since wine components strongly determine its stability, organoleptic or nutrition characteristics. In addition, wine analysis is also important to prevent fraud and to assess toxicological issues. Among the different analytical techniques described in the literature, atomic spectrometry has been traditionally employed for elemental wine analysis due to its simplicity and good analytical figures of merit. The scope of this review is to summarize the main advantages and drawbacks of various atomic spectrometry techniques for elemental wine analysis. Special attention is paid to interferences (i.e. matrix effects) affecting the analysis as well as the strategies available to mitigate them. Finally, latest studies about wine speciation are briefly discussed. Copyright © 2011 Elsevier B.V. All rights reserved.

Trace element determination using static high-sensitivity inductively coupled plasma optical emission spectrometry (SHIP-OES).

Science.gov (United States)

Engelhard, Carsten; Scheffer, Andy; Nowak, Sascha; Vielhaber, Torsten; Buscher, Wolfgang

2007-02-05

A low-flow air-cooled inductively coupled plasma (ICP) design for optical emission spectrometry (OES) with axial plasma viewing is described and an evaluation of its analytical capabilities in trace element determinations is presented. Main advantage is a total argon consumption of 0.6 L min(-1) in contrast to 15 L min(-1) using conventional ICP sources. The torch was evaluated in trace element determinations and studied in direct comparison with a conventional torch under the same conditions with the same OES system, ultrasonic nebulization (USN) and single-element optimization. A variety of parameters (x-y-position of the torch, rf power, external air cooling, gas flow rates and USN operation parameters) was optimized to achieve limits of detection (LOD) which are competitive to those of a conventional plasma source. Ionic to atomic line intensity ratios for magnesium were studied at different radio frequency (rf) power conditions and different sample carrier gas flows to characterize the robustness of the excitation source. A linear dynamic range of three to five orders of magnitude was determined under compromise conditions in multi-element mode. The accuracy of the system was investigated by the determination of Co, Cr, Mn, Zn in two certified reference materials (CRM): CRM 075c (Copper with added impurities), and CRM 281 (Trace elements in rye grass). With standard addition values of 2.44+/-0.04 and 3.19+/-0.21 microg g(-1) for Co and Mn in the CRM 075c and 2.32+/-0.09, 81.8+/-0.4, 32.2+/-3.9 for Cr, Mn and Zn, respectively, were determined in the samples and found to be in good agreement with the reported values; recovery rates in the 98-108% range were obtained. No influence on the analysis by the matrix load in the sample was observed.

Determination of elemental composition of metals using ambient organic mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Shiea, Christopher [Department of Medical Laboratory Science and Biotechnology, Kaohsiung Medical University, 100 Shih-Chuan 1st Rd, Kaohsiung 807, Taiwan (China); Huang, Yeou-Lih [Department of Medical Laboratory Science and Biotechnology, Kaohsiung Medical University, 100 Shih-Chuan 1st Rd, Kaohsiung 807, Taiwan (China); Department of Chemistry, National Sun Yat-Sen University, 70 Lien-Hai Rd, Kaohsiung 804, Taiwan (China); Cheng, Sy-Chyi; Chen, Yi-Lun [Department of Chemistry, National Sun Yat-Sen University, 70 Lien-Hai Rd, Kaohsiung 804, Taiwan (China); Shiea, Jentaie, E-mail: jetea@mail.nsysu.edu.tw [Department of Chemistry, National Sun Yat-Sen University, 70 Lien-Hai Rd, Kaohsiung 804, Taiwan (China); Department of Medicinal and Applied Chemistry, Kaohsiung Medical University, 100 Shih-Chuan 1st Rd, Kaohsiung 807, Taiwan (China)

2017-05-22

Conventional inorganic mass spectrometric (MS) analysis of metals can require time-consuming and tedious sample preparation. We thus report the novel and direct characterization of metals in solid samples using an organic MS technique known as electrospray laser desorption ionization mass spectrometry (ELDI/MS). No sample pretreatment was needed, and results were rapidly obtained due to the ambient and laser-based nature of ELDI/MS. Metals from samples were desorbed and ionized by laser irradiation, after which they reacted with EDTA and then post-ionized and detected as metal-EDTA complexes. Aluminum, copper, iron, lead, nickel, and zinc from plates, foils, and coins were characterized in seconds. This study demonstrates that an ESI/MS system can be easily modified to analyze metal elements in solids by involving a chelating agent, indicating a potentially promising development in MS towards the analysis of metals using organic MS. - Highlights: • “Organic MS” was utilized as “inorganic MS” to detect metal ions in solid samples. • Element ions desorbed by laser irradiation rapidly reacted with a chelating reagent before they were detected by MS. • Elemental composition of metals was determined by this “Organic MS” method.

Determination of elemental composition of metals using ambient organic mass spectrometry

International Nuclear Information System (INIS)

Shiea, Christopher; Huang, Yeou-Lih; Cheng, Sy-Chyi; Chen, Yi-Lun; Shiea, Jentaie

2017-01-01

Conventional inorganic mass spectrometric (MS) analysis of metals can require time-consuming and tedious sample preparation. We thus report the novel and direct characterization of metals in solid samples using an organic MS technique known as electrospray laser desorption ionization mass spectrometry (ELDI/MS). No sample pretreatment was needed, and results were rapidly obtained due to the ambient and laser-based nature of ELDI/MS. Metals from samples were desorbed and ionized by laser irradiation, after which they reacted with EDTA and then post-ionized and detected as metal-EDTA complexes. Aluminum, copper, iron, lead, nickel, and zinc from plates, foils, and coins were characterized in seconds. This study demonstrates that an ESI/MS system can be easily modified to analyze metal elements in solids by involving a chelating agent, indicating a potentially promising development in MS towards the analysis of metals using organic MS. - Highlights: • “Organic MS” was utilized as “inorganic MS” to detect metal ions in solid samples. • Element ions desorbed by laser irradiation rapidly reacted with a chelating reagent before they were detected by MS. • Elemental composition of metals was determined by this “Organic MS” method.

Application of neutron activation analysis and inductively coupled plasma mass spectrometry to the determination of toxic and essential elements in Australian foods

International Nuclear Information System (INIS)

Fardy, J.J.; McOrist, G.D.; Bowles, C.J.; Farrar, Y.J.; Warner, I.M.

1990-01-01

Current Australian legislation specifies the maximum permitted levels of nine toxic elements in foods while the National Health and Medical Research Council (NH and NRC) has listed recommended daily intake figures for seven essential elements. This investigation examined the compliance of Australian foods with both these requirements. Australia-wide samples of representative foods from the diets of Australians were used in this study after the NH and NRC kindly permitted us to join their Market Basket (Noxious Substance) Survey. Both toxic and essential element concentrations in these foods were determined using the advanced analytical techniques of instrumental and radiochemical neutron activation analysis and inductively coupled plasma mass spectrometry. With very few exceptions foods do not exceed the maximum, permitted levels for toxic substances. Daily intake figures for essential elements generally lie close to the maximum recommended values listed by NH and NRC. (author). 11 refs, 22 figs, 17 tabs

Analysis of soils by glow discharge mass spectrometry

International Nuclear Information System (INIS)

Duckworth, D.C.; Barshick, C.M.; Smith, D.H.

1993-01-01

The analysis of soils by conventional solution-based techniques, such as inductively coupled plasma and thermal ionization mass spectrometry, is complicated by the need for sample dissolution or the combination of a solids atomizer with an auxiliary ionization source. Since time is an important consideration in waste remediation, there exists a need for a method of rapidly analysing many soil samples with little sample preparation; glow discharge mass spectrometry (GDMS) has the potential to meet this need. Because GDMS is a bulk solids technique, sample preparation is simplified in comparison to other methods. Even with the most difficult samples (geological materials, such as soils and volcanic rock), all that is required is grinding, drying and mixing with a conducting host material prior to electrode formation. As a first test of GDMS for soil analysis, a National Institute of Standards and Technology (NIST) Standard Reference Material (SRM) was analysed by direct current GDMS. Fifty-one elements were quantified from a single cathode using ion beam ratios and ''standard'' relative elemental sensitivity factors (RSF). Average errors for the suite of elements were less than a factor of 4 and 1.4 for uncorrected and corrected values, respectively. User-generated RSF values were applied to the analysis of several elements in NIST SRM 2704 Buffalo River Sediment. In the absence of isobaric interferences, accuracies ranging from 0.6 to 73% were observed, demonstrating the potential of the technique for the determination of many elements. The presence of entrained water and inhomogeneity resulting from cathode preparation is thought to affect matrix-to-matrix reproducibility. While further success depends on developing means of circumventing mass spectral interferences and addressing factors affecting plasma chemistry, the immediate goal of developing a screening method for priority metals in soils was met. (Author)

Liquid phase microextraction for the analysis of trace elements and their speciation

International Nuclear Information System (INIS)

Hu, Bin; He, Man; Chen, Beibei; Xia, Linbo

2013-01-01

Trace/ultra-trace elements and their speciation analysis in complex matrices usually require sample preparation procedures to achieve sample clean-up and analyte preconcentration. Sample preparation is often the bottleneck in trace elements and their speciation analysis which has a direct impact on accuracy, precision and limits of detection and is often the rate-determining step of the analytical process. Recent trends in sample preparation include miniaturization, automation, high-throughput performance and reduction in solvent/sample consumption and operation time. Liquid-phase microextraction (LPME) technique as a novel and promising alternative in sample preparation can meet these requirements and has become a very efficient sample preparation technique. This review updates the state of art of LPME for trace elements and their speciation analysis and discusses its promising prospects. The major thrust of the article highlights the applications of LPME including single-drop microextraction (SDME), hollow fiber-liquid phase microextraction (HF-LPME), dispersive liquid liquid microextraction (DLLME) and solidified floating organic drop microextraction (SFODME) to the fields of elemental and their speciation analysis by atomic spectrometry-based methods, especially inductively coupled plasma mass spectrometry. General and specific concepts, different extraction formats and characteristics of LPME are described and compared, along with examples of recent innovations and applications presented to demonstrate its potential for trace elements and their speciation analysis in biological and environmental fields. Moreover, the application potential and an outlook on the combination of LPME and atomic spectrometry-based techniques for inorganic analysis are commentated. - Highlights: • The state of art of LPME for trace elements and their speciation analysis is updated. • Different extraction formats of LPME are described. • The application potential and future

Effects of Heat Input and Bead Generation Methods on Finite Element Analysis of Multi-Pass Welding Process

Energy Technology Data Exchange (ETDEWEB)

Park, Won Dong; Kim, Ji Hoon; Bahn, Chi Bum [Pusan National University, Busan (Korea, Republic of)

2016-10-15

Welding residual stresses are determined by various factors such as heat input, initial temperature of molten bead, heating time, cooling time, cooling conditions, and boundary conditions. In this study, a sensitivity analysis was performed to find the major factors and reasonable assumptions for simulation. Two-dimensional axisymmetric simulation was conducted by using commercial finite element analysis program ABAQUS, for multi-pass Alloy 82 welds in a 304 Stainless Steel and SA-105 Carbon Steel. The major object is to evaluate effects of the heat input methods and weld bead generation methods on the welding residual stress distribution. Totally four kinds of methods were compared. From the previous results, we could make the following conclusions. 1. Although there are non-negligible differences in HAZ depending on heat input method, welding residual stress distributions have roughly similar trends. However, it is needed to perform the more exact analysis to apply heat energy more carefully into the individual bead. 2. Residual stress distribution were similar for the two weld bead generation technique. However, overlapping was happened when element birth technique was applied. Effects of overlapping could not ignore as deformation increases. However, overlapping problem was avoided when quiet element technique was used. 3. Since existence of inactive bead elements, inaccurate weld residual stresses could be occurred in boundaries of previous and next weld elements in case of quiet element technique.

Rapid methods for multi-elemental X-ray fluorescence analysis using excitation isotope sources and Si(Li)-semiconductor detector

International Nuclear Information System (INIS)

Zhuravleva, E.L.

1980-01-01

Some rapid methods using an unique calibration curve have been developed for multi-elemental X-ray fluorescence analysis of thin and thick layers of various samples having low contents of heavy elements. The matrix absorption effect in thick samples is taken into account according to the scattered radiation.The similar method using a unique calibration curve for determination of low contents of trace elements in thin layers without account of matrix effect is proposed. The results on the intercomposition run soil-5 are in good agreement with the data obtained in different laboratories. The errors of the method are 10 %; in a case of peak superposition - 15 %

Wideband multi-element Er-doped fiber amplifier

International Nuclear Information System (INIS)

Thipparapu, N K; Jain, S; May-Smith, T C; Sahu, J K

2014-01-01

A multi-element Er-doped fiber amplifier (MEEDFA) is demonstrated in which the gain profile is extended into the S and L bands. Each fiber element of the MEEDFA is found to provide a maximum gain of 37 dB and a noise figure of < 4 dB in the C-band. The gain profile of the amplifier is shifted towards longer wavelength by cascading fiber elements. The novel geometry of the multi-element fiber (MEF) could allow for the development of a broadband amplifier in a split-band configuration. The proposed amplifier can operate in the wavelength band of 1520 to 1595 nm (75 nm), with a minimum gain of 20 dB. (letter)

Novel product ions of 2-aminoanilide and benzimidazole Ag(I) complexes using electrospray ionization with multi-stage tandem mass spectrometry.

Science.gov (United States)

Johnson, Byron S; Burinsky, David J; Burova, Svetlana A; Davis, Roman; Fitzgerald, Russ N; Matsuoka, Richard T

2012-05-15

The 2-aminoaniline scaffold is of significant value to the pharmaceutical industry and is embedded in a number of pharmacophores including 2-aminoanilides and benzimidazoles. A novel application of coordination ion spray mass spectrometry (CIS-MS) for interrogating the silver ion (Ag(+)) complexes of a homologous series of these compounds using multi-stage tandem mass spectrometry is described. Unlike the ubiquitous alkali metal ion complexes, Ag(+) complexes of 2-aminoanilides and benzimidazoles were found to yield [M - H](+) ions in significant abundance via gas-phase elimination of the metal hydride (AgH) resulting in unique product ion cascades. Sample introduction was by liquid chromatography with mass spectrometry analysis performed on a hybrid linear ion trap/orbitrap instrument capable of high-resolution measurements. Rigorous structural characterization by multi-stage tandem mass spectrometry using [M +  H](+), [M - H](-) and [M - H](+) precursor ions derived from ESI and CIS experiments was performed for the homologous series of 2-aminoanilide and benzimidazole compounds. A full tabular comparison of structural information resulting from these product ion cascades was produced. Multi-stage tandem mass spectrometry of [M - H](+) ions resulting from Ag(+) complexes of 2-aminoanilides and benzimidazoles in CIS-MS experiments produced unique product ion cascades that exhibited complementary structural information to that obtained from tandem mass spectrometry of [M  +  H](+) and [M - H](-) ions by electrospray ionization (ESI). These observations may be broadly applicable to other compounds that are observed to form Ag(+) complexes and eliminate AgH. Copyright © 2012 John Wiley & Sons, Ltd.

Analysis of heavy metals and minerals elements in the turmeric using Total-Reflection X-ray Fluorescence analysis technique and Atomic Absorption Spectrometry

International Nuclear Information System (INIS)

Andriamisetra, V.M.Z.

2014-01-01

Currently, many studies demonstrate anti-cancer and anti-inflammatory benefits of turmeric. The aims of this work is to perform analysis of metals such as calcium, chromium, manganese, iron, cobalt, nickel, copper, zinc, arsenic, bromine, rubidium, strontium, cadmium and lead in the turmeric collected from various places in Madagascar. The analysis by total reflection X-ray fluorescence technique is used to determine the concentrations of heavy metals, while the atomic absorption spectrometry is used for the determination of trace elements. Analysis results show that the concentration of calcium in the turmeric is very high, its average concentration is 1025.8 mg.kg -1 . The average concentrations of manganese, of copper and of iron are respectively 44.7 mg.kg -1 ; 19.7 mg.kg -1 and 53.6 mg.kg -1 . The average concentrations of zinc, of rubidium and of strontium are respectively 17.3 mg.kg -1 ; 35.2 mg.kg -1 and 21.7 mg.kg -1 [fr

The X-ray spectrometry Si(Li) system and it's application in quantitative analysis of rare-earth elements

International Nuclear Information System (INIS)

Barbosa, J.B.S.

1985-11-01

The basic principles involved in Si(Li) system used in X-ray spectrometry is described. It also demonstrates its application in the energy range where the resolution is better than that characteristic of conventional spectrometers. The theoretical principles underlying the interaction between the electromagnetic radiation and matter, and a review on semiconductors are presented at first. It emphasizes the fluorescence phenomenon and the process of photon detection by semiconductor crystals whose properties and characteristics allow, in the specific case of Si-crystal, the confection of detectors with large sensitivity volume useful for X-ray spectrometry. In addition, the components of the Si(Li) system are described individually, with special attention to the operating aspects, and to the parameters affecting the quality of pulse height spectrum. Finally, the spectrometer performance is experimentally evaluated though the quantitative analyses of rare-earth element oxides (La, Ce, Pr, Nd). It should be stressed that this research indicates that the X-ray emission-transmission analysis is the most adequate method under the activation conditions provided by the spectrometer, where Am 241 emissor UPSILON of 60KeV is the photon source for the fluorescence. Therefore, the experimental work was extended in order to include all the necessary treatment. (Author) [pt

X-ray fluorescence spectrometry and related techniques an introduction

CERN Document Server

Margui, Eva

2013-01-01

X-ray fluorescence spectrometry (XRF) is a well-established analytical technique for qualitative and quantitative elemental analysis of a wide variety of routine quality control and research samples. Among its many desirable features, it delivers true multi-element character analysis, acceptable speed and economy, easy of automation, and the capacity to analyze solid samples. This remarkable contribution to this field provides a comprehensive and up-to-date account of basic principles, recent developments, instrumentation, sample preparation procedures, and applications of XRF analysis. If you are a professional in materials science, analytic chemistry, or physics, you will benefit from not only the review of basics, but also the newly developed technologies with XRF. Those recent technological advances, including the design of low-power micro- focus tubes and novel X-ray optics and detectors, have made it possible to extend XRF to the analysis of low-Z elements and to obtain 2D or 3D information on a microme...

Analysis of trace elements in opal using PIXE

Energy Technology Data Exchange (ETDEWEB)

Hinrichs, Ruth, E-mail: ruth.hinrichs@ufrgs.br [Instituto de Geociências, Universidade Federal do Rio Grande do Sul, Porto Alegre, RS (Brazil); Programa de Pós-graduação em Física, UFRGS, Porto Alegre, RS (Brazil); Bertol, A.P.L. [Programa de Pós-graduação em Física, UFRGS, Porto Alegre, RS (Brazil); Vasconcellos, M.A.Z. [Programa de Pós-graduação em Física, UFRGS, Porto Alegre, RS (Brazil); Instituto de Física, UFRGS, Porto Alegre, RS (Brazil)

2015-11-15

Particle induced X-ray emission (PIXE) analysis is particularly important for the analysis of trace elements of precious samples, being one of the few methods to determine elements with ppm concentration that does not affect sample integrity. A PIXE methodology for trace element analysis in opal was developed. To avoid detector count saturation due to the high number of Si-Kα X-rays generated in the sample, several filters were employed to optimize the reduction of the Si-Kα signal, while maintaining acceptable intensities of the other relevant X-ray lines. Two proton beam energies were tested, to establish the signal to noise ratio in different X-ray energies. Spectra were fitted with the software GUPIX, using a matrix composition determined with electron beam excited energy dispersive X-ray spectrometry. Above the energy of the silicon X-ray, several trace elements were quantified.

Analysis of TRU waste for RCRA-listed elements

International Nuclear Information System (INIS)

Mahan, C.; Gerth, D.; Yoshida, T.

1996-01-01

Analytical methods for RCRA listed elements on Portland cement type waste have been employed using both microwave and open hot plate digestions with subsequent analysis by inductively coupled plasma atomic emission spectroscopy (ICP-AES), inductively coupled plasma mass spectrometry (ICP-AES), inductively coupled plasma mass spectrometry (ICP-MS), graphite furnace atomic absorption (GFAA) and cold vapor atomic absorption and fluorescence (CVAA/CVAFS). Four different digestion procedures were evaluated including an open hot plate nitric acid digestion, EPA SW-846 Method 3051, and 2 methods using modifications to Method 3051. The open hot plate and the modified Method 3051, which used aqua regia for dissolution, were the only methods which resulted in acceptable data quality for all 14 RCRA-listed elements. Results for the nitric acid open hot plate digestion were used to qualify the analytical methods for TRU waste characterization, and resulted in a 99% passing score. Direct chemical analysis of TRU waste is being developed at Los Alamos National Laboratory in an attempt to circumvent the problems associated with strong acid digestion methods. Technology development includes laser induced breakdown spectroscopy (LIBS), laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS), dc arc CID atomic emission spectroscopy (DC-AES), and glow discharge mass spectrometry (GDMS). Analytical methods using the Portland cement matrix are currently being developed for each of the listed techniques. Upon completion of the development stage, blind samples will be distributed to each of the technology developers for RCRA metals characterization

The microwave induced plasma with optical emission spectrometry (MIP-OES) in 23 elements determination in geological samples.

Science.gov (United States)

Niedzielski, P; Kozak, L; Wachelka, M; Jakubowski, K; Wybieralska, J

2015-01-01

The article presents the optimisation, validation and application of the microwave induced plasma optical emission spectrometry (MIP-OES) dedicated for a routine determination of Ag, Al, B, Ba, Bi, Ca, Cd, Cr, Cu, Fe, Ga, In, K, Li, Mg, Mn, Mo, Na, Ni, Pb, Sr, Tl, Zn, in the geological samples. The three procedures of sample preparation has been proposed: sample digestion with the use of hydrofluoric acid for determination of total concentration of elements, extraction by aqua regia for determination of the quasi-total element concentration and extraction by hydrochloric acid solution to determine contents of the elements in acid leachable fraction. The detection limits were on the level 0.001-0.121 mg L(-1) (from 0.010-0.10 to 1.2-12 mg kg(-1) depend on the samples preparation procedure); the precision: 0.20-1.37%; accuracy 85-115% (for recovery for certified standards materials analysis and parallel analysis by independent analytical techniques: X-ray fluorescence (XRF) and flame absorption spectrometry (FAAS)). The conformity of the results obtained by MIP-OES analytical procedures with the results obtained by XRF and FAAS analysis allows to propose the procedures for studies of elemental composition of the fraction of the geological samples. Additionally, the MIP-OES technique is much less expensive than ICP techniques and much less time-consuming than AAS techniques. Copyright © 2014 Elsevier B.V. All rights reserved.

Qualitative and quantitative analysis of environmental samples by laser-induced breakdown spectrometry

International Nuclear Information System (INIS)

Zorov, N B; Popov, A M; Zaytsev, S M; Labutin, T A

2015-01-01

The key achievements in the determination of trace amounts of components in environmental samples (soils, ores, natural waters, etc.) by laser-induced breakdown spectrometry are considered. Unique capabilities of this method make it suitable for rapid analysis of metals and alloys, glasses, polymers, objects of cultural heritage, archaeological and various environmental samples. The key advantages of the method that account for its high efficiency are demonstrated, in particular, a small amount of analyzed material, the absence of sample preparation, the possibility of local and remote analysis of either one or several elements. The use of chemometrics in laser-induced breakdown spectrometry for qualitative sample classification is described in detail. Various approaches to improving the figures of merit of quantitative analysis of environmental samples are discussed. The achieved limits of detection for most elements in geochemical samples are critically evaluated. The bibliography includes 302 references

Detection and quantification of proteins and cells by use of elemental mass spectrometry: progress and challenges.

Science.gov (United States)

Yan, Xiaowen; Yang, Limin; Wang, Qiuquan

2013-07-01

Much progress has been made in identification of the proteins in proteomes, and quantification of these proteins has attracted much interest. In addition to popular tandem mass spectrometric methods based on soft ionization, inductively coupled plasma mass spectrometry (ICPMS), a typical example of mass spectrometry based on hard ionization, usually used for analysis of elements, has unique advantages in absolute quantification of proteins by determination of an element with a definite stoichiometry in a protein or attached to the protein. In this Trends article, we briefly describe state-of-the-art ICPMS-based methods for quantification of proteins, emphasizing protein-labeling and element-tagging strategies developed on the basis of chemically selective reactions and/or biospecific interactions. Recent progress from protein to cell quantification by use of ICPMS is also discussed, and the possibilities and challenges of ICPMS-based protein quantification for universal, selective, or targeted quantification of proteins and cells in a biological sample are also discussed critically. We believe ICPMS-based protein quantification will become ever more important in targeted quantitative proteomics and bioanalysis in the near future.

Automation system for measurement of gamma-ray spectra of induced activity for multi-element high-volume neutron activation analysis at the IBR-2 reactor of FLNP at JINR

International Nuclear Information System (INIS)

Pavlov, S.S.; Dmitriev, A.Yu.; Chepurchenko, I.A.; Frontas'eva, M.V.

2014-01-01

The automation system for measurement of induced activity of gamma-ray spectra for multi-element high-volume neutron activation analysis (NAA) was designed, developed and implemented at the IBR-2 reactor. The system consists of three devices of automatic sample changers for three Canberra HPGe detector-based gamma spectrometry systems. Each sample changer consists of two-axis linear positioning module M202A by DriveSet (DriveSet.de) company and disk with 45 slots for containers with samples. Control of automatic sample changer is performed by the Xemo S360U controller by Systec (systec.de) company. Positioning accuracy can reach 0.1 mm. Special software performs automatic changing of samples and measurement of gamma spectra at constant interaction with the NAA database. The system is unique and can be recommended for other laboratories as one of the possible ways of the NAA integrated automation

Multi-elemental analysis of marine sediments of Sorsogon Bay using x-ray fluorescence spectroscopy

International Nuclear Information System (INIS)

Gonzales, Ralph Roly A.; Quirit, Leni L.; Rosales, Colleen Marciel F.; Pabroa, Preciosa Corazon B.; Sta Maria, Efren J.

2011-01-01

Metal composition and nutrient loadings of our bodies of water, when uncontrolled, may cause harmful bacterial contamination and pose threats in aquatic and human life. Toxic and trace element inputs in Sorsogon Bay sediments were determined using nuclear analytical techniques, more specifically, x-ray fluorescence spectrometry, in this study. Pre-treated marine sediment samples from Sorsogon Bay were homogenized using SPEX # 8000 mixer/mill and agate mortar and pestle, pelletized into 31-mm flat discs using SPEX 3630 X-Press and analyzed using PAN Analytical Epsilon 5 EDX X-ray Fluorescence Spectrometer with the emission and transmission method using silver and germanium secondary targets. Spectrum fitting performed using AXIL (Analysis of X-ray Spectra by Iterative Least-Squares Fitting), a subprogram in Quantitative X-ray Analysis System developed by the International Atomic Energy Agency and Quantitative Analysis of Environmental Samples program, was used for quantification of results. Results indicate generally moderate to high metal enrichment, specifically manganese, lead, cadmium, zinc and copper. Mercury and iron level enrichment are found to be low, marking an improvement from previous studies indicating high enrichment of these metals. (author)

Elemental labelling combined with liquid chromatography inductively coupled plasma mass spectrometry for quantification of biomolecules: A review

Science.gov (United States)

Kretschy, Daniela; Koellensperger, Gunda; Hann, Stephan

2012-01-01

This article reviews novel quantification concepts where elemental labelling is combined with flow injection inductively coupled plasma mass spectrometry (FI-ICP-MS) or liquid chromatography inductively coupled plasma mass spectrometry (LC–ICP-MS), and employed for quantification of biomolecules such as proteins, peptides and related molecules in challenging sample matrices. In the first sections an overview on general aspects of biomolecule quantification, as well as of labelling will be presented emphasizing the potential, which lies in such methodological approaches. In this context, ICP-MS as detector provides high sensitivity, selectivity and robustness in biological samples and offers the capability for multiplexing and isotope dilution mass spectrometry (IDMS). Fundamental methodology of elemental labelling will be highlighted and analytical, as well as biomedical applications will be presented. A special focus will lie on established applications underlining benefits and bottlenecks of such approaches for the implementation in real life analysis. Key research made in this field will be summarized and a perspective for future developments including sophisticated and innovative applications will given. PMID:23062431

Determination of essential and toxic elements in commercial baby foods by instrumental neutron activation analysis and atomic absorption spectrometry

International Nuclear Information System (INIS)

Vallinoto, Priscila

2013-01-01

The World Health Organization recommends that infants should be breast fed exclusively for at least six months after birth. After this period, it is recommended to start introducing complementary foods, in order to meet the child's nutritional, mineral and energy needs. Commercial food products for infants form an important part of the diet for many babies. Thus, it is very important that such food contains sufficient amounts of minerals. Inadequate complementary feeding is a major cause of high rates of infant malnutrition in developing countries. In this study, essential elements: Ca, Cl, Co, Cr, Fe, K, Mg, Mn, Na, Se and Zn and toxic elements: As, Cd, Hg levels were determined in twenty seven different commercial infant food product samples by Instrumental Neutron Activation Analysis (INAA) and Atomic Absorption Spectrometry (AAS). In order to validate both methodologies the reference material: INCT MPH-2 Mixed Polish Herbs and NIST - SRM 1577b Bovine Liver by INAA and NIST - SRM 1548th Typical Diet and NIST - SRM 1547 Peach Leaves by AAS were analyzed. The twenty seven baby food samples were acquired from Sao Paulo city supermarkets and stores. Essential and toxic elements were determined. Most of the essential element concentrations obtained were lower than the World Health Organization requirements, while concentrations of toxic elements were below the tolerable upper limit. These low essential element concentrations in these samples indicate that infants should not be fed only with commercial complementary foods. (author)

Analysis of low Z elements in various environmental samples with total reflection X-ray fluorescence (TXRF) spectrometry

International Nuclear Information System (INIS)

Hoefler, H.; Streli, C.; Wobrauschek, P.; Ovari, M.; Zaray, Gy.

2006-01-01

Recently there is a growing interest in low Z elements such as carbon, oxygen up to sulphur and phosphorus in biological specimen. Total reflection X-ray fluorescence (TXRF) spectrometry is a suitable technique demanding only very small amounts of sample. On the other side, the detection of low Z elements is a critical point of this analytical technique. Besides other effects, self absorption may occur in the samples, because of the low energy of the fluorescence radiation. The calibration curves might be not linear any longer. To investigate this issue water samples and samples from human cerebrospinal fluid were used to examine absorption effects. The linearity of calibration curves in dependence of sample mass was investigated to verify the validity of the thin film approximation. The special requirements to the experimental setup for low Z energy dispersive fluorescence analysis were met by using the Atominstitute's TXRF vacuum chamber. This spectrometer is equipped with a Cr-anode X-ray tube, a multilayer monochromator and a SiLi detector with 30 mm 2 active area and with an ultrathin entrance window. Other object on this study are biofilms, living on all subaqueous surfaces, consisting of bacteria, algae and fungi embedded in their extracellular polymeric substances (EPS). Many trace elements from the water are bound in the biofilm. Thus, the biofilm is a useful indicator for polluting elements. For biomonitoring purposes not only the polluting elements but also the formation and growth rate of the biofilm are important. Biofilms were directly grown on TXRF reflectors. Their major elements and C-masses correlated to the cultivation time were investigated. These measured masses were related to the area seen by the detector, which was experimentally determined. Homogeneity of the biofilms was checked by measuring various sample positions on the reflectors

Analysis of low Z elements in various environmental samples with total reflection X-ray fluorescence (TXRF) spectrometry

Energy Technology Data Exchange (ETDEWEB)

Hoefler, H. [Atominstitut of the Austrian Universities, TU-Wien, A-1020 Vienna (Austria); Streli, C. [Atominstitut of the Austrian Universities, TU-Wien, A-1020 Vienna (Austria)]. E-mail: streli@ati.ac.at; Wobrauschek, P. [Atominstitut of the Austrian Universities, TU-Wien, A-1020 Vienna (Austria); Ovari, M. [Eoetvoes University, Institute of Chemistry, H-1117, Budapest, Pazmany P. stny 1/a. (Hungary); Zaray, Gy. [Eoetvoes University, Institute of Chemistry, H-1117, Budapest, Pazmany P. stny 1/a. (Hungary)

2006-11-15

Recently there is a growing interest in low Z elements such as carbon, oxygen up to sulphur and phosphorus in biological specimen. Total reflection X-ray fluorescence (TXRF) spectrometry is a suitable technique demanding only very small amounts of sample. On the other side, the detection of low Z elements is a critical point of this analytical technique. Besides other effects, self absorption may occur in the samples, because of the low energy of the fluorescence radiation. The calibration curves might be not linear any longer. To investigate this issue water samples and samples from human cerebrospinal fluid were used to examine absorption effects. The linearity of calibration curves in dependence of sample mass was investigated to verify the validity of the thin film approximation. The special requirements to the experimental setup for low Z energy dispersive fluorescence analysis were met by using the Atominstitute's TXRF vacuum chamber. This spectrometer is equipped with a Cr-anode X-ray tube, a multilayer monochromator and a SiLi detector with 30 mm{sup 2} active area and with an ultrathin entrance window. Other object on this study are biofilms, living on all subaqueous surfaces, consisting of bacteria, algae and fungi embedded in their extracellular polymeric substances (EPS). Many trace elements from the water are bound in the biofilm. Thus, the biofilm is a useful indicator for polluting elements. For biomonitoring purposes not only the polluting elements but also the formation and growth rate of the biofilm are important. Biofilms were directly grown on TXRF reflectors. Their major elements and C-masses correlated to the cultivation time were investigated. These measured masses were related to the area seen by the detector, which was experimentally determined. Homogeneity of the biofilms was checked by measuring various sample positions on the reflectors.

Imaging mass spectrometry statistical analysis.

Science.gov (United States)

Jones, Emrys A; Deininger, Sören-Oliver; Hogendoorn, Pancras C W; Deelder, André M; McDonnell, Liam A

2012-08-30

Imaging mass spectrometry is increasingly used to identify new candidate biomarkers. This clinical application of imaging mass spectrometry is highly multidisciplinary: expertise in mass spectrometry is necessary to acquire high quality data, histology is required to accurately label the origin of each pixel's mass spectrum, disease biology is necessary to understand the potential meaning of the imaging mass spectrometry results, and statistics to assess the confidence of any findings. Imaging mass spectrometry data analysis is further complicated because of the unique nature of the data (within the mass spectrometry field); several of the assumptions implicit in the analysis of LC-MS/profiling datasets are not applicable to imaging. The very large size of imaging datasets and the reporting of many data analysis routines, combined with inadequate training and accessible reviews, have exacerbated this problem. In this paper we provide an accessible review of the nature of imaging data and the different strategies by which the data may be analyzed. Particular attention is paid to the assumptions of the data analysis routines to ensure that the reader is apprised of their correct usage in imaging mass spectrometry research. Copyright © 2012 Elsevier B.V. All rights reserved.

Atomic mass spectrometry

International Nuclear Information System (INIS)

Sanz-Medel, A.

1997-01-01

The elemental inorganic analysis seems to be dominated today by techniques based on atomic spectrometry. After an evaluation of advantages and limitations of using mass analysers (ion detectors) versus conventional photomultipliers (photon detector) a brief review of the more popular techniques of the emerging Atomic Mass spectrometry is carried out. Their huge potential for inorganic trace analysis is such that in the future we could well witness how this end of the century and millennium marked the fall of the photons empire in Analytical Atomic Spectrometry. (Author)

Trace and surface analysis of ceramic layers of solid oxide fuel cells by mass spectrometry.

Science.gov (United States)

Becker, J S; Breuer, U; Westheide, J; Saprykin, A I; Holzbrecher, H; Nickel, H; Dietze, H J

1996-06-01

For the trace analysis of impurities in thick ceramic layers of a solid oxide fuel cell (SOFC) sensitive solid-state mass spectrometric methods, such as laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and radiofrequency glow discharge mass spectrometry (rf-GDMS) have been developed and used. In order to quantify the analytical results of LA-ICP-MS, the relative sensitivity coefficients of elements in a La(0.6)Sr(0.35)MnO(3) matrix have been determined using synthetic standards. Secondary ion mass spectrometry (SIMS) - as a surface analytical method - has been used to characterize the element distribution and diffusion profiles of matrix elements on the interface of a perovskite/Y-stabilized ZrO(2) layer. The application of different mass spectrometric methods for process control in the preparation of ceramic layers for the SOFC is described.

MicroCT parameters for multi material elements assessment

Energy Technology Data Exchange (ETDEWEB)

Araújo, Olga M.O. de; Machado, Alessandra S.; Santos, Thaís M.P. dos; Ferreira, Cintia G.; Lopes, Ricardo T., E-mail: olgaufrjlin@gmail.com [Universidade Federal do Rio de Janeiro (UFRJ), Rio de Janeiro, RJ (Brazil). Programa de Engenharia Nuclear; Bastos, Jaqueline Silva [Universidade Estadual Paulista Julio de Mesquita Filho (UNESP), São Paulo, SP (Brazil)

2017-07-01

Microtomography is a non-destructive testing technique for quantitative and qualitative analysis. The investigation of multi material elements with great difference of density can result in artifacts that degrade image quality depending on combination of additional filter. The aim of this study is the selection of parameters most appropriate for analysis of bone tissue with metallic implant. The results show the simulation with MCNPX code for the distribution of energy without additional filter, with use of aluminum, copper and brass filters and their respective reconstructed images showing the importance of the choice of these parameters in image acquisition process on computed microtomography. (author)

Simultaneous Atomic Absorption Spectrometry for Cadmium and Lead Determination in Wastewater: A Laboratory Exercise

Science.gov (United States)

Correia, Paulo R. M.; Oliveira, Pedro V.

2004-01-01

The simultaneous determination of cadmium and lead by multi-element atomic absorption spectrometry with electrochemical atomization is proposed by employing a problem-based approach. The reports indicate that the students assimilated the principles of the simultaneous atomic absorption spectrometry (SIMAAS), the role of the chemical modifier, the…

Multi-element Analysis of variable sample matrices using collision/reaction cell inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Zahran, N.F.; Helal, A.I.; Amr, M.A.; Amr, M.A.; Al-saad, K.A.

2008-01-01

An ICP-MS with an octopole reaction/collision cell is used for the multielement determination of trace elements in water, plants, and soil samples. The use of a reaction or collision gas reduces serious spectral interferences from matrix elements such as Ar Cl or Ar Na. The background equivalent concentration (BEC) is reduced one order of magnitude at helium flow rate of 1 mL/min. Certified reference material namely , NIST Water-1643d, Tomato leaves 1573a, and Montana soil 2711 are used. The trace elements Mn, Fe, Co, Ni, Cu, Zn, As, Mo, Cd and Pb are determined in the different matrices with a accuracy better than 8% to the certified values

Microwave assisted digestion of atmospheric aerosol samples followed by inductively coupled plasma mass spectrometry determination of trace elements

Energy Technology Data Exchange (ETDEWEB)

Swami, K.; Judd, C.D.; Orsini, J.; Yang, K.X. [New York State Dept. of Health, Albany, NY (United States). Wadsworth Center for Labs. and Research; Husain, L. [New York State Dept. of Health, Albany, NY (United States). Wadsworth Center for Labs. and Research; Dept. of Environmental Health and Toxicology, State Univ. of New York, Albany (United States)

2001-01-01

A microwave digestion method in a closed vessel was developed for the determination of trace metals in atmospheric aerosols using inductively coupled plasma mass spectrometry (ICP-MS). A recovery study for the elements V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Cd, Sb, and Pb was conducted using multi-elemental standard solutions, NIST 1633b Trace Elements in Coal Fly Ash, and NIST 1648 Urban Particulate Matter. A simple digestion method using only HNO{sub 3}/H{sub 2}O{sub 2}gave good recoveries (90%-108%) for all elements except Cr in SRM 1648, but yielded low recoveries for SRM 1633b. A more robust method using HNO {sub 3}/H {sub 2}O {sub 2}/HF/H {sub 3}BO {sub 3} yielded higher recoveries (82%-103%) for the lighter elements (V - Zn) in SRM 1633b, and improved the Cr recovery in SRM 1648, but decreased the Se recovery in both SRMs. A comparative analysis of aerosol samples obtained at a remote mountain location Nathiagali, Pakistan (2.5 km above mean sea level), and Mayville, New York, downwind from the highly industrialized Midwestern United States, was carried out using Instrumental Neutron Activation Analysis (INAA) for the elements Cr, Mn, Fe, Co, Zn, As, Se, and Sb. The simple digestion method yielded excellent agreement for Cr, Fe, Zn, As, Se, and Sb, with slopes of the ICP-MS vs. INAA regressions of 0.90-1.00 and R {sup 2} values of 0.96-1.00. The regressions for Mn and Co had slopes of 0.82 and 0.84 with R {sup 2} values of 0.83 and 0.82, respectively. Addition of HF/H {sub 3}BO {sub 3} did not improve the correlation for any of the elements and degraded the precision somewhat. The technique provides sensitivity and accuracy for trace elements in relatively small aerosol samples used in atmospheric chemistry studies related to SO {sub 2} oxidation in cloud droplets. The ability to determine concentrations of a very large number of elements from a single analysis will permit source apportionment of various trace pollutants and hence strategies to control the

Comparison of inductively coupled plasma mass spectrometry with inductively coupled plasma atomic emission spectrometry and instrumental neutron activation analysis for the determination of rare earth elements in Greek bauxites

International Nuclear Information System (INIS)

Ochsenkuehn-Petropoulou, Maria; Luck, Joachim

1991-01-01

Fore the determination of rare earth elements (REE) in bauxitic materials the techniques of inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma atomic emission spectrometry (ICP-AES) and instrumental neutron activation analysis (INAA) were compared. In the NIST (National Institute of Standards and Technology) bauxites SRM 697 Dominican, and SRM 69 b Arkansas, the concentration of some REEs were determined. With the reference bauxite BX-N of the ARNT (Association Nationale de la Recherche Technique) the precision and accuracy of ICP-AES for the determination of REEs in bauxites was tested. Furthermore, Greek bauxites of the Parnassos-Giona area were investigated. In a comparison of the three methods it was possible to calculate from the data series the precision of each method, which showed that the tendency found in the deviations for the different REEs is in accordance with published values. Also the limits of detection for REEs in bauxites were calculated and found to be in the same range as those in the literature. (author)

Ultratrace analysis of uranium and plutonium by mass spectrometry

International Nuclear Information System (INIS)

Wogman, N.A.; Wacker, J.F.; Olsen, K.B.; Petersen, S.L.; Farmer, O.T.; Kelley, J.M.; Eiden, G.C.; Maiti, T.C.

2002-01-01

Full text: Uranium and plutonium have traditionally been analyzed using alpha energy spectrometry. Both isotopic compositions and elemental abundances can be characterized on samples containing microgram to milligram quantities of uranium and nanogram to microgram quantities of plutonium. In the past ten years or so, considerable interest has developed in measuring nanograms quantities of uranium and sub-picogram quantities of plutonium in environmental samples. Such measurements require high sensitivity and as a consequence, sensitive mass spectrometric-based methods have been developed. Thus, the analysis of uranium and plutonium have gone from counting decays to counting atoms, with considerable increases in both sensitivity and precision for isotopic measurements. At the Pacific Northwest National Laboratory (PNNL), we have developed highly sensitive methods to analyze uranium and plutonium in environmental samples. The development of an ultratrace analysis capability for measuring uranium and plutonium has arisen from a need to detect and characterize environmental samples for signatures associated with nuclear industry processes. Our most sensitive well-developed methodologies employ thermal ionization mass spectrometry (TIMS), however, recent advances in inductively coupled plasma mass spectrometry (ICP-MS) have shown considerable promise for use in detecting uranium and plutonium at ultratrace levels. The work at PNNL has included the development of both chemical separation and purification techniques, as well as the development of mass spectrometric instrumentation and techniques. At the heart of our methodology for TIMS analysis is a procedure that utilizes 100-microliter-volumes of analyte for chemical processing to purify, separate, and load actinide elements into resin beads for subsequent mass spectrometric analysis. The resin bead technique has been combined with a thorough knowledge of the physicochemistry of thermal ion emission to achieve

Applications of plasma spectrometry and high performance liquid chromatography in environmental and food science

International Nuclear Information System (INIS)

Iordache, Andreea-Maria; Biraruti, Elisabeta-Irina; Ionete, Roxana-Elena

2008-01-01

Full text: Plasma spectrometry has many applications in food science in analysis of a wide range of samples in the food chain. Food science in the broadest sense can be extended to include soil chemistry, plant uptake and, at the other end of the food chain, studies into the metabolic fate of particular elements or elemental species when the foods are consumed by humans or animals. Inductively Coupled Plasma Mass Spectrometry allows multi-element measurements of most elements in the periodic table. A very sensitive analytical technique for trace analysis of samples can be performed by inductively plasma mass spectrometer with quadrupolar detector using ultrasonic nebulization. High Performance Liquid Chromatography (HPLC) is an analytical technique for the separation and determination of organic and inorganic solutes in any samples especially biological, pharmaceutical, food, environmental. The present paper emphasizes that the future tendencies HPLC-ICP-MS is often the preferred analytical technique for these applications due to the simplicity of the coupling between the HPLC and ICP-MS Varian 820 using ultrasonic nebulization, potential for on-line separations with high species specificity and the capability for optimum limits of detection without the necessity of using complex hydride generation mechanisms. (authors)

Multi element analysis by X-ray fluorescence. A powerful tool of ivory identification from various origins

International Nuclear Information System (INIS)

Kautenburger, R.; Mueller, P.; Wannemacher, J.

2004-01-01

The 11th CITES Conference in 2000 decided to maintain a total worldwide ban on trade of elephant ivory. The 12th Conference in 2002 decided to allow a conditional trade in stockpiled ivory in 2004. Reopening of the ivory trade would require methods to identify the origin of the ivory so that legal ivory can be distinguished from the black-market ones. X-ray fluorescence multi-element analysis of ivory samples from various regions of Africa and Southeast-Asia to characterize ivory of the various elephant populations is described. (author)

Discrimination of wine from grape cultivated in Japan, imported wine, and others by multi-elemental analysis.

Science.gov (United States)

Shimizu, Hideaki; Akamatsu, Fumikazu; Kamada, Aya; Koyama, Kazuya; Okuda, Masaki; Fukuda, Hisashi; Iwashita, Kazuhiro; Goto-Yamamoto, Nami

2018-04-01

Differences in mineral concentrations were examined among three types of wine in the Japanese market place: Japan wine, imported wine, and domestically produced wine mainly from foreign ingredients (DWF), where Japan wine has been recently defined by the National Tax Agency as domestically produced wine from grapes cultivated in Japan. The main objective of this study was to examine the possibility of controlling the authenticity of Japan wine. The concentrations of 18 minerals (Li, B, Na, Mg, Si, P, S, K, Ca, Mn, Co, Ni, Ga, Rb, Sr, Mo, Ba, and Pb) in 214 wine samples were determined by inductively coupled-plasma mass spectrometry (ICP-MS) and ICP-atomic emission spectrometry (ICP-AES). In general, Japan wine had a higher concentration of potassium and lower concentrations of eight elements (Li, B, Na, Si, S, Co, Sr, and Pb) as compared with the other two groups of wine. Linear discriminant analysis (LDA) models based on concentrations of the 18 minerals facilitated the identification of three wine groups: Japan wine, imported wine, and DWF with a 91.1% classification score and 87.9% prediction score. In addition, an LDA model for discrimination of wine from four domestic geographic origins (Yamanashi, Nagano, Hokkaido, and Yamagata Prefectures) using 18 elements gave a classification score of 93.1% and a prediction score of 76.4%. In summary, we have shown that an LDA model based on mineral concentrations is useful for distinguishing Japan wine from other wine groups, and can contribute to classification of the four main domestic wine-producing regions of Japan. Copyright © 2017 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

Analysis of trace elements in serum from human eating irradiated food

International Nuclear Information System (INIS)

Huang Zongzhi; Zhou Hongdi; Chen Shijie; Gao Sumei

1987-01-01

A method of trace element analysis by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AEC) in serum from human eating food preserved by irradiation is described. Trace element analysis in human serum is one of the research projects concerning the wholesomeness. 78 serum samples of the human eating food preserved by irradiation were collected. After ashing and solving ICP-AES analysis of serum is performed for detecting 12 trace elements in specimen solution. The detection limitations are in the range of 10 -2 - 10 -3 ppm for differemt elements. The recoveries of elements are over 73%. Concentrations of 12 trace elements in 78 human serum has been calculated with F and t tests at PDP 11/70 computer and it was concluded that there is no significant difference between testing group and control group

Capture analysis of element content of a substance with other neutron methods

International Nuclear Information System (INIS)

Kurbanov, B.I.

2004-01-01

Full text: Neutron analysis method of determining element composition have found wide range of applications in industry thanks to different types of interaction of neutron with substances /1/. With the aim of widening the range of problems to be solved, on the basis of the device /2/ for determining the element content of substance, possibilities of combining the method based on the use of neutron capture gamma-ray spectrometry with other neutron methods, in particular neutron activation analysis and neutron absorption analysis were studied. In this radionuclide source ( 252 Cf) with the yield of 1,5 x 10 7 neutron/sec is used. By means of using neutron capture gamma radiation spectrometry the possibilities of determining some elements (H, B, N, S etc. ), which are not determined by very widely used method, activation analysis. These elements can be determined by both the semiconductor and scintillation detectors with parameters fitting the manufacturing requirements. And for a number of elements ( B, Cl, Cd, Sm, Gd) very high limits of determination ( up to 10- 5 %) are possible using semiconductor Ge (Li) -detectors with high resolution. Possibility of determination of some 'well' activated elements ( K, Al, Fe, Mn, Ti, Sc etc.) in samples of ore and products of their processing using the neutron-activation analysis. For 1 hour of irradiation on the experimental device quite accurate analytical peak, of these elements are obtained, allowing to determine them qualitatively. However, with decreasing neutron yield of radionuclide source it becomes more difficult to achieve the necessary parameters both in neutron capture and activation analysis. Experimental works on determination of some elements with large cross-sections of capture ( B, Cd, Sm ) by absorption of neutrons in the investigated substance, i.e. using the neutron absorption analysis method with absence of other large capture cross section elements in the samples being studied

Reliability modelling and analysis of a multi-state element based on a dynamic Bayesian network

Science.gov (United States)

Li, Zhiqiang; Xu, Tingxue; Gu, Junyuan; Dong, Qi; Fu, Linyu

2018-04-01

This paper presents a quantitative reliability modelling and analysis method for multi-state elements based on a combination of the Markov process and a dynamic Bayesian network (DBN), taking perfect repair, imperfect repair and condition-based maintenance (CBM) into consideration. The Markov models of elements without repair and under CBM are established, and an absorbing set is introduced to determine the reliability of the repairable element. According to the state-transition relations between the states determined by the Markov process, a DBN model is built. In addition, its parameters for series and parallel systems, namely, conditional probability tables, can be calculated by referring to the conditional degradation probabilities. Finally, the power of a control unit in a failure model is used as an example. A dynamic fault tree (DFT) is translated into a Bayesian network model, and subsequently extended to a DBN. The results show the state probabilities of an element and the system without repair, with perfect and imperfect repair, and under CBM, with an absorbing set plotted by differential equations and verified. Through referring forward, the reliability value of the control unit is determined in different kinds of modes. Finally, weak nodes are noted in the control unit.

Synthetic multi-element standards: a good tool for calibration and quality control of irradiation facilities used for neutron activation analysis

International Nuclear Information System (INIS)

Vermaercke, P.

2007-01-01

Neutron activation analysis (NAA) is a physical technique used for the absolute measurement of the concentration of substances in solids and liquids. The method uses neutron irradiation which is commonly realised using a nuclear reactor in order to activate (make radioactive) different isotopes of the elements present in the sample. The radionuclides produced in this way emit gamma-rays that are characteristic of the elements present in the sample. Using gamma-ray spectrometry these radionuclides can then be identified and quantified, and hence their concentration in the sample can be determined. Although NAA is a straightforward method it requires a sound control of the many physical parameters involved to obtain accurate results and to guarantee a set accuracy in routine analysis. The accuracy of NAA depends on the specific measurement method used. One can perform NAA in a relative way by co-irradiating a known standard and the unknown sample in the same conditions and by comparing the ratio of gamma-rays they emit. Relative NAA has limited applicability since it requires reference standards with a comparable composition as the unknown. A more generally applicable method is the k0-NAA method. In the k0-NAA method all measurements are relative to the element Au resulting in 198Au when irradiated. The k0-NAA method further relies on the fact that the neutron energy spectrum produced in a given position in the reactor can be parameterised with two parameters: the shape factor of the epithermal neutron flux, indicating the deviation of the epithermal neutron spectrum from the ideal 1/E shape approximated by a 1/E1+a distribution, with E the neutron energy; f: the thermal-to-epithermal neutron flux ratio. The parameters f and a are characteristic for the irradiation facility (reactor and irradiation channels) and may change or fluctuate in time according to the irradiation conditions. The way elements activate (become radioactive) when interacting with neutrons is

Comparison of a portable micro-X-ray fluorescence spectrometry with inductively coupled plasma atomic emission spectrometry for the ancient ceramics analysis

International Nuclear Information System (INIS)

Papadopoulou, D.N.; Zachariadis, G.A.; Anthemidis, A.N.; Tsirliganis, N.C.; Stratis, J.A.

2004-01-01

Two multielement instrumental methods of analysis, micro X-ray fluorescence spectrometry (micro-XRF) and inductively coupled plasma atomic emission spectrometry (ICP-AES) were applied for the analysis of 7th and 5th century B.C. ancient ceramic sherds in order to evaluate the above two methods and to assess the potential to use the current compact and portable micro-XRF instrument for the in situ analysis of ancient ceramics. The distinguishing factor of interest is that micro-XRF spectrometry offers the possibility of a nondestructive analysis, an aspect of primary importance in the compositional analysis of cultural objects. Micro-XRF measurements were performed firstly directly on the ceramic sherds with no special pretreatment apart from surface cleaning (micro-XRF on sherds) and secondly on pressed pellet disks which were prepared for each ceramic sherd (micro-XRF on pellet). For the ICP-AES determination of elements, test solutions were prepared by the application of a microwave-assisted decomposition procedure in closed high-pressure PFA vessels. Also, the standard reference material SARM 69 was used for the efficiency calibration of the micro-XRF instrument and was analysed by both methods. In order to verify the calibration, the standard reference materials NCS DC 73332 and SRM620 as well as the reference materials AWI-1 and PRI-1 were analysed by micro-XRF. Elemental concentrations determined by the three analytical procedures (ICP-AES, micro-XRF on sherds and micro-XRF on pellets) were statistically treated by correlation analysis and Student's t-test (at the 95% confidence level)

Comparison of a portable micro-X-ray fluorescence spectrometry with inductively coupled plasma atomic emission spectrometry for the ancient ceramics analysis

Energy Technology Data Exchange (ETDEWEB)

Papadopoulou, D.N. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece); Zachariadis, G.A. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece); Anthemidis, A.N. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece); Tsirliganis, N.C. [Archaeometry Laboratory, Cultural and Educational Technology Institute, Tsimiski 58, GR-67100, Xanthi (Greece); Stratis, J.A. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece)]. E-mail: jstratis@chem.auth.gr

2004-12-01

Two multielement instrumental methods of analysis, micro X-ray fluorescence spectrometry (micro-XRF) and inductively coupled plasma atomic emission spectrometry (ICP-AES) were applied for the analysis of 7th and 5th century B.C. ancient ceramic sherds in order to evaluate the above two methods and to assess the potential to use the current compact and portable micro-XRF instrument for the in situ analysis of ancient ceramics. The distinguishing factor of interest is that micro-XRF spectrometry offers the possibility of a nondestructive analysis, an aspect of primary importance in the compositional analysis of cultural objects. Micro-XRF measurements were performed firstly directly on the ceramic sherds with no special pretreatment apart from surface cleaning (micro-XRF on sherds) and secondly on pressed pellet disks which were prepared for each ceramic sherd (micro-XRF on pellet). For the ICP-AES determination of elements, test solutions were prepared by the application of a microwave-assisted decomposition procedure in closed high-pressure PFA vessels. Also, the standard reference material SARM 69 was used for the efficiency calibration of the micro-XRF instrument and was analysed by both methods. In order to verify the calibration, the standard reference materials NCS DC 73332 and SRM620 as well as the reference materials AWI-1 and PRI-1 were analysed by micro-XRF. Elemental concentrations determined by the three analytical procedures (ICP-AES, micro-XRF on sherds and micro-XRF on pellets) were statistically treated by correlation analysis and Student's t-test (at the 95% confidence level)

Finite element analysis of multi-material models using a balancing domain decomposition method combined with the diagonal scaling preconditioner

International Nuclear Information System (INIS)

Ogino, Masao

2016-01-01

Actual problems in science and industrial applications are modeled by multi-materials and large-scale unstructured mesh, and the finite element analysis has been widely used to solve such problems on the parallel computer. However, for large-scale problems, the iterative methods for linear finite element equations suffer from slow or no convergence. Therefore, numerical methods having both robust convergence and scalable parallel efficiency are in great demand. The domain decomposition method is well known as an iterative substructuring method, and is an efficient approach for parallel finite element methods. Moreover, the balancing preconditioner achieves robust convergence. However, in case of problems consisting of very different materials, the convergence becomes bad. There are some research to solve this issue, however not suitable for cases of complex shape and composite materials. In this study, to improve convergence of the balancing preconditioner for multi-materials, a balancing preconditioner combined with the diagonal scaling preconditioner, called Scaled-BDD method, is proposed. Some numerical results are included which indicate that the proposed method has robust convergence for the number of subdomains and shows high performances compared with the original balancing preconditioner. (author)

ICP-AES determination of trace elements in carbon steel

International Nuclear Information System (INIS)

Sengupta, Arijit; Rajeswari, B.; Kadam, R.M.; Babu, Y.; Godbole, S.V.

2010-01-01

Full text: Carbon steel, a combination of the elements iron and carbon, can be classified into four types as mild, medium, high and very high depending on the carbon content which varies from 0.05% to 2.1%. Carbon steel of different types finds application in medical devices, razor blades, cutlery and spring. In the nuclear industry, it is used in feeder pipes in the reactor. A strict quality control measure is required to monitor the trace elements, which have deleterious effects on the mechanical properties of the carbon steel. Thus, it becomes imperative to check the purity of carbon steel as a quality control measure before it is used in feeder pipes in the reactor. Several methods have been reported in literature for trace elemental determination in high purity iron. Some of these include neutron activation analysis, atomic absorption spectrometry and atomic emission spectrometry. Inductively coupled plasma atomic emission spectrometry (ICP-AES) is widely recognized as a sensitive technique for the determination of trace elements in various matrices, its major advantages being good accuracy and precision, high sensitivity, multi-element capability, large linear dynamic range and relative freedom from matrix effects. The present study mainly deals with the direct determination of trace elements in carbon steel using ICP-AES. An axially viewing ICP spectrometer having a polychromator with 35 fixed analytical channels and limited sequential facility to select any analytical line within 2.2 nm of a polychromator line was used in these studies. Iron, which forms one of the main constituents of carbon steel, has a multi electronic configuration with line rich emission spectrum and, therefore, tends to interfere in the determination of trace impurities in carbon steel matrix. Spectral interference in ICP-AES can be seriously detrimental to the accuracy and reliability of trace element determinations, particularly when they are performed in the presence of high

Effects of Heat Input and Bead Generation Methods on Finite Element Analysis of Cylindrical Multi-Pass Welding Process of Metals

International Nuclear Information System (INIS)

Park, Won Dong; Bahn, Chi Bum; Kim, Ji Hoon

2017-01-01

In this study, a finite element analysis of a cylindrical multi-pass weldment for dissimilar metals was performed. The effects of the heat input method and weld bead generation method were considered. We compared two heat input methods: the heat flux method and the temperature method. We also compared two weld bead generation methods: the element birth method and the quiet element method. Although the results of the thermal analysis show deviations between the two heat input methods, the welding residual stresses were similar. Because the areas exposed to high temperature were similar and the strength of the material was very low in high temperature (above the 1000 ℃), the effects of the weld bead temperature were insignificant. The distributions of the welding residual stress were similar to each other. However, gaps and overlaps occurred on the welding boundary surfaces when the element birth method was applied. The quiet element method is more suitable for a large deformation model in order to simulate a more accurate weld shape.

Effects of Heat Input and Bead Generation Methods on Finite Element Analysis of Cylindrical Multi-Pass Welding Process of Metals

Energy Technology Data Exchange (ETDEWEB)

Park, Won Dong; Bahn, Chi Bum; Kim, Ji Hoon [Pusan Nat’l Univ., Busan (Korea, Republic of)

2017-06-15

In this study, a finite element analysis of a cylindrical multi-pass weldment for dissimilar metals was performed. The effects of the heat input method and weld bead generation method were considered. We compared two heat input methods: the heat flux method and the temperature method. We also compared two weld bead generation methods: the element birth method and the quiet element method. Although the results of the thermal analysis show deviations between the two heat input methods, the welding residual stresses were similar. Because the areas exposed to high temperature were similar and the strength of the material was very low in high temperature (above the 1000 ℃), the effects of the weld bead temperature were insignificant. The distributions of the welding residual stress were similar to each other. However, gaps and overlaps occurred on the welding boundary surfaces when the element birth method was applied. The quiet element method is more suitable for a large deformation model in order to simulate a more accurate weld shape.

Using the ion microprobe mass analyser for trace element analysis

International Nuclear Information System (INIS)

Schilling, J.H.

1978-01-01

Most techniques for the analysis of trace elements are capable of determining the concentrations in a bulk sample or solution, but without reflecting their distribution. In a bulk analysis therefore elements which occur in high concentration in a few precipitates would still be considered trace elements even though their local concentration greatly exceed the normally accepted trace elements concentration limit. Anomalous distribution is also shown by an oxide layer, a few hundred Angstrom thick, on an aluminium sample. A low oxide concentration would be reported if it were included in the bulk analysis, which contradicts the high surface concentration. The importance of a knowledge of the trace element distribution is therefore demonstrated. Distributional trace element analysis can be carried out using the ion microprobe mass analyser (IMMA). Since the analytical technique used in this instrument, namely secondary ion mass spectrometry (SIMS), is not universally appreciated, the instrument and its features will be described briefly followed by a discussion of quantitative analysis and the related subjects of detection limit and sample consumption. Finally, a few examples of the use of the instrument are given

Determination of wheat quality by mass spectrometry and multivariate data analysis

DEFF Research Database (Denmark)

Gottlieb, D.M.; Schultz, J.; Petersen, M.

2002-01-01

Multivariate analysis has been applied as support to proteome analysis in order to implement an easier and faster way of data handling based on separation by matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry. The characterisation phase in proteome analysis by means...... of simple visual inspection is a demanding process and also insecure because subjectivity is the controlling element. Multivariate analysis offers, to a considerable extent, objectivity and must therefore be regarded as a neutral way to evaluate results obtained by proteome analysis.Proteome analysis...

Game meat authentication through rare earth elements fingerprinting.

Science.gov (United States)

Danezis, G P; Pappas, A C; Zoidis, E; Papadomichelakis, G; Hadjigeorgiou, I; Zhang, P; Brusic, V; Georgiou, C A

2017-10-23

Accurate labelling of meat (e.g. wild versus farmed, geographical and genetic origin, organic versus conventional, processing treatment) is important to inform the consumers about the products they buy. Meat and meat products declared as game have higher commercial value making them target to fraudulent labelling practices and replacement with non-game meat. We have developed and validated a new method for authentication of wild rabbit meat using elemental metabolomics approach. Elemental analysis was performed using rapid ultra-trace multi-element measurement by inductively coupled plasma mass spectrometry (ICP-MS). Elemental signatures showed excellent ability to discriminate the wild rabbit from non-wild rabbit meat. Our results demonstrate the usefulness of metabolic markers -rare earth signatures, as well as other trace element signatures for game meat authentication. Copyright © 2017 Elsevier B.V. All rights reserved.

Integration of Solid-phase Extraction with Electrothermal Atomic Absorption Spectrometry for Determination of Trace Elements

OpenAIRE

NUKATSUKA, Isoshi; OHZEKI, Kunio

2006-01-01

An enrichment step in a sample treatment is essential for trace analysis to improve the sensitivity and to eliminate the matrix of the sample. Solid-phase extraction (SPE) is one of the widely used enrichment technique. Electrothermal atomic absorption spectrometry (ETAAS) is a well-established determination technique for trace elements. The integration of SPE with ETAAS leads to further improvement of sensitivity, an automation of the measurement and the economy in the sample size, amounts o...

Detection of negative ions in glow discharge mass spectrometry for analysis of solid specimens

DEFF Research Database (Denmark)

Canulescu, Stela; Molchan, Igor S.; Tauziede, C.

2010-01-01

A new method is presented for elemental and molecular analysis of halogen-containing samples by glow discharge time-of-flight mass spectrometry, consisting of detection of negative ions from a pulsed RF glow discharge in argon. Analyte signals are mainly extracted from the afterglow regime...... be used to study the distribution of a tantalum fluoride layer within the anodized tantala layer. Further, comparison is made with data obtained using glow-discharge optical emission spectroscopy, where elemental fluorine can only be detected using a neon plasma. The ionization mechanisms responsible...... for the formation of negative ions in glow discharge time-of-flight mass spectrometry are briefly discussed....

Study on elemental analysis of metal and ceramic samples by using laser ablation ion trap mass spectrometry(LAITMS)

International Nuclear Information System (INIS)

Cha, Hyung Ki; Park, Hyun Kook; Lee, Sang Chun; SONG, Kyu Seok

2002-01-01

Laser ablation ion trap mass spectrometry (LAITMS) was developed for the analysis of metal and ceramic samples. For this study, XeCl excimer laser (308 nm) was used for ablating the samples and ITMS was used as a detector. Samples were introduced from outside of a ring electrode and this way of sample introduction was very effective for solid samples when laser ablation was employed. Helium gas was used as a buffer gas, and its effect on sensitivity and some parameters (buffer gas pressure, ion storage time, and cut-off RF voltage) were studied. The optimized conditions were 1 x 10 - 4 Torr of buffer gas pressure, 100 ms of ion storage time and 1150 V p- p of cut-off RF voltage. From that results, copper (Cu) and molybdenum(Mo) metals were tested with LAITMS and the mass spectra of these pure metals were compared with the natural abundance of isotope ratio. We also examined ceramic samples (Al 2 O 3 , ZrO 2 ) and represented the result of elements analysis

Single cell elemental analysis using nuclear microscopy

International Nuclear Information System (INIS)

Ren, M.Q.; Thong, P.S.P.; Kara, U.; Watt, F.

1999-01-01

The use of Particle Induced X-ray Emission (PIXE), Rutherford Backscattering Spectrometry (RBS) and Scanning Transmission Ion Microscopy (STIM) to provide quantitative elemental analysis of single cells is an area which has high potential, particularly when the trace elements such as Ca, Fe, Zn and Cu can be monitored. We describe the methodology of sample preparation for two cell types, the procedures of cell imaging using STIM, and the quantitative elemental analysis of single cells using RBS and PIXE. Recent work on single cells at the Nuclear Microscopy Research Centre,National University of Singapore has centred around two research areas: (a) Apoptosis (programmed cell death), which has been recently implicated in a wide range of pathological conditions such as cancer, Parkinson's disease etc, and (b) Malaria (infection of red blood cells by the malaria parasite). Firstly we present results on the elemental analysis of human Chang liver cells (ATTCC CCL 13) where vanadium ions were used to trigger apoptosis, and demonstrate that nuclear microscopy has the capability of monitoring vanadium loading within individual cells. Secondly we present the results of elemental changes taking place in individual mouse red blood cells which have been infected with the malaria parasite and treated with the anti-malaria drug Qinghaosu (QHS)

Simultaneous determination of macro and trace elements in biological reference materials by microwave induced plasma optical emission spectrometry with slurry sample introduction

International Nuclear Information System (INIS)

Matusiewicz, Henryk; Golik, Bartosz

2004-01-01

A slurry sampling technique (SST) has been utilized for simultaneous multi-element analysis by microwave-induced plasma optical emission spectrometry (MIP-OES). Slurry samples from a spray chamber are fed directly into the microwave cavity-torch assembly (power 300 W) with no desolvation apparatus. The performance of SST-MIP-OES was demonstrated by the determination of macro (Na, K, Ca, Mg, P) and trace (Cd, Cu, Mn, Sr, Zn) elements in three biological certified reference materials using a V-groove, clog-free Babington-type nebulizer. Slurry concentrations up to 1% m/v (particles 3 (pH 1.2) containing 0.01% of Triton X-100, were used with calibration by the standard additions method. The method offers relatively good precision (R.S.D. ranged from 7 to 11%) with measured concentrations being in satisfactory agreement with certified values for NRCC TORT-1 (Lobster hepatopancreas), NRCC LUTS-1 (Lobster hepatopancreas) and IAEA-153 (Milk powder). The concentrations of Na, K, Ca, Mg, P and Cd, Cu, Mn, Sr, Zn were determined in the range 90-22 000 μg/g and 1-420 μg/g, respectively. The method could be useful as a routine procedure

Multi photon ionization mass spectrometry of carbamate pesticides, herbicides and fungicides

International Nuclear Information System (INIS)

Grun, Carsten; Koenig, Marcelle; Grotemeyer, Juergen

2001-01-01

Pesticides and herbicides are useful for a wide range of applications today. The determination of these substances either in the pure form or in complex matrices is of high analytical interest. Especially since these substances can by found in every day products. The combination of multi photon ionization (MUPI) and time of flight laser mass spectrometry may be a powerful tool for achieving fast well interpretable mass spectra for analytical purposes. In this paper we will discuss the mass spectra of several pesticides and herbicides accessed by MUPI-time-of-flight mass spectrometry. The influence of the laser pulse duration on the mass spectra are discussed

Determination of C and O and other elements by alpha-induced X-ray energy spectrometry

International Nuclear Information System (INIS)

Henningsen, W.P.; Schaetzler, H.P.; Kuehn, W.

1978-01-01

X-ray energy spectrometry combined with alpha-excitation by means of radionuclides, especially Po-210, has been found as a versatile tool for multielement analysis. Down to Z = 6 (carbon) qualitative and quantitative measurements have been carried out with energy resolution good enough to separate adjacent elements. Thereby errors and lowest detectable concentrations were in the region of one percent. By utilizing M- and L-X-radiation the set of detectable elements can be opened to high atomic numbers. As an example with special regard to environmental research cadmium in organic matrix was measured down to 100 ppm without any preconcentration. Much lower detection limits might be reached by appropriate measures. (orig.) [de

Guideline on Isotope Dilution Mass Spectrometry

Energy Technology Data Exchange (ETDEWEB)

Gaffney, Amy [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

2017-05-19

Isotope dilution mass spectrometry is used to determine the concentration of an element of interest in a bulk sample. It is a destructive analysis technique that is applicable to a wide range of analytes and bulk sample types. With this method, a known amount of a rare isotope, or ‘spike’, of the element of interest is added to a known amount of sample. The element of interest is chemically purified from the bulk sample, the isotope ratio of the spiked sample is measured by mass spectrometry, and the concentration of the element of interest is calculated from this result. This method is widely used, although a mass spectrometer required for this analysis may be fairly expensive.

Elemental hair analysis: A review of procedures and applications

International Nuclear Information System (INIS)

Pozebon, D.; Scheffler, G.L.; Dressler, V.L.

2017-01-01

Although exogenous contamination and unreliable reference values have limited the utility of scalp hair as a biomarker of chemical elements exposure, its use in toxicological, clinical, environmental and forensic investigations is growing and becoming more extensive. Therefore, hair elemental analysis is reviewed in the current manuscript which spans articles published in the last 10 years. It starts with a general discussion of history, morphology and possible techniques for elemental analysis, where inductively coupled plasma-mass spectrometry (ICP-MS) is clearly highlighted since this technique is leading quantitative ultra-trace elemental analysis. Emphasis over sampling, quality assurance, washing procedures and sample decomposition is given with detailed protocols compiled in tables as well as the utility of hair to identify human gender, age, diseases, healthy conditions, nutrition status and contamination sites. Isotope ratio information, chemical speciation analysis and analyte preconcentration are also considered for hair. Finally, the potential of laser ablation ICP-MS (LA-ICP-MS) to provide spatial resolution and time-track the monitoring of elements in hair strands instead of conventional bulk analysis is spotlighted as a real future trend in the field. - Highlights: • Elemental analysis of hair is critically reviewed, with focus on ICP-MS employment. • Standards protocols of hair washing and sample decomposition are compiled. • The usefulness of elemental and/or isotopic analysis of hair is demonstrated. • The potential of LA-ICP-MS for elemental time tracking in hair is highlighted.

Trace metal analysis of road dust by inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Powell, M.J.; Liu, L.; Gnanalingham, N.; Peters, L.

2000-01-01

Dust from roads in an air impingement zone close to anthropogenic sources of air pollutants can be a concern for people living in the immediate vicinity. The Ministry of the Environment (MOE) has conducted a case study to monitor the concentration of uranium, strontium, thorium and arsenic in road dust from one such area. A method for the analysis of road dust by inductively coupled plasma mass spectrometry (ICP-MS) has been developed with detection limits in the ng/1 range. A digestion technique has been developed by conducting experiments using single and combinations of acids in open-vessel wet digestions. Accuracy has been determined by the use of matrix representative certified reference materials (CRMs). Digestion precision was determined by elemental concentration measurements of the most representative CRM through replicates. Spike recovery data were from 95% to 110% for all elements, and inter-method comparison studies between hydride generation atomic absorption spectrometry (AAS) inductively coupled plasma atomic emission spectrometry (ICP-AES) and ICP-MS for arsenic and strontium show good agreement. (author)

Burn up determination of IEAR-1 fuel elements by non destructive gamma ray spectrometry method

International Nuclear Information System (INIS)

Soares, A.J.

1977-01-01

Measurement of nuclear fuel burn up by non destructive gamma ray spectrometry is discussed, and results of such measurements, made at the Instituto de Energia Atomica (IEA), are given. Specifically, the burn up of an MTR (Material Testing Reactor) fuel element removed from the IEAR-1 swimming pool reactor in 1958 is evaluated from the measured Cs-137 activity, which gives a single 661,6 keV gamma ray. Due to the long decay time of the test element, no other fission decay product activity could be detected. Analysis of measurements, made with a 3'' x 3'' NaI(Tl) detector at 330 distinct points of the element, showed the total burn up to 3.3 +- -+ 0.8 mg. This is in agreement with a calculated value. As the maximum temperature of IEAR-1 fuel elements is of the order of 40 0 C, migration effects of Cs-137 was not considered, this being significant only at fuel temperature in excess of 1000 0 C [pt

Preparation and certification of rice flour reference materials for trace elements analysis

International Nuclear Information System (INIS)

Cho, Kyung Haeng; Park, Chang Joon; Woo, Jin Choon; Suh, Jung Ki; Han, Myung Sub; Lee, Jong Hae

1998-01-01

Rice flour reference materials were prepared from the unpolished rice grown in korea and certified for elemental composition. The reference materials consist of two samples containing normal and high level. The reference material at elevated level was prepared by spiking to the normal rice flour six toxic elements of As, Cd, Cu, Cr, Hg, Pb with 1.0μg/g on a dry weight basis. Homogeneity of the prepared materials was evaluated through the determination of Ca, Cu, Fe, Mn, Zn by instrumental neutron activation analysis (INAA) and atomic absorption spectrometry (AAS). Small variance of elemental composition among inter-bottled samples assured homogeneity of the prepared materials. The materials were decomposed by high pres-sure digestion and microwave digestion method. INAA, AAS, inductively coupled plasma-atomic absorption spectrometry (ICP-AES), ICP-mass spectrometry (MS) and vapour generation techniques were employed to analyze the reference materials. From this independent analytical results, the certified or reference values are determined for As, Ca, Cd, Cr, Cu, Fe, Hg, K, Mg, Mn, Mo, Na, P, Pb, Se, Zn

Major and Trace Element Analysis of Natural and Experimental Igneous Systems using LA-ICP-MS

Science.gov (United States)

Jenner, Frances E.; Arevalo, Ricardo D., Jr.

2016-01-01

Major- and trace-element compositions of minerals provide valuable information on a variety of global Earth-system processes, including melting of distinct mantle reservoirs, the growth and evolution of the Earths crust and the formation of economically viable ore deposits. In the mid-1980s and early 1990s, attempts were made to couple laser ablation (LA) systems to inductively coupled plasma mass spectrometry (ICPMS) instruments (e.g. Fryer et al. 1995; Jackson et al. 1992). The goal was to develop a rapid, highly sensitive in situ analytical technique to measure abundances and spatial distributions of trace elements in minerals and other geological samples. Elemental analysis using LAICPMS was envisaged as a quicker and less destructive means of chemical analysis (requiring only g quantities) than labour-intensive sample digestion and solution analysis (requiring mg-levels of material); and it would be a more cost-effective method than secondary ion mass spectrometry (SIMS) for the routine analysis of trace elements from solid samples. Furthermore, it would have lower limits-of-detection than electron probe microanalysis (EPMA) (e.g. Jackson et al. 1992; Eggins 2003).

Determination of trace elements in maifanite by outer cover electrode atomic emission spectrometry

Institute of Scientific and Technical Information of China (English)

LI Jianqiang; LU Yiqiang; JIANG Wei

2005-01-01

Maifanite is a nature medicinal stone used in many fields for long time. The research on it showed that there are many trace elements in maifanite. In this paper, 36 trace elements in maifanite were determined by outer cover electrode atomic emission spectrometry, and the determination conditions were studied systematically. The results show that the concentrafions of elements, which are beneficial to human health, are higher, and the elements harmful to people health such as As, Cd, Hg, Cr, and Pb are tiny in maifanite. The precision and the accuracy were also discussed.

The use of reference materials in the elemental analysis of biological samples

International Nuclear Information System (INIS)

Bowen, H.J.M.

1975-01-01

Reference materials (RMs) are useful to compare the accuracy and precision of laboratories and techniques. The desirable properties of biological reference materials are listed, and the problems of production, homogenization and storage described. At present there are only 10 biological RMs available compared with 213 geological and 520 metallurgical RMs. There is a need for more biological RMs including special materials for microprobe analysis and for in vivo activation analysis. A study of 650 mean values for elements in RM Kale, analysed by many laboratories, leads to the following conclusions. 61% of the values lie within +-10% of the best mean, and 80% lie within +-20% of the best mean. Atomic absorption spectrometry gives results that are 5-30% high for seven elements, while intrumental neutron activation analysis gives low and imprecise results for K. Other techniques with poor interlaboratory precision include neutron activation for Mg, polarography for Zn and arc-spectrometry for many elements. More than half the values for elements in Kale were obtained by neutron activation, confirming the importance of this technique and the need for RMs. As a rough estimate, 6 x 10 9 elemental analyses of biological materials are carried out each year, mostly by medical, agricultural and food scientists. It seems likely that a substantial percentage of these are inaccurate, a situation that might be improved by quality control using standard RMs. (author)

Neutron activation analysis of trace elements in rain water

International Nuclear Information System (INIS)

Luten, J.B.

1977-01-01

In this thesis the principles and practical aspects of activation analysis which are of direct importance in the analysis of rain water, are presented together with recent literature data on other techniques. Problems due to the storage of rain water samples are discussed. A multi-element method for the determination of trace elements in rain water by instrumental neutron activation analysis is described. Gamma ray spectrometry using Ge(Li) detectors offers the possibility to determine Na, Al, Cl, V, Mn, Co, Cu, Br and I in rain water samples of 2.5 ml after a 4-min irradiation in a thermal neutron flux of 5 x 10 13 n cm -2 s -1 . In residues of rain water samples of 100 ml, irradiated during 2 days in a thermal neutron flux of >5 x 10 13 n cm -2 s -1 Cr, Fe, Co, Zn and Sb can be determined after a cooling period of approximately 21 days. The detection limits are lower than those reported in previous investigations except for Cu. The precision is about 10% or better, except for Co, Cu and I. A routine method for the determination of bromine and iodine in rain water by n.a.a. is presented. The elements are isolated by isotope exchange between the irradiated sample and a solution of Br 2 or I 2 in CCl 4 . The method is not sensitive to the chemical species in which the halogen is present. Irradiation of solutions of iodine compounds in a high thermal neutron flux gives rise to the formation of iodate. Results of a further investigation of this phenomenon are given, as well as the determination of iodate in rain water by n.a.a. Iodate is separated by anion exchange. The combination of n.a.a. and solvent extraction is used for the determination of five trace elements (V, Co, Cu, Zn and In) in 10-ml rain water samples. For V, Co and Cu this method is more sensitive and reproducible than instrumental n.a.a. The results of the analysis of eleven sequential 30-ml samples from the beginning of the shower are presented as an illustration of possible applications of the

Analysis of trace elements in ceramic prints on automobile glasses for forensic examination using high-energy synchrotron radiation x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Nishiwaki, Yoshinori; Takatsu, Masahisa; Miyamoto, Naoki; Watanabe, Seiya; Shimoda, Osamu; Muratsu, Seiji; Nakanishi, Toshio; Nakai, Izumi

2007-01-01

This study revealed that high-energy SRXRF (synchrotron radiation X-ray fluorescence spectrometry) utilizing 75.5 keV X-rays of SPring-8 is a powerful technique for trace elemental analysis of ceramic prints on automotive glasses for forensic examination. Fragments of 99 ceramic prints were collected from automobiles of various manufacturers, types and model years. Their major heavy element-components were found to be either Pb or Bi. Because of recent environment protection movement for lead-free material, there was a tendency of the shift of material from the Pb Type to the Bi Type with years of the production. A utilization of 75.5 keV X-rays as excitation source allowed us to detect trace heavy-elements, such as Sb, La, Ce, Hf and W, as well as relatively light-elements, such as V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Zr and Mo, in samples using K series of XRF emission lines. XRF intensities of these elements normalized by those of the major heavy-elements (Pb or Bi) became characteristic finger prints, showing the identity of each sample with a size of less than 0.5x0.5 mm 2 . The mean relative standard deviations of the normalized XRF intensities measured for the three fragments of each sample were less than 9.3%. These results show that the ceramic prints on automobile glasses contain rich elemental information for discrimination, and therefore the materials can be important evidence for practical forensic examinations. (author)

Stable isotope dilution analysis by thermal ionization mass spectrometry. Pt. 2

International Nuclear Information System (INIS)

Broekman, A.; Raaphorst, J.G. van

1984-01-01

The combination of stable isotope dilution analysis (SIDA) and thermal ionization mass spectrometry (TIMS) is in use for lead and uranium determination at milligram per kilogram levels for over 20 years. However, several other elements can also be determined accurately by SIDA/TIMS. In this study the determinations of cadmium and copper are described. Details of the digestion, electrochemical and ion-exchange separations and the loading of the elements on a filament are given. The advantages of the SIDA/TIMS technique are shown and illustrated with results for several certified reference materials. (orig.) [de

Quantitative analysis of major and trace elements in NH4HF2-modified silicate rock powders by laser ablation - inductively coupled plasma mass spectrometry.

Science.gov (United States)

Zhang, Wen; Hu, Zhaochu; Liu, Yongsheng; Yang, Wenwu; Chen, Haihong; Hu, Shenghong; Xiao, Hongyan

2017-08-29

In this paper, we described a NH 4 HF 2 digestion method as sample preparation for the rapid determination of major and trace elements in silicate rocks using laser ablation-inductively coupled plasma mass spectrometry (LA-ICP-MS). Sample powders digested by NH 4 HF 2 at 230 °C for 3 h form ultrafine powders with a typical grain size d 80  rocks have a consistent grain morphology and size, allowing us to produce pressed powder pellets that have excellent cohesion and homogeneity suitable for laser ablation micro-analysis without the addition of binder. The influences of the digestion parameters were investigated and optimized, including the evaporation stage of removing residual NH 4 HF 2 , sample homogenization, selection of the digestion vessel and calibration strategy of quantitative analysis. The optimized NH 4 HF 2 digestion method was applied to dissolve six silicate rock reference materials (BCR-2, BHVO-2, AGV-2, RGM-2, GSP-2, GSR-1) covering a wide range of rock types. Ten major elements and thirty-five trace elements were simultaneously analyzed by LA-ICP-MS. The analytical results of the six reference materials generally agreed with the recommended values, with discrepancies of less than 10% for most elements. The analytical precision is within 5% for most major elements and within 10% for most trace elements. Compared with previous methods of LA-ICP-MS bulk analysis, our method enables the complete dissolution of refractory minerals, such as zircon, in intermediate-acidic intrusive rocks and limits contamination as well as the loss of volatile elements. Moreover, there are many advantages for the new technique, including reducing matrix effects between reference materials and samples, spiking the internal standard simply and feasibly and sample batch processing. The applicability filed of the new technique in this study was focused on the whole-rock analysis of igneous rock samples, which are from basic rocks to acid rocks (45% rock analysis

Determination of rare-earth elements in rocks by isotope-excited X-ray fluorescence spectrometry

DEFF Research Database (Denmark)

Kunzendorf, Helmar; Wollenberg, H.A.

1970-01-01

Isotope-excited X-ray fluorescence spectrometry furnishes a rapid determination of rare-earth elements in unprepared rock samples. The samples are excited by 241Am γ-rays, generating X-ray spectra on a multichannel pulse-height analyser. Gaussian peaks of the Kα and Kβ X-ray energies are treated ......-ray spectrometric scan of a longitudinally sliced drill core showed a close correlation between rare-earth abundances and appropriate minerals.......Isotope-excited X-ray fluorescence spectrometry furnishes a rapid determination of rare-earth elements in unprepared rock samples. The samples are excited by 241Am γ-rays, generating X-ray spectra on a multichannel pulse-height analyser. Gaussian peaks of the Kα and Kβ X-ray energies are treated...

Determination of experimental conditions for the analysis of rare-earth elements by X-ray fluorescence spectrometry. Application to oxalates and potassium sulphate matrices

International Nuclear Information System (INIS)

Bayon Fuentes, A.; Bermudez Polonio, J.

1969-01-01

A previous theoretical and experimental study is carried out in order to analyze the rare earths elements by X-ray florescence spectrometry. All possible spectral interferences are considered. The working conditions for each element were selected, taking into account the peak/background ratio values for the following parameters: tungsten, molybdenum and chromium targets, current and voltage, analyzing crystals, and scintillation and flow proportional counters. Calibration curves were plotted showing the concentration of rare earths elements in oxalates and potassium sulphate matrices, and the theoretical detection limits for each element: are calculated. (Author) 8 refs

Development of a procedure for the multi-element determination of trace elements in wine by ICP-MS

Energy Technology Data Exchange (ETDEWEB)

Castineira, M.M.; Brandt, R.; von Bohlen, A.; Jakubowski, N. [Institut fuer Spektrochemie und Angewandte Spektroskopie e.V., Dortmund (Germany)

2001-07-01

An inductively coupled plasma mass spectrometric (ICP-MS) procedure has been developed for the determination of trace elements in wine. The procedure consists in simple 1+1 dilution of the wine and semi-quantitative analysis (without external calibration) using In as internal standard. Thirty-one elements at concentrations ranging from 0.1 mg mL{sup -1} to 0.5 ng mL{sup -1} can be determined by ICP-MS analysis with and without digestion. It was investigated whether a matrix effect observed for EtOH in the wine matrix can be overcome by application of a micro-concentric nebulizer with a membrane desolvator (MCN 6000). The results obtained for the MCN 6000 are compared with those obtained by use of a conventional Meinhard nebulizer. It is shown that the observed matrix effect can only be compensated by use of an internal standard for the Meinhard nebulizer, but not for the MCN 6000. Results for ICP-MS are compared with those obtained by total reflection X-ray fluorescence spectrometry (TXRF). (orig.)

Enantiomer-specific analysis of multi-component mixtures by correlated electron imaging-ion mass spectrometry

NARCIS (Netherlands)

Rafiee Fanood, M.M.; Ram, N.B.; Lehmann, C.S.; Powis, I.; Janssen, M.H.M.

2015-01-01

Simultaneous, enantiomer-specific identification of chiral molecules in multi-component mixtures is extremely challenging. Many established techniques for single-component analysis fail to provide selectivity in multi-component mixtures and lack sensitivity for dilute samples. Here we show how

Speciation of protein-bound trace elements by gel electrophoresis and atomic spectrometry.

Science.gov (United States)

Ma, Renli; McLeod, Cameron W; Tomlinson, Kerry; Poole, Robert K

2004-08-01

The metabolism of trace elements, in particular their binding to proteins in biological systems is of great importance in biochemical, toxicological, and pharmacological studies. As a result there has been a sustained interest over the last two decades in the speciation of protein-bound metals. Various analytical approaches have been employed, combining efficient separation of metalloproteins by liquid chromatography or electrophoresis with high-sensitivity elemental detection. Slab-gel electrophoresis (GE) is a key platform for high-resolution protein separation, and has been combined with autoradiography and various atomic spectrometric techniques for in-gel determination of protein-bound metals. Recently, the combination of GE with state-of-the-art inductively coupled plasma-mass spectrometry (ICP-MS), particularly when linked to laser ablation (LA) for direct gel interrogation, has opened up new opportunities for rapid characterization of metalloproteins. The use of GE and atomic spectrometry for the speciation of protein-bound trace elements is reviewed in this paper. Technical requirements for gel electrophoresis/atomic spectrometric measurement are considered in terms of method compatibilities, detection capability and potential usefulness. The literature is also surveyed to illustrate current status and future trends. Copyright 2004 Wiley-VCH Verlag GmbH and Co.

ICP Mass and Optical Emission Spectrometry of Ore Samples Containing Rare Earth Elements

International Nuclear Information System (INIS)

Mohammed, A.E.W.M.

2013-01-01

Inductively Coupled Plasma Optical Emission and Mass Spectrometry (ICP-OES and ICPMS) are widely accepted as a rapid and sensitive techniques for Rare Earth Elements (REEs) analysis of geological samples. However, the achievable accuracy of these techniques are seriously limited by the problem of matrix interferences. In this study, matrix effects in ICP-AES were addressed using two approaches. In the first approach, the mechanisms of matrix interferences and analyte excitation were elucidated fundamentally. First, matrix effects from a comprehensive list of thirty-nine elements were investigated. It was confirmed that matrix elements with low second (instead of the widely reported first) ionization potentials (IP) produce a stronger matrix effect in all cases. Another critical parameter defining the severity of the matrix effect was found to be the availability of low-lying energy levels in the doubly charged matrix ion. Penning ionization followed by ion electron recombination through successive cycles is proposed as the mechanism for the more severe matrix effects caused by low second-IP matrices. In the second approach ICP-OES and ICP-MS are applied in this study for the analysis of Rare Earth Elements of two selected standard reference samples namely AGV-2 and BCR-2 beside a fluorspar geological sample (G-9 sample). Effective procedures are developed to avoid the spectral interference from matrix elements by using ion exchange resin Amberlite IR-120 before determination of REEs using ICP-OES and ICPMS. The potential of the method is evaluated by analysis of Certified Reference Materials (AGV-2 and BCR-2). Results obtained by ICP-MS show that experimental data are in agreement with the certified values and their values could be used as a quantitative data. The results obtained using ICP-OES were compared and discussed.

Application of inductively coupled plasma mass spectrometry (ICP/MS) to detection of trace elements, heavy metals and radioisotopes in scalp hair

International Nuclear Information System (INIS)

Ozturk, Yildirim; Benderli, Cihan

2010-01-01

Trace element analysis of human hair has the potential to reveal retrospective information about an individual's nutritional status and exposure. As trace elements are incorporated into the hair during the growth process, longitudinal segments of the hair may reflect the body burden during the growth period. it was evaluated the potential of human hair to indicate exposure or nutritional status over time by analysing trace element profiles in single strands of human hair. By using inductively coupled plasma mass spectrometry (ICP-MS), it was achieved profiles of 43 elements in single strands of human hair. It was shown that trace element analysis along single strands of human hair can yield information about essential and toxic elements and for some elements, can be correlated with seasonal changes in diet and exposure. The information obtained from the trace element profiles of human hair in this study substantiates the potential of hair as a biomarker

Integrated Process Design and Control of Multi-element Reactive Distillation Processes

DEFF Research Database (Denmark)

Mansouri, Seyed Soheil; Sales-Cruz, Mauricio; Huusom, Jakob Kjøbsted

2016-01-01

In this work, integrated process design and control of reactive distillation processes involving multi-elements is presented. The reactive distillation column is designed using methods and tools which are similar in concept to non-reactive distillation design methods, such as driving force approach....... The methods employed in this work are based on equivalent element concept. This concept facilitates the representation of a multi-element reactive system as equivalent binary light and heavy key elements. First, the reactive distillation column is designed at the maximum driving force where through steady...

Direct trace-elemental analysis of urine samples by laser ablation-inductively coupled plasma mass spectrometry after sample deposition on clinical filter papers.

Science.gov (United States)

Aramendía, Maite; Rello, Luis; Vanhaecke, Frank; Resano, Martín

2012-10-16

Collection of biological fluids on clinical filter papers shows important advantages from a logistic point of view, although analysis of these specimens is far from straightforward. Concerning urine analysis, and particularly when direct trace elemental analysis by laser ablation-inductively coupled plasma mass spectrometry (LA-ICPMS) is aimed at, several problems arise, such as lack of sensitivity or different distribution of the analytes on the filter paper, rendering obtaining reliable quantitative results quite difficult. In this paper, a novel approach for urine collection is proposed, which circumvents many of these problems. This methodology consists on the use of precut filter paper discs where large amounts of sample can be retained upon a single deposition. This provides higher amounts of the target analytes and, thus, sufficient sensitivity, and allows addition of an adequate internal standard at the clinical lab prior to analysis, therefore making it suitable for a strategy based on unsupervised sample collection and ulterior analysis at referral centers. On the basis of this sampling methodology, an analytical method was developed for the direct determination of several elements in urine (Be, Bi, Cd, Co, Cu, Ni, Sb, Sn, Tl, Pb, and V) at the low μg L(-1) level by means of LA-ICPMS. The method developed provides good results in terms of accuracy and LODs (≤1 μg L(-1) for most of the analytes tested), with a precision in the range of 15%, fit-for-purpose for clinical control analysis.

Head of detector for multi-element analysis

International Nuclear Information System (INIS)

Frynta, Z.

1983-01-01

The detector head mounted on the scintillation counter consists of a hollow hexagonal rotary support axially arranged with the photomultiplier of the scintillation counter. In the walls of the hexagonal rotary support there are openings in which are inserted absorption filters. The mounting of the absorption filters on the rotary support allows the analysis of a greater number of elements without the dismantling of the head and the replacement of filters. The suitable geometry of the head is retained so that it is possible to insert the head into the hollows similarly as the scintillation counter. (J.P.)

Multielement ultratrace analysis in tungsten using secondary ion mass spectrometry

International Nuclear Information System (INIS)

Wilhartitz, P.; Virag, A.; Friedbacher, G.; Grasserbauer, M.

1987-01-01

The ever increasing demands on properties of materials create a trend also towards ultrapure products. Characterization of these materials is only possible with modern, highly sophisticated analytical techniques such as activation analysis and mass spectrometry, particularly SSMS, SIMS and GDMS. Analytical strategies were developed for the determination of about 40 elements in a tungsten matrix with high-performance SIMS. Difficulties like the elimination of interferences had to be overcome. Extrapolated detection limits were established in the range of pg/g (alkali metals, halides) to ng/g (e.g. Ta, Th). Depth profiling and ion imaging gave additional information about the lateral and the depth distribution of the elements. (orig.)

Modeling of Plutonium Ionization Probabilities for Use in Nuclear Forensic Analysis by Resonance Ionization Mass Spectrometry

Science.gov (United States)

2016-12-01

masses collide, they form a supercritical mass . Criticality refers to the neutron population within the system. A critical system is one that can...Spectrometry, no. 242, pp. 161–168, 2005. [9] S. Raeder, “Trace analysis of actinides in the environment by means of resonance ionization mass ...first ionization potential of actinide elements by resonance ionization mass spectrometry.” Spectrochimica Acta part B: Atomic Spectroscopy. vol. 52

Simultaneous determination of macro and trace elements in biological reference materials by microwave induced plasma optical emission spectrometry with slurry sample introduction

Energy Technology Data Exchange (ETDEWEB)

Matusiewicz, Henryk E-mail: Henryk.Matusiewicz@put.poznan.pl; Golik, Bartosz

2004-05-21

A slurry sampling technique (SST) has been utilized for simultaneous multi-element analysis by microwave-induced plasma optical emission spectrometry (MIP-OES). Slurry samples from a spray chamber are fed directly into the microwave cavity-torch assembly (power 300 W) with no desolvation apparatus. The performance of SST-MIP-OES was demonstrated by the determination of macro (Na, K, Ca, Mg, P) and trace (Cd, Cu, Mn, Sr, Zn) elements in three biological certified reference materials using a V-groove, clog-free Babington-type nebulizer. Slurry concentrations up to 1% m/v (particles <20 {mu}m), prepared in 10% HNO{sub 3} (pH 1.2) containing 0.01% of Triton X-100, were used with calibration by the standard additions method. The method offers relatively good precision (R.S.D. ranged from 7 to 11%) with measured concentrations being in satisfactory agreement with certified values for NRCC TORT-1 (Lobster hepatopancreas), NRCC LUTS-1 (Lobster hepatopancreas) and IAEA-153 (Milk powder). The concentrations of Na, K, Ca, Mg, P and Cd, Cu, Mn, Sr, Zn were determined in the range 90-22 000 {mu}g/g and 1-420 {mu}g/g, respectively. The method could be useful as a routine procedure.

Neutron activation analysis of lipsticks using gamma-ray spectrometry

International Nuclear Information System (INIS)

Mirsa, G.; Mittal, V.K.

2004-01-01

Neutron activation analysis with gamma-ray spectrometry was used to measure the concentrations of various elements in lipsticks of popular Indian and foreign brands. The aim of the present work was to study the possibility of existence of trace elements in samples of lipsticks (the ingredients of which are mostly organic in nature) and to see whether trace elements could distinguish lipsticks of different Indian and foreign brands from the forensic point of view apart from their inter-se differentiation. In the different samples of lipsticks that were analysed the following elements were detected: Au, Ba, Br, Ca, Cs, Fe, Na, Ru, Sb, Sc, Ta, Yb, Zn, Rb and Se. It was found that inter-se differentiation of lipsticks was possible on the basis of concentrations of trace elements and their profile. Concentration of bromine in samples of lipsticks identified lipsticks of different Indian brands. Samples of lipsticks of Indian and foreign brands could be differentiated on the basis of concentrations of cesium, antimony and scandium which were found to be higher in foreign brands as compared to those in Indian brands. (authors)

Dual element ((15)N/(14)N, (13)C/(12)C) isotope analysis of glyphosate and AMPA by derivatization-gas chromatography isotope ratio mass spectrometry (GC/IRMS) combined with LC/IRMS.

Science.gov (United States)

Mogusu, Emmanuel O; Wolbert, J Benjamin; Kujawinski, Dorothea M; Jochmann, Maik A; Elsner, Martin

2015-07-01

To assess sources and degradation of the herbicide glyphosate [N-(phosphonomethyl) glycine] and its metabolite AMPA (aminomethylphosphonic acid), concentration measurements are often inconclusive and even (13)C/(12)C analysis alone may give limited information. To advance isotope ratio analysis of an additional element, we present compound-specific (15)N/(14)N analysis of glyphosate and AMPA by a two step derivatization in combination with gas chromatography/isotope ratio mass spectrometry (GC/IRMS). The N-H group was derivatized with isopropyl chloroformate (iso-PCF), and remaining acidic groups were subsequently methylated with trimethylsilyldiazomethane (TMSD). Iso-PCF treatment at pH 10 indicated decomposition of the derivative. At pH 10, and with an excess of iso-PCF by 10-24, greatest yields and accurate (15)N/(14)N ratios were obtained (deviation from elemental analyzer-IRMS: -0.2 ± 0.9% for glyphosate; -0.4 ± 0.7% for AMPA). Limits for accurate δ(15)N analysis of glyphosate and AMPA were 150 and 250 ng injected, respectively. A combination of δ(15)N and δ(13)C analysis by liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) (1) enabled an improved distinction of commercial glyphosate products and (2) showed that glyphosate isotope values during degradation by MnO2 clearly fell outside the commercial product range. This highlights the potential of combined carbon and nitrogen isotopes analysis to trace sources and degradation of glyphosate.

Characterisation of synthetic multi-element standards (SMELS) used for the validation of k(o)-NAA

Czech Academy of Sciences Publication Activity Database

Vermaercke, P.; Robouch, P.; Eguskiza, M.; De Corte, F.; Kennedy, G.; Smodiš, B.; Jaćimović, R.; Yonezawa, C.; Matsue, H.; Lin, X.; Blaauw, M.; Kučera, Jan

2006-01-01

Roč. 564, č. 2 (2006), s. 675-682 ISSN 0168-9002 Institutional research plan: CEZ:AV0Z10480505 Keywords : neutron activation analysis * ko-standardization * multi-element standard Subject RIV: CB - Analytical Chemistry, Separation

Game meat authentication through rare earth elements fingerprinting

International Nuclear Information System (INIS)

Danezis, G.P.; Pappas, A.C.; Zoidis, E.; Papadomichelakis, G.; Hadjigeorgiou, I.; Zhang, P.; Brusic, V.; Georgiou, C.A.

2017-01-01

Accurate labelling of meat (e.g. wild versus farmed, geographical and genetic origin, organic versus conventional, processing treatment) is important to inform the consumers about the products they buy. Meat and meat products declared as game have higher commercial value making them target to fraudulent labelling practices and replacement with non-game meat. We have developed and validated a new method for authentication of wild rabbit meat using elemental metabolomics approach. Elemental analysis was performed using rapid ultra-trace multi-element measurement by inductively coupled plasma mass spectrometry (ICP-MS). Elemental signatures showed excellent ability to discriminate the wild rabbit from non-wild rabbit meat. Our results demonstrate the usefulness of metabolic markers -rare earth signatures, as well as other trace element signatures for game meat authentication. - Highlights: • Elemental metabolomics is a powerful new methodology for authentication of game rabbit meat. • New method for meat authentication utilizing rare earths elemental signatures. • Samples are compared to group signatures using angular and Euclidean distances. • Meat reference materials (>70 elements) can be used for cross-comparison between studies.

Chemical analysis of useful trace elements in sea water

International Nuclear Information System (INIS)

Katoh, Shunsaku; Fujii, Ayako; Miyai, Yoshitaka; Sakane, Kohji; Ogata, Noboru.

1983-01-01

The methods for the analysis of useful trace elements in sea water which have been tried so far are reviewed, and these methods are described briefly from the standpoint of studying the collection of resources. Ag and Au can be determined by concentrating sea water by ion-exchange method, solvent extraction method and electrodeposition method, then the elements are measured quantitatively by activation analysis and atomic absorption spectrochemical analysis. Sr, B and Li, which exist in relatively high concentration in sea water, are determined easily by atomic absorption spectrochemical analysis and absorption spectrometry. U, Mo and V are measured suitably by concentrating the elements by coprecipitation or solvent extraction method, and measuring by fluorescence analysis and arsenazo-3 method for U and through graphite-atomic absorption analysis for Mo and V. It has been revealed that the concentration of Ag and Au in sea water is extremely low, accordingly the recovery study is not conducted recently. On the other hand, the adsorption method using hydrated titanium oxide and amidoxim adsorbents for U, Mo and V, the adsorption method using aluminum adsorbent for Li, and the adsorption method using magnesium oxide and zirconium hydroxide and the solvent extraction method for B are hopeful to recover these elements. (Yoshitake, I.)

Recent advances in on-line coupling of capillary electrophoresis to atomic absorption and fluorescence spectrometry for speciation analysis and studies of metal-biomolecule interactions

International Nuclear Information System (INIS)

Li Yan; Yin Xuebo; Yan Xiuping

2008-01-01

Speciation information is vital for the understanding of the toxicity, mobility and bioavailability of elements in environmental or biological samples. Hyphenating high resolving power of separation techniques and element-selective detectors provides powerful tools for studying speciation of trace elements in environmental and biological systems. During the last five years several novel hybrid techniques based on capillary electrophoresis (CE) and atomic spectrometry have been developed for speciation analysis and metal-biomolecule interaction study in our laboratory. These techniques include CE on-line coupled with atomic fluorescence spectrometry (AFS), chip-CE on-line coupled with AFS, CE on-line coupled with flame heated quartz furnace atomic absorption spectrometry (FHF-AAS), and CE on-line coupled with electrothermal atomic absorption spectrometry (ETAAS). The necessity for the development of these techniques, their interface design, and applications in speciation analysis and metal-biomolecule interaction study are reviewed. The advantages and limitations of the developed hybrid techniques are critically discussed, and further development is also prospected

Theoretical background and implementation of the finite element method for multi-dimensional Fokker-Planck equation analysis

Czech Academy of Sciences Publication Activity Database

Král, Radomil; Náprstek, Jiří

2017-01-01

Roč. 113, November (2017), s. 54-75 ISSN 0965-9978 R&D Projects: GA ČR(CZ) GP14-34467P; GA ČR(CZ) GA15-01035S Institutional support: RVO:68378297 Keywords : Fokker-Planck equation * finite element method * simplex element * multi-dimensional problem * non-symmetric operator Subject RIV: JM - Building Engineering OBOR OECD: Mechanical engineering Impact factor: 3.000, year: 2016 https://www.sciencedirect.com/science/ article /pii/S0965997817301904

Multi-Element Analysis and Geochemical Spatial Trends of Groundwater in Rural Northern New York

Directory of Open Access Journals (Sweden)

Michael O’Connor

2010-05-01

Full Text Available Samples from private wells (n = 169 throughout St. Lawrence County, NY were analyzed by ICP-MS multi-element techniques. St. Lawrence County spans three diverse bedrock terranes including Precambrian crystalline rocks of the Adirondack Lowlands (mostly paragneisses and Highlands (mostly orthogneisses, as well as Paleozoic sedimentary rocks of the St. Lawrence Valley. An ArcGIS database was constructed and used to generate contour plots for elements across the county. Strontium isotopes and unique geochemical signatures were used to distinguish water from various geologic units. The results were consistent with a large (7,309 km2, sparsely populated (~110,000, rural region with diverse bedrock and glacial cover.

Standard test methods for chemical analysis of ceramic whiteware materials using wavelength dispersive X-Ray fluorescence spectrometry

CERN Document Server

American Society for Testing and Materials. Philadelphia

2004-01-01

1.1 These test methods cover the determination of ten major elements (SiO2, Al2O3, Fe2O3, MgO, CaO, Na2O, K2O, TiO2, P2O5, MnO, and LOI in ceramic whitewares clays and minerals using wavelength dispersive X-ray fluorescence spectrometry (WDXRF). The sample is first ignited, then fused with lithium tetraborate and the resultant glass disc is introduced into a wavelength dispersive X-ray spectrometer. The disc is irradiated with X-rays from an X-ray tube. X-ray photons emitted by the elements in the samples are counted and concentrations determined using previously prepared calibration standards. (1) In addition to 10 major elements, the method provides a gravimetric loss-on-ignition. Note 1—Much of the text of this test method is derived directly from Major element analysis by wavelength dispersive X-ray fluorescence spectrometry, included in Ref (1). 1.2 Interferences, with analysis by WDXRF, may result from mineralogical or other structural effects, line overlaps, and matrix effects. The structure of the...

Analysis of Rare Earth Elements in Geologic Samples using Inductively Coupled Plasma Mass Spectrometry; US DOE Topical Report - DOE/NETL-2016/1794

Energy Technology Data Exchange (ETDEWEB)

Bank, Tracy L. [AECOM, Pittsburgh, PA (United States); Roth, Elliot A. [National Energy Technology Lab. (NETL), Pittsburgh, PA, (United States); Tinker, Phillip [AECOM, Pittsburgh, PA (United States); Granite, Evan [National Energy Technology Lab. (NETL), Pittsburgh, PA, (United States)

2016-04-17

Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is used to measure the concentrations of rare earth elements (REE) in certified standard reference materials including shale and coal. The instrument used in this study is a Perkin Elmer Nexion 300D ICP-MS. The goal of the study is to identify sample preparation and operating conditions that optimized recovery of each element of concern. Additionally, the precision and accuracy of the technique are summarized and the drawbacks and limitations of the method are outlined.

A site-specific and multi-element isotopic approach to origin inference of sugars in foods and beverages

International Nuclear Information System (INIS)

Martin, M.L.; Martin, G.J.; Guillou, C.

1991-01-01

A strategy is presented for the characterization of sugars according to their botanical origin. The samples fermented in standardized conditions can be described in the multi-dimensional space of the overall carbon isotope ratio of ethanol measured by isotope ratio mass spectrometry (IRMS) and of the specific hydrogen isotope parameters of the methyl and methylene sites derived from nuclear magnetic resonance investigation of site-specific natural isotope fractionation (SNIF-NMR method). In the comparison of natural juices, the deuterium and oxygen-18 parameters of water extracted from the juice and from the end fermentation medium also contain information on the origin of the product. The isotopic effects of the concentration processes leading to concentrated juices, musts and syrups can be estimated and taken into account in interpreting the data. The classification power of this multi-element and multi-site approach is illustrated by discriminant analyses involving selected isotopic variables associated with pineapple, apple and barley sugars, compared to beet and cane sugars which are common sources of enrichment. The ability of the method to detect adulteration by exogenous sugars is improved when environmental conditions can be taken into account. (authors)

Multi-element RIMS Analysis of Genesis Solar Wind Collectors

Science.gov (United States)

Veryovkin, I. V.; Tripa, C. E.; Zinovev, A. V.; King, B. V.; Pellin, M. J.; Burnett, D. S.

2009-12-01

The samples of Solar Wind (SW) delivered by the NASA Genesis mission, present significant challenges for surface analytical techniques, in part due to severe terrestrial contamination of the samples on reentry, in part due to the ultra-shallow and diffused ion implants in the SW collector materials. We are performing measurements of metallic elements in the Genesis collectors using Resonance Ionization Mass Spectrometry (RIMS), an ultra-sensitive analytical method capable of detecting SW in samples with lateral dimensions of only a few mm and at concentrations from above one ppm to below one ppt. Since our last report at 2008 AGU Fall Meeting, we have (a) developed and tested new resonance ionization schemes permitting simultaneous measurements of up to three (Ca, Cr, and Mg) elements, and (b) improved reproducibility and accuracy of our RIMS analyses for SW-like samples (i.e. shallow ion implants) by developing and implementing an optimized set of new analytical protocols. This is important since the quality of scientific results from the Genesis mission critically depends on the accuracy of analytical techniques. In this work, we report on simultaneous RIMS measurements of Ca and Cr performed on two silicon SW collector samples, (#60179 and #60476). First, we have conducted test experiments with 3×1013 at/cm2 52Cr and 44Ca implants in silicon to evaluate the accuracy of our quantitative analyses. Implant fluencies were measured by RIMS to be 2.73×1013 and 2.71×1013 at/cm2 for 52Cr and 44Ca, respectively, which corresponds to an accuracy of ≈10%. Using the same implanted wafer as a reference, we conducted RIMS analyses of the Genesis samples: 3 spots on #60179 and 4 spots on #60476. The elemental SW fluencies expected for Cr and Ca are 2.95×1010 and 1.33×1011 at/cm2 , respectively. Our measurements of 52Cr yielded 3.0±0.6×1011 at/cm2 and 5.1±4.1×1010 at/cm2 for #60179 and #60476, respectively. For 40Ca, SW fluencies of 1.39±0.70×1011 at/cm2 in #60179

Resonance enhanced laser mass spectrometry for process- and environmental-analysis: Applications and perspectives

International Nuclear Information System (INIS)

Zimmermann, Ralf; Dorfner, Ralph; Kettrup, Antonius; Heger, Hans Joerg; Boesl, Ulrich

1998-01-01

Laser induced Resonance-Enhanced Multi-Photon Ionization Time-Of-Flight Mass Spectrometry (REMPI TOFMS) is a highly selective as well as sensitive analytical technique, well suited for species selective, on-line monitoring of trace-substances. In this contribution some analytical applications of a mobile REMPI-TOFMS are presented. This includes REMPI-TOMS on-line analysis of coffee roasting gas and waste incineration flue gas as well as headspace measurements of pulp processing lye or rapid analysis of polycyclic aromatic hydrocarbons from soil samples via thermal desorption

Analysis of burnt nuclear fuel elements by gamma-spectrometry

International Nuclear Information System (INIS)

Lammer, M.

1978-01-01

Gamma-spectrometry allows a non-destructive determination of the fission and activation product content of spent nuclear fuel. The concentration of some of these products depends significantly on the so-called fuel parameters which describe the irradiation history and the fuel composition. The use of these dependences for deriving ''unknown fuel parameters'' from measured fission product activities is investigated in this work. Relevant application fields are burnup determination, fuel testing and inspections within the nuclear materials safeguards programme. The present thesis investigates how these dependences can be used to derive unknown fuel parameters. The possibilities and basic limitations of deriving information from a measured gamma spectrum are considered on principle. The main conclusion is that only ratios of fission product activities allow the development of an interpretation method which is generally applicable to all types of fuel from different reactors. The dependence of activity ratios on cooling time, irradiation time, integrated and final neutron flux, fuel composition, as well as fission and breeding rates are then investigated and presented graphically in a way suitable for applicaton. These relationships can be used for the analysis of spent fuel, and the detailed procedures, which depend on the applicaton field, are worked out in this work. In order to test the interpretation methods, samples of nuclear fuel have been irradiated and the gamma spectra analysed. The methods developed in this work can be applied successfully to the analysis of burnt fuel in the frame of fuel testing programmes and to safeguards verification purposes. If however, apart from a gamma spectrum, no information on the investigated fuel is available, the above-mentioned parameters can be derived with low accuracy only. (author)

Direct atomic spectrometric analysis by slurry atomisation: Pt. 7. Analysis of coal using inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Ebdon, Les; Foulkes, M E; Parry, H G.M.; Tye, C T

1988-09-01

The application of slurry atomisation - inductively coupled plasma mass spectrometry (ICP-MS) to major, minor and trace element determination in coals has been investigated. Eight certified reference material (CRM) coals have been ground by the bottle and bead method and analysed using both rapid scan semi-quantitative analysis, employing a single rhodium internal standard, and full quantitative analysis using simple aqueous standards for calibration. The semi-quantitative mode, which determines the concentration using the mass-response curve for 68 elements against the single internal standard, produced values which were within a factor of two of the certified reference value, in most instances. The full quantitative determination gave excellent agreement with the certified reference material coals for a large number of elemental constituents. The results from the determination of 16 elements of interest are discussed including the effects of polyatomic interferents and isotope sensitivity.

Neutron activation analysis of trace elements in foodstuffs

International Nuclear Information System (INIS)

Schelenz, R.; Fischer, E.

1976-05-01

A neutron activation method for multielement determination in biological material was developed. The individual steps of the method include radiochemical processing as well as nondestructive techniques. In order to develop a high resolution gamma spectrometric method the indispensable assumptions were the application of Ge(Li)-semiconductor detectors, multi-channel pulse height analyzers and the use of electronic data evaluation with mini-computers for the automatic evaluation of complex gamma spectra. After radiochemical separation (RNAA) 33 elements can be determined in biological materials and by application of nondestructive, purely instrumental techniques (INAA) 25 elements. The time required for the analysis of 33 elements can be determined in biological materials and by application of nondestructive, purely instrumental techniques (INAA) 25 elements. The time required for the analysis of 33 elements is 4 days. The neutron activation method is used routinely for the determination of trace elements in foodstuffs and in the field of nutrition research. (orig.) [de

Multivariate analysis method for energy calibration and improved mass assignment in recoil spectrometry

International Nuclear Information System (INIS)

El Bouanani, Mohamed; Hult, Mikael; Persson, Leif; Swietlicki, Erik; Andersson, Margaretha; Oestling, Mikael; Lundberg, Nils; Zaring, Carina; Cohen, D.D.; Dytlewski, Nick; Johnston, P.N.; Walker, S.R.; Bubb, I.F.; Whitlow, H.J.

1994-01-01

Heavy ion recoil spectrometry is rapidly becoming a well established analysis method, but the associated data analysis processing is still not well developed. The pronounced nonlinear response of silicon detectors for heavy ions leads to serious limitation and complication in mass gating, which is the principal factor in obtaining energy spectra with minimal cross talk between elements. To overcome the above limitation, a simple empirical formula with an associated multiple regression method is proposed for the absolute energy calibration of the time of flight-energy dispersive detector telescope used in recoil spectrometry. A radical improvement in mass assignment was realized, which allows a more accurate and improved depth profiling with the important feature of making the data processing much easier. ((orig.))

Intercomparison and determination of trace elements in urban dust by neutron activation analysis

International Nuclear Information System (INIS)

Chung, Yong Sam; Moon, Jong Hwa; Kim, Sun Ha; Park, Kwang Won; Kang, Sang Hun

2000-01-01

Trace elements in air samples artificially loaded on filters with urban dust and the bulk material of urban dust as an environmental sample were determined non-destructively using instrumental neutron activation analysis. Standard reference material (Urban Dust, SRM 1648) of the National Institute of Standard and Technology was used for the analytical quality control. The relative error for 37 elements was less than 15% and the standard deviation was less than 10%. 29 elements in the urban dust and 21 elements in the loaded filter sample were determined respectively. To evaluate the proficiency and reliability of the measurement, data intercomparison was performed and 39 analytical laboratories participated in the analysis using different analytical methods; neutron activation analysis, particle induced X-ray emission analysis, X-ray fluorescence analysis and atomic absorption spectrometry. Z-scores were calculated using the standard deviation of the laboratory's mean as target standard deviation, and a good result was obtained that the values fall between-1 and +1 except some elements. (author)

Application of high resolution x-ray spectrometry preceded by neutron activation for elemental analysis of soil samples

International Nuclear Information System (INIS)

Hernandez Rivero, A.; Capote Rodriguez, G.; Padilla Alvarez, R.; Herrera Peraza, E.

1997-01-01

Utilization of High Resolution X-Ray Spectrometry preceded by activation of the samples by irradiation with neutron fluxes (NAA-RX) is a relatively modern trend in application of nuclear techniques. This method may complement advantageously the usual Neutron Activation Analysis by means of Gamma Spectrometry (NAA-G). In this work results obtained by the application of NAA-RX for non-destructive analysis of Cuban soil samples are discussed. The samples were irradiated with reactor neutron fluxes and the induced characteristic X-rays were measured by using Si(Li)-detector. Concentrations of Fe, Zn and Eu as determined by NAA-RX are compared with both NAA-G and XRF data. For the elaboration of X-Ray and Gamma Spectra the computer programs AXIL and ACTAN were used respectively. (author) [es

Application of high resolution x-ray spectrometry preceded by neutron activation for elemental analysis of soil samples

International Nuclear Information System (INIS)

Hernandez Rivero, A.; Capote Rodriguez, G.; Herrera Peraza, E.

1996-01-01

Utilization of High Resolution X-Ray Spectrometry preceded by activation of the samples by irradiation with neutron fluxes (NAA R X) is a relatively modern trend in application of nuclear techniques. This method may complement advantageously the usual Neutron Activation Analysis by means of Gamma Spectrometry (NAA-G) In this work results obtained by the application of NAA-RX for non-destructive analysis of Cuban soil samples are discussed. The samples were irradiated with reactor neutron fluxes and the induced characteristic X-rays were measured by using Si(li)-detector. Concentrations of Fe, Zn and Eu as determined by NAA-RX are compared with both NAA-G and XRF data. For the elaboration of X-ray and Gamma Spectra the computer programs AXIL and ACTAN were used respectively

Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Oliveira Souza, Sidnei de; Silvério Lopes da Costa, Silvânio; Santos, Dayane Melo; Santos Pinto, Jéssica dos; Garcia, Carlos Alexandre Borges

2014-01-01

An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg −1 for Mn to 77.3 mg kg −1 for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento — MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES). - Highlights: • Determination of inorganic constituents in mineral fertilizers was proposed. • Experimental design methodology was used to optimize analytical method. • The sample preparation procedure using diluted reagents (HNO 3 and H 2 O 2 ) was employed. • The analytical method was satisfactorily to the determination of thirteen elements. • The ICP OES technique can be

Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Oliveira Souza, Sidnei de [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); Silvério Lopes da Costa, Silvânio [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); Coordenação de Química, Universidade Federal de Alagoas (UFAL), Campus Arapiraca, 57309-005, Arapiraca, AL (Brazil); Santos, Dayane Melo; Santos Pinto, Jéssica dos; Garcia, Carlos Alexandre Borges [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); and others

2014-06-01

An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg{sup −1} for Mn to 77.3 mg kg{sup −1} for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento — MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES). - Highlights: • Determination of inorganic constituents in mineral fertilizers was proposed. • Experimental design methodology was used to optimize analytical method. • The sample preparation procedure using diluted reagents (HNO{sub 3} and H{sub 2}O{sub 2}) was employed. • The analytical method was satisfactorily to the determination of thirteen elements. • The

Multidimensional elemental analysis with the Sandia nuclear microprobe

International Nuclear Information System (INIS)

Doyle, B.L.

1988-01-01

It is well known that many of the ion beam analysis techniques such as Rutherford backscattering spectrometry, elastic recoil detection, resonant and nonresonant nuclear reaction analysis can be used to nondestructively obtain concentration depth profiles of elements in solids. When these techniques are combined with the small beam spot capabilities of a scanned nuclear microprobe, sample composition can be determined in up to three dimensions. This paper will review the various procedures used to collect and analyze multidimensional data using the Sandia nuclear microprobe. In addition, examples of how these data are being used in the study of materials will be shown. (author)

New developments in glow discharge optical emission and mass spectrometry

International Nuclear Information System (INIS)

Hoffmann, Volker; Dorka, Roland; Wilken, Ludger; Wetzig, Klaus

2000-01-01

This paper describes new developments in flow discharge optical emission (GD-OES) and mass spectrometry (GD-MS) at IFW and presents corresponding new applications (analysis of microelectronic multi-layer system by radio frequency glow discharge optical emission spectrometry (RF-GD-OES) and analysis of pure iron by a new Grimm-type GD-MS source)

Elemental content profiles in propolis from several cities of Turkey

Directory of Open Access Journals (Sweden)

Canan Aksoy

2017-08-01

Full Text Available Background: Macro-element content profiles in propolis that have been previously used in traditional folk medicine have provided enough information to develop a classification of the geological origin of propolis. Within this study, we aim to contribute our research to existing literatüre, particularly through our use of EDXRF spectroscopy, which has not been used to study propolis before. The results of the study led us to conclude that the residues of heavy metals were a limited concentration in Turkish propolis samples. Objective: The purpose of this study was to investigate the macro-element profiles in Turkish propolis from 18 different cities of Turkey. Methods: The macro-element of 22 raw propolis samples were investigated using Energy-Dispersive X-ray fluorescence spectrometry. Results: Turkish Propolis was discovered to be rich with minerals of potassium, sodium which could be more beneficial in human nutrition. Potassium content was at a relatively higher level than other elements in these samples, while calcium content was at alower level in those samples from various regions of Turkey. Conclusion: The elements of propolis that we studied were distinctive enough to make the discrimination of propolis from different locations in Turkey possible. The quantification by energy-dispersive X-ray fluorescence spectrometry procedures provided good resolution of multi-element analysis in propolis samples.

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

Science.gov (United States)

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

2018-05-11

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

Stable Chlorine Isotopes and Elemental Chlorine by Thermal Ionization Mass Spectrometry and Ion Chromatography; Martian Meteorites, Carbonaceous Chondrites and Standard Rocks

Science.gov (United States)

Nakamura, N.; Nyquist, L. E.; Reese, Y.; Shih, C.-Y.; Fujitani, T.; Okano, O.

2011-01-01

Recently significantly large mass fractionation of stable chlorine isotopes has been reported for terrestrial and lunar samples [1,2]. In addition, in view of possible early solar system processes [3] and also potential perchlorate-related fluid/microbial activities on the Martian surface [4,5], a large chlorine isotopic fractionation might be expected for some types of planetary materials. Due to analytical difficulties of isotopic and elemental analyses, however, current chlorine analyses for planetary materials are controversial among different laboratories, particularly between IRMS (gas source mass spectrometry) and TIMS (Thermal Ionization Mass Spectrometry) groups [i.e. 1,6,7] for isotopic analyses, as well as between those doing pyrohydrolysis and other groups [i.e. 6,8]. Additional careful investigations of Cl isotope and elemental abundances are required to confirm real chlorine isotope and elemental variations for planetary materials. We have developed a TIMS technique combined with HF-leaching/ion chromatography at NASA JSC that is applicable to analysis of small amounts of meteoritic and planetary materials. We present here results for several standard rocks and meteorites, including Martian meteorites.

Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

Science.gov (United States)

de Oliveira Souza, Sidnei; da Costa, Silvânio Silvério Lopes; Santos, Dayane Melo; dos Santos Pinto, Jéssica; Garcia, Carlos Alexandre Borges; Alves, José do Patrocínio Hora; Araujo, Rennan Geovanny Oliveira

2014-06-01

An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg- 1 for Mn to 77.3 mg kg- 1 for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento - MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES).

Multi elemental analysis of indigenous food spices in Southern Ethiopia using INAA technique

International Nuclear Information System (INIS)

Melkegna, T.H.; Chaubey, A.K.; Beyene, G.A.; Bitewlign, T.A.

2017-01-01

The objective of this study is a quantitative and qualitative analysis of essential and trace elements of four indigenous Ethiopian spices and herbs using instrumental neutron activation analysis technique. Results obtained for 16 elements: Major elements; Mg, Cl, and K; Minor elements; Na, Fe, and Mn, Zn, Br. While Al, V, Sm, Sc, La, Ba, Eu, Rb were found in traces. The spices, Affromumom korarima and Lippa Adonesis var. Koseret sebsebe were found to be very good sources of essential trace elements like Fe, Zn and Mn. The highest concentration of Mg was found in Ajowan whereas K and Fe were measured in Coriander seeds. The average daily dietary intake of some essential elements from the use of these spices were found to be below the recommended upper limit by WHO. (author)

Multidisciplinary approach and multi-scale elemental analysis and separation chemistry

International Nuclear Information System (INIS)

Mariet, Clarisse

2014-01-01

The development of methods for the analysis of trace elements is an important component of my research activities either for a radiometric measure or mass spectrometric detection. Many studies raise the question of the chemical signature of a sample or a process: eruptive behavior of a volcano, indicator of pollution, ion exchange in vectors vesicles of active principles,... Each time, highly sensitive analytical procedures, accurate and multi-elementary as well as the development of specific protocols were needed. Neutron activation analysis has often been used as reference procedure and allowed to validate the chemical lixiviation and the measurement by ICP-MS. Analysis of radioactive samples requires skills in analysis of trace but also separation chemistry. Two separation methods occupy an important place in the separation chemistry of radionuclides: chromatography and liquid-liquid extraction. The study of extraction of Lanthanide (III) by the oxide octyl (phenyl)-n, N-diisobutyl-carbamoylmethyl phosphine (CMPO) and a calixarene-CMPO led to better understand and quantify the influence of operating conditions on their performance of extraction and selectivity. The high concentration of salts in aqueous solutions required to reason in terms of thermodynamic activities in relying on a comprehensive approach to quantification of deviations from ideality. In order to reduce the amount of waste generated and costs, alternatives to the hydrometallurgical extraction processes were considered using ionic liquids at low temperatures as alternative solvents in biphasic processes. Remaining in this logic of effluent reduction, miniaturization of the liquid-liquid extraction is also study so as to exploit the characteristics of microscopic scale (very large specific surface, short diffusion distances). The miniaturization of chromatographic separations carries the same ambitions of gain of volumes of wastes and reagents. The miniaturization of the separation Uranium

Coulomb matrix elements in multi-orbital Hubbard models.

Science.gov (United States)

Bünemann, Jörg; Gebhard, Florian

2017-04-26

Coulomb matrix elements are needed in all studies in solid-state theory that are based on Hubbard-type multi-orbital models. Due to symmetries, the matrix elements are not independent. We determine a set of independent Coulomb parameters for a d-shell and an f-shell and all point groups with up to 16 elements (O h , O, T d , T h , D 6h , and D 4h ). Furthermore, we express all other matrix elements as a function of the independent Coulomb parameters. Apart from the solution of the general point-group problem we investigate in detail the spherical approximation and first-order corrections to the spherical approximation.

Trace and ultratrace level elemental and speciation analysis

International Nuclear Information System (INIS)

Arunachalam, J.

2012-01-01

Accurate determination of elements present at parts per million and billion levels in various matrices is a growing requirement in different fields. In environmental sciences various trace elements need to be analyzed so as establish the dispersal models of pollutants or the adequacy of effluent treatment prior to discharge into water bodies. The issues of bioaccumulation and magnification are important in aquatic systems. In nutrition and biochemistry one has to establish the bio-availability of essential and toxic elemental species as toxic elements prevent assimilation of essential elements. Fission and fusion technologies use a variety of structural materials requiring many trace elements to be present at levels strictly below the specified levels. Ultra-pure bulk semiconductor materials are required for fabrication devices. In metallurgy and materials sciences too, various trace elements are known to influence the properties. In the emerging fields like nanotechnology, it is necessary to understand the passage and accumulation of nano-particles inside the cells, through trace analysis. Many analytical techniques exist which can provide the concentration information in the bulk materials with good accuracy. They include ICP-AES, FAAS, and ICP-MS, which are solution based techniques. Direct solid state analytical techniques are Glow Discharge Mass Spectrometry (GDMS) and XRF. Accelerator based ion-beam analysis techniques can provide information on concentration and depth profiles of different elements in layered structures. Hyphenated techniques such as HPLC/lC-ICPMS, are helpful in identifying various chemical oxidation states in which a given element might be present in a matrix, which is termed as speciation analysis. This presentation will include the existing analytical competencies and the laboratory requirements for trace and ultra trace element elemental and speciation analyses and their applications. (author)

High-resolution continuum source atomic absorption spectrometry for the simultaneous or sequential monitoring of multiple lines. A critical review of current possibilities

International Nuclear Information System (INIS)

Resano, M.; Flórez, M.R.; García-Ruiz, E.

2013-01-01

This work examines the capabilities and limitations of commercially available high-resolution continuum source atomic absorption spectrometry instrumentation for multi-line monitoring, discussing in detail the possible strategies to develop multi-element methodologies that are truly simultaneous, or else sequential, but from the same sample aliquot. Moreover, the simultaneous monitoring of various atomic or molecular lines may bring other important analytical advantages, such as: i) expansion of the linear range by monitoring multiplets; ii) improvements in the limit of detection and in precision by summing the signals from different lines of the same element or molecule; iii) simple correction for matrix-effects by selecting a suitable internal standard; or iv) accurate mathematical correction of spectral overlaps by simultaneous monitoring of free lines of the interfering molecule or element. This work discusses how authors have made use of these strategies to develop analytical methodologies that permit the straightforward analysis of complex samples. - Highlights: • HR CS AAS potential for simultaneous multi-line monitoring is critically examined. • Strategies to develop simultaneous multi-element methods are discussed. • Other benefits of multi-line monitoring (e.g., use of an IS or LSBC) are highlighted. • Selected examples from the literature are discussed in detail

Segmentation of Multi-Isotope Imaging Mass Spectrometry Data for Semi-Automatic Detection of Regions of Interest

Science.gov (United States)

Poczatek, J. Collin; Turck, Christoph W.; Lechene, Claude

2012-01-01

Multi-isotope imaging mass spectrometry (MIMS) associates secondary ion mass spectrometry (SIMS) with detection of several atomic masses, the use of stable isotopes as labels, and affiliated quantitative image-analysis software. By associating image and measure, MIMS allows one to obtain quantitative information about biological processes in sub-cellular domains. MIMS can be applied to a wide range of biomedical problems, in particular metabolism and cell fate [1], [2], [3]. In order to obtain morphologically pertinent data from MIMS images, we have to define regions of interest (ROIs). ROIs are drawn by hand, a tedious and time-consuming process. We have developed and successfully applied a support vector machine (SVM) for segmentation of MIMS images that allows fast, semi-automatic boundary detection of regions of interests. Using the SVM, high-quality ROIs (as compared to an expert's manual delineation) were obtained for 2 types of images derived from unrelated data sets. This automation simplifies, accelerates and improves the post-processing analysis of MIMS images. This approach has been integrated into “Open MIMS,” an ImageJ-plugin for comprehensive analysis of MIMS images that is available online at http://www.nrims.hms.harvard.edu/NRIMS_ImageJ.php. PMID:22347386

Filterless preconcentration, flow injection analysis and detection by inductively-coupled plasma mass spectrometry

DEFF Research Database (Denmark)

Andersen, Jens Enevold Thaulov

The influence of interferences in the analysis of elements by inductively-coupled-plasma mass-spectrometry (ICP-MS) may be significantly diminished by utilising a protocol of flow-injection analysis (FIA). The method is based on filterless preconcentration of metallic elements at the walls...... of a knotted reactor that was made of nylon tubings. In the load mode, the preconcentration was accomplished by precipitation of metallic species in alkaline-buffered carriers onto the inner walls of the hydrofilic tube. After a preconcen-tration period of 40-120 seconds using sample volumes of 4-10 m...... of 10-30 were obtained in the analysis of aluminium, of chromium and of iron, which resulted in detection limits (3) down to 20 g/L at a sampling frequency of 50 per hour. The preconcentration protocol improves the selectivity thus allowing direct determination of the elements in saline media. Anionic...

Structural analysis of ITER multi-purpose deployer

International Nuclear Information System (INIS)

Manuelraj, Manoah Stephen; Dutta, Pramit; Gotewal, Krishan Kumar; Rastogi, Naveen; Tesini, Alessandro; Choi, Chang-Hwan

2016-01-01

Highlights: • System modelling for structural analysis of the Multi-Purpose Deployer (MPD). • Finite element modeling of the Multi-Purpose Deployer (MPD). • Static, modal and seismic response analysis of the Multi-Purpose Deployer (MPD). • Iterative structural analysis and design update to satisfy the structural criteria. • Modal analysis for various kinematic configurations. • Reaction force calculations on the interfacing systems. - Abstract: The Multi-Purpose Deployer (MPD) is a general purpose ITER in-vessel remote handling (RH) system. The main handling equipment, known as the MPD Transporter, consists of a series of linked bodies, which provide anchoring to the vacuum vessel port and an articulated multi-degree of freedom motion to perform various in-vessel maintenance tasks. During the in-vessel operations, the structural integrity of the system should be guaranteed against various operational and seismic loads. This paper presents the structural analysis results of the concept design of the MPD Transporter considering the seismic events. Static structural, modal and frequency response spectrum analyses have been performed to verify the structural integrity of the system, and to provide reaction forces to the interfacing systems such as vacuum vessel and cask. Iterative analyses and design updates are carried out based on the reference design of the system to improve the structural behavior of the system. The frequency responses of the system in various kinematics and payloads are assessed.

Nondestructive analysis of silver in gold foil using synchrotron radiation X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Kasamatsu, Masaaki; Suzuki, Yasuhiro; Suzuki, Shinichi; Nakanishi, Toshio; Shimoda, Osamu; Nishiwaki, Yoshinori; Miyamoto, Naoki

2005-01-01

Small particles of gold foil detached from an indoor decoration might be important evidence to associate a suspect with a crime scene. We have investigated the application of elemental analysis using synchrotron radiation X-ray fluorescence spectrometry to discriminate small particles of gold foil. Eight kinds of gold foil samples collected in Japan were used in the experiments. As a result of synchrotron radiation X-ray fluorescence spectrometry, only two elements, gold and silver, were detected from all gold foil samples. The intensity ratios of AgK α /AuL α showed good correlation with the content ratios of Ag/Au. The variation of intensity ratio within a same sample was sufficiently small compared with those of different samples. Therefore the comparison of this intensity ratio can be an effective method to discriminate small particles originating from different types of gold foil. (author)

Determination of 25 elements in biological standard reference materials by neutron activation analysis

International Nuclear Information System (INIS)

Guzzi, G.; Pietra, R.; Sabbioni, E.

1974-12-01

Standard and Certified Reference Materials programme of the JRC includes the determination of trace elements in complex biological samples delivered by the U.S. National Bureau of Standards: Bovine liver (NBS SRM 1577), Orchard Leaves (NBS SRM 1571) and Tomato Leaves. The study has been performed by the use of neutron activation analysis. Due to the very low concentration of some elements, radiochemical groups or elemental separation procedures were necessary. The paper describes the techniques used to analyse 25 elements. Computer assisted instrumental neutron activation analysis with high resolution Ge(Li) spectrometry was considerably advantageous in the determination of Na, K, Cl, Mn, Fe, Rb and Co and in some cases of Ca, Zn, Cs, Sc, and Cr. For low contents of Ca, Mg, Ni and Si special chemical separation schemes, followed by Cerenkov counting have been developped. Two other separation procedures allowing the determination of As, Cd, Ga, Hg, Mo, Cu, Sr Se, Ba and P have been set up. The first, the simplified one involves the use of high resolution Ge(Li) detectors, the second, the more complete one involves a larger number of shorter measurements performed by simpler and more sensitive techniques, such as NaI(Tl) scintillation spectrometry and Cerenkov counting. The results obtained are presented and discussed

Fast Multi-blind Modification Search through Tandem Mass Spectrometry*

Science.gov (United States)

Na, Seungjin; Bandeira, Nuno; Paek, Eunok

2012-01-01

With great biological interest in post-translational modifications (PTMs), various approaches have been introduced to identify PTMs using MS/MS. Recent developments for PTM identification have focused on an unrestrictive approach that searches MS/MS spectra for all known and possibly even unknown types of PTMs at once. However, the resulting expanded search space requires much longer search time and also increases the number of false positives (incorrect identifications) and false negatives (missed true identifications), thus creating a bottleneck in high throughput analysis. Here we introduce MODa, a novel “multi-blind” spectral alignment algorithm that allows for fast unrestrictive PTM searches with no limitation on the number of modifications per peptide while featuring over an order of magnitude speedup in relation to existing approaches. We demonstrate the sensitivity of MODa on human shotgun proteomics data where it reveals multiple mutations, a wide range of modifications (including glycosylation), and evidence for several putative novel modifications. Based on the reported findings, we argue that the efficiency and sensitivity of MODa make it the first unrestrictive search tool with the potential to fully replace conventional restrictive identification of proteomics mass spectrometry data. PMID:22186716

Homogenization on Multi-Materials’ Elements: Application to Printed Circuit Boards and Warpage Analysis

Directory of Open Access Journals (Sweden)

Araújo Manuel

2016-01-01

Full Text Available Multi-material domains are often found in industrial applications. Modelling them can be computationally very expensive due to meshing requirements. The finite element properties comprising different materials are hardly accurate. In this work, a new homogenization method that simplifies the computation of the homogenized Young modulus, Poisson ratio and thermal expansion coefficient is proposed, and applied to composite-like material on a printed circuit board. The results show a good properties correspondence between the homogenized domain and the real geometry simulation.

Determination of rare earth elements in high purity rare earth oxides by liquid chromatography, thermionic mass spectrometry and combined liquid chromatography/thermionic mass spectrometry

International Nuclear Information System (INIS)

Stijfhoorn, D.E.; Stray, H.; Hjelmseth, H.

1993-01-01

A high-performance liquid chromatographic (HPLC) method for the determination of rare earth elements in rocks has been modified and used for the determination of rare earth elements (REE) in high purity rare earth oxides. The detection limit was 1-1.5 ng or 2-3 mg/kg when a solution corresponding to 0.5 mg of the rare earth oxide was injected. The REE determination was also carried out by adding a mixture of selected REE isotopes to the sample and analysing the collected HPLC-fractions by mass spectrometry (MS) using a thermionic source. Since the matrix element was not collected, interference from this element during the mass spectrometric analysis was avoided. Detection limits as low as 0.5 mg/kg could then be obtained. Detection limits as low as 0.05 mg/kg were possible by MS without HPLC-pre-separation, but this approach could only be used for those elements that were not affected by the matrix. Commercial samples of high purity Nd 2 O 3 , Gd 2 O 3 and Dy 2 O 3 were analysed in this study, and a comparison of results obtained by HPLC, combined HPLC/MS and direct MS is presented. (Author)

Multi-element neutron activation analysis of Brazilian coal samples

International Nuclear Information System (INIS)

Atalla, L.T.; Requejo, C.S.

1982-09-01

The elements U, Th, La, Ce, Nd, Sm, Eu, Dy, Tb, Yb, Lu, Sc, Ta, Hf, Co, Ni, Cr, Mo, Ti, V, W, In, Ga, Mn, Ba, Sr, Mg, Rb, Cs, K, Cl, Br, As, Sb, Au, Ca, Al and Fe were determined in coal samples by instrumental neutron activation analysis, by using both thermal and epithermal neutron irradiations. The irradiation times were 10 minutes and 8 or 16 hours in a position where the thermal neutron flux was about 10 12 n.cm - 2 .s - 1 and 72 non-consecutive hours for epithermal irradiation at a flux of about 10 11 n.Cm - 2 .s - 1 . After the instrumental analysis of the above mentioned elements, Zn and Se were determined with chemical separation. The relative standard deviation of, at least, 4 determinations was about + - 10% for the majority of the results. The coal samples analysed were supplied by: Cia. Estadual da Tecnologia e Saneamento Basico (CETESB-SP), Cia. de Pesquisas e Lavras Minerais (COPELMI-RS), Cia. Carbonifera Urussunga (SC), Cia. Carbonifera Prospera (SC), Cia. Carbonifera Treviso (SC), Cia. Nacional de Mineracao de Carvao do Barro Branco (SC) and Comissao Nacional de Energia Nuclear (CNEN-RJ). (Author) [pt

Application of neutron activation analysis and inductively coupled plasma mass spectrometry to the determination of toxic and essential elements in Australian foods

International Nuclear Information System (INIS)

Fardy, J.J.; McOrist, G.D.; Farrar, Y.J.; Bowles, C.J.; Warner, I.M.; Tan Mingguang

1994-01-01

Current Australian Legislation specifies the maximum permitted levels of nine toxic elements in food while the National Health and Medical Research Council (NH and MRC) has listed recommended daily intake figures for seven essential elements. This investigation examined the compliance of Australian foods with both these requirements. Australia-wide samples of representative foods from the diets of Australians were used in this study after the NH and MRC kindly permitted us to join their Market Basket (Noxious Substance) Survey. Both toxic and essential element concentrations in these foods were determined using the advanced analytical techniques of instrumental (INAA) and radiochemical neutron activation analysis (RNAA) and inductively coupled plasma mass spectrometry (ICP-MS). With very few exceptions, foods do not exceed the maximum permitted levels for toxic substances. Daily intake figures for essential elements generally lie close to the maximum recommended values listed by NH and MRC. Since another source of toxic element intake is drinking water, samples from different locations were analyzed by NAA and inductively coupled plasma atomic emission spectroscopy (ICP-AES). They were extremely low in trace elements with the exception of copper, iron, zinc and lead which approached the maximum permitted concentrations. The performance of NAA and ICP-MS for analyzing biological materials were compared. NAA cannot match the superior sensitivity for a wider range of elements obtained by ICP-MS. This has been verified for a wide range of food materials. While NAA is an inconvenient and time-consuming technique for many applications, it does not suffer from blank problems after irradiation of the sample and becomes the preferred technique where low limits of detection are required for trace concentrations in solid samples. (author). 22 refs, 27 figs, 21 tabs

Association of glass fragments by their trace elemental content using ICP-MS and LA-ICP-MS in the analysis scheme

Science.gov (United States)

Almirall, Jose R.; Montero, Shirly; Furton, Kenneth G.

2002-08-01

The importance of glass as evidence of association between a crime event and a suspect has been recognized for some time. Glass is a fragile material that is often found at the scenes of crimes such as burglaries, hit-and-run accidents and violent crime offenses. The physical and chemical properties of glass can be used to differentiate between possible sources and as evidence of association between two fragments of glass thought to originate from the same source. Refractive index (RI) comparisons have been used for this purpose but due to the improved control over glass manufacturing processes, RI values often cannot differentiate glasses, even if the glass originates from different sources. Elemental analysis methods such as NAA, XRF, ICP-AES, and Inductively Coupled Plasma Mass Spectrometry (ICP-MS) have also been used for the comparison of trace elemental compositions and these techniques have been shown to provide an improvement in the discrimination of glass fragments over RI comparisons alone. The multi-element capability and the sensitivity of ICP-MS combined with the simplified sample introduction of laser ablation prior to ion detection provides for an excellent and relatively non-destructive technique for elemental analysis of glass fragments. The methodology for solution analysis (digestion procedure) and solid sample analysis (laser ablation) of glass is reported and the analytical results are compared. An isotope dilution method is also reported as a high precision technique for elemental analysis of glass fragments. The optimum sampling parameters for laser ablation, for semi-quantitative analysis and element ratio comparisons are also presented. Finally, the results of a case involving the breaking of 15 vehicle windows in an airport parking lot and the association of a suspect to the breakings by the glass fragments found on his person are also presented.

Electrothermal vaporisation ICP-mass spectrometry (ETV-ICP-MS) for the determination and speciation of trace elements in solid samples - A review of real-life applications from the author's lab

Energy Technology Data Exchange (ETDEWEB)

Vanhaecke, Frank; Resano, Martin; Moens, Luc [Laboratory of Analytical Chemistry, Ghent University, Institute for Nuclear Sciences, Proeftuinstraat 86, 9000 Ghent (Belgium)

2002-09-01

The use of electrothermal vaporisation (ETV) from a graphite furnace as a means of sample introduction in inductively coupled plasma mass spectrometry (ICP-MS) permits the direct analysis of solid samples. A multi-step furnace temperature programme is used to separate the vaporisation of the target element(s) and of the matrix components from one another. Sometimes, a chemical modifier is used to enable a higher thermal pre-treatment temperature, by avoiding premature analyte losses (stabilisation) or promoting the selective volatilisation of matrix components. In almost all instances, accurate results can be obtained via external calibration or single standard addition using an aqueous standard solution. Absolute limits of detection are typically 1 pg, which corresponds to 1 ng/g for a typical sample mass of 1 mg. Real-life applications carried out in the author's lab are used to illustrate the utility of this approach. These applications aim at trace element determination in industrial and environmental materials. The industrial materials analysed include different types of plastics - Carilon, polyethylene, poly(ethyleneterephtalate) and polyamide - and photo- and thermographic materials. As samples from environmental origin, plant material, animal tissue and sediments were investigated. Some applications aimed at a multi-element determination, while in other, the content of a single, but often challenging, element (e.g., Si or S) had to be measured. ETV-ICP-MS was also used in elemental speciation studies. Separation of Se-containing proteins was accomplished using polyacrylamide gel electrophoresis (PAGE). Subsequent quantification of the Se content in the protein spots was carried out using ETV-ICP-MS. As the volatilisation of methylmercury and inorganic mercury could be separated from one another with respect to time, no chromatographic or electrophoretic separation procedure was required, but ETV-ICP-MS as such sufficed for Hg speciation in fish tissue

Multielement determination and speciation of major-to-ultratrace elements in green tea leaves by ICP-AES and ICP-MS

International Nuclear Information System (INIS)

Matsuura, Hirotaka; Hokura, Akiko; Haraguchi, Hiroki

2000-01-01

In order to investigate the multi-elemental composition of green tea leaves as well as chemical species in tea infusions, inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS) were used for elemental analysis and elemental speciation with the aid of size exclusion chromatography (SEC). As a result, the multielement determination of major-to-ultratrace elements in green tea leaves and green tea infusions was carried out by ICP-AES and ICP-MS. About 40 elements in these tea samples could be determined in a wide concentration range of over 8 orders of magnitude. The extraction efficiency of each element was estimated as the ratio of its concentration in tea infusion to that in tea leaves. It was found from the experimental results that the elements in tea leaves could be classified into three characteristic groups, depending on their extraction efficiencies. Furthermore, tea infusions were analyzed by a combined system of SEC, UV absorption detector, and ICP-AES (or ICP-MS) for the speciation of major-to-ultratrace elements. Most of the elements in tea infusions were found to be present as associated complexes with large organic molecules. (author)

Computational analyses of spectral trees from electrospray multi-stage mass spectrometry to aid metabolite identification.

Science.gov (United States)

Cao, Mingshu; Fraser, Karl; Rasmussen, Susanne

2013-10-31

Mass spectrometry coupled with chromatography has become the major technical platform in metabolomics. Aided by peak detection algorithms, the detected signals are characterized by mass-over-charge ratio (m/z) and retention time. Chemical identities often remain elusive for the majority of the signals. Multi-stage mass spectrometry based on electrospray ionization (ESI) allows collision-induced dissociation (CID) fragmentation of selected precursor ions. These fragment ions can assist in structural inference for metabolites of low molecular weight. Computational investigations of fragmentation spectra have increasingly received attention in metabolomics and various public databases house such data. We have developed an R package "iontree" that can capture, store and analyze MS2 and MS3 mass spectral data from high throughput metabolomics experiments. The package includes functions for ion tree construction, an algorithm (distMS2) for MS2 spectral comparison, and tools for building platform-independent ion tree (MS2/MS3) libraries. We have demonstrated the utilization of the package for the systematic analysis and annotation of fragmentation spectra collected in various metabolomics platforms, including direct infusion mass spectrometry, and liquid chromatography coupled with either low resolution or high resolution mass spectrometry. Assisted by the developed computational tools, we have demonstrated that spectral trees can provide informative evidence complementary to retention time and accurate mass to aid with annotating unknown peaks. These experimental spectral trees once subjected to a quality control process, can be used for querying public MS2 databases or de novo interpretation. The putatively annotated spectral trees can be readily incorporated into reference libraries for routine identification of metabolites.

Critical comparison of performances of inductively coupled plasma atomic emission spectrometry and neutron activation analysis for the determination of elements in human lungs

International Nuclear Information System (INIS)

Alimonti, A.; Coni, E.; Caroli, S.; Sabbioni, E.; Nicolaou, G.E.; Pietra, R.

1989-01-01

A study was carried out to assess the performance of inductively coupled plasma atomic emission spectrometry (ICP-AES) and neutron activation analysis (NAA) techniques for determining reference values for Al, Cd, Cr, Cu, Mg, Mn, V and Zn in human lungs of urban non-smoking subjects. Experimental data were subjected to the usual basic statistical tests to evaluate the respective merits of the two basically different analytical techniques. Both approaches, if used under carefully optimised experimental conditions, can yield reliable results affected only minimally by systematic and random errors. On the other hand, on a more routine basis, particular attention should be paid to elements such as Al, Cd and V which may pose some problems with both techniques. (author)

Multi-element analysis of wheat flour and white bread by neutron activation

International Nuclear Information System (INIS)

Godinez A, M.A.

1994-01-01

One of the best source of feeding even for the human being as for animals are the Cereals. Although they are mainly energetic aliment, due to its composition in starch, they are a very important source of proteins and amino acids. They contribute mineral elements to the diet. Even those elements constitute a very small part of the total diet, they take a very important place in many human metabolic processes. To make a multielemental analysis of an aliment is very important that we are based on a very sensible analytic technique so we are able to find them, just as the Neutronic Activation. This Nuclear technique allows you to make a qualitative and quantitative analysis of the elements that are in a sample, but it does n't show the way in which the elements are presented. It is based in turning those elements into radioactive ones through its exposition to an uniform and constant fluid of neutrons, so then its radioactivity can be determined. The present work has as a main purpose to make a multielemental analysis of the wheat flour and white bread through the Neutronic Activation Technique, using the comparator method and establishing previously the most appropriate work conditions as much irradiation as digestion and measuring of the radioactivity of the sample. In this way, it was able to know that the wheat flour has potassium, chlorine, magnesium, sodium, iron, zinc, manganese, rubidium and selenium elements in a concentration of 2000, 700, 500, 25, 18, 13, 5.5, 0.9 and 0.01 - 0.3 mg/g respectively. In an other hand it was found that the white bread has the same elements than the wheat flour but its concentration was: 1700, 9000, 400, 7000, 52, 13, 6, 1 and 0.05 - 0.3 mg/g respectively. (Author)

X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Ray, N.B.

1977-01-01

The principle, instrument and procedure of X-ray fluorescence spectrometry are described. It is a rapid, simple and sensitive method for the trace analysis of elements from sodium to uranium in powder, liquid or metal samples. (M.G.B.)

Multi-Capillary Column-Ion Mobility Spectrometry of Volatile Metabolites Emitted by Saccharomyces Cerevisiae

Directory of Open Access Journals (Sweden)

Christoph Halbfeld

2014-09-01

Full Text Available Volatile organic compounds (VOCs produced during microbial fermentations determine the flavor of fermented food and are of interest for the production of fragrances or food additives. However, the microbial synthesis of these compounds from simple carbon sources has not been well investigated so far. Here, we analyzed the headspace over glucose minimal salt medium cultures of Saccharomyces cerevisiae using multi-capillary column-ion mobility spectrometry (MCC-IMS. The high sensitivity and fast data acquisition of the MCC-IMS enabled online analysis of the fermentation off-gas and 19 specific signals were determined. To four of these volatile compounds, we could assign the metabolites ethanol, 2-pentanone, isobutyric acid, and 2,3-hexanedione by MCC-IMS measurements of pure standards and cross validation with thermal desorption–gas chromatography-mass spectrometry measurements. Despite the huge biochemical knowledge of the biochemistry of the model organism S. cerevisiae, only the biosynthetic pathways for ethanol and isobutyric acid are fully understood, demonstrating the considerable lack of research of volatile metabolites. As monitoring of VOCs produced during microbial fermentations can give valuable insight into the metabolic state of the organism, fast and non-invasive MCC-IMS analyses provide valuable data for process control.

Multi Scale Finite Element Analyses By Using SEM-EBSD Crystallographic Modeling and Parallel Computing

International Nuclear Information System (INIS)

Nakamachi, Eiji

2005-01-01

A crystallographic homogenization procedure is introduced to the conventional static-explicit and dynamic-explicit finite element formulation to develop a multi scale - double scale - analysis code to predict the plastic strain induced texture evolution, yield loci and formability of sheet metal. The double-scale structure consists of a crystal aggregation - micro-structure - and a macroscopic elastic plastic continuum. At first, we measure crystal morphologies by using SEM-EBSD apparatus, and define a unit cell of micro structure, which satisfy the periodicity condition in the real scale of polycrystal. Next, this crystallographic homogenization FE code is applied to 3N pure-iron and 'Benchmark' aluminum A6022 polycrystal sheets. It reveals that the initial crystal orientation distribution - the texture - affects very much to a plastic strain induced texture and anisotropic hardening evolutions and sheet deformation. Since, the multi-scale finite element analysis requires a large computation time, a parallel computing technique by using PC cluster is developed for a quick calculation. In this parallelization scheme, a dynamic workload balancing technique is introduced for quick and efficient calculations

Multi-Element Lean Direct Injection Combustor Module, Phase I

Data.gov (United States)

National Aeronautics and Space Administration — We propose to develop a Multi-Element Lean Direct Injection, ME-LDI, Combustion concept with the following innovative features: 1. Independent, mini burning zones...

Design and Fabrication of High Gain Multi-element Multi-segment Quarter-sector Cylindrical Dielectric Resonator Antenna

Science.gov (United States)

Ranjan, Pinku; Gangwar, Ravi Kumar

2017-12-01

A novel design and analysis of quarter cylindrical dielectric resonator antenna (q-CDRA) with multi-element and multi-segment (MEMS) approach has been presented. The MEMS q-CDRA has been designed by splitting four identical quarters from a solid cylinder and then multi-segmentation approach has been utilized to design q-CDRA. The proposed antenna has been designed for enhancement in bandwidth as well as for high gain. For bandwidth enhancement, multi-segmentation method has been explained for the selection of dielectric constant of materials. The performance of the proposed MEMS q-CDRA has been demonstrated with design guideline of MEMS approach. To validate the antenna performance, three segments q-CDRA has been fabricated and analyzed practically. The simulated results have been in good agreement with measured one. The MEMS q-CDRA has wide impedance bandwidth (|S11|≤-10 dB) of 133.8 % with monopole-like radiation pattern. The proposed MEMS q-CDRA has been operating at TM01δ mode with the measured gain of 6.65 dBi and minimum gain of 4.5 dBi in entire operating frequency band (5.1-13.7 GHz). The proposed MEMS q-CDRA may find appropriate applications in WiMAX and WLAN band.

Results and comments on the gamma spectrometry examinations carried out on PWR and fast neutron fuel elements

International Nuclear Information System (INIS)

Pineira, Thomas; Mouchnino, Michel; Juste, Guy; Vignesoult, Nicole.

1980-05-01

The gamma spectrometry analyses on the fuel elements of PWR and fast neutron systems have experienced a significant growth in the CEA. This nondestructive, quick, inexpensive and quantitative method, seems to us particularly advantageous for qualifying the behavior of fuel under irradiation. However, in order to use it to the maximum, it must have reached a high degree of automation and the interpretation of the results must be the outcome of a coherent team that includes gamma spectrometry and fuel element specialists, since the growth of hot cell gamma spectrometry involves the processing of a considerable number of data upon which the quality of the results depends (large number of spectra per pencil analyzed, dimension of the 2000 or 4000 channel spectra, number of lines studied, etc.). Therefore the need to make the most of the information and, in particular, to present the results in a form suitable for direct processing in a minimum response time, requires a highly automated system. Further, the more specific results of gamma spectrometry correlated to the metallurgical results obtained in the laboratories should contribute efficiently to obtaining major information [fr

Radiochemical neutron activation analysis based multi-elemental analysis of high purity gallium

International Nuclear Information System (INIS)

Tashimova, F.A.; Sadikov, I.I; Salimov, M.I.; Zinov'ev, V.G.

2006-01-01

Full text: Gallium is one of the widely used materials in semiconductor and optoelectronics industry. Gallium is used to produce infrared detectors, piezoelectric sensors, high- and low-temperature transistors for space and defense technology. One of the most important requirements for semiconductor materials of gallium compounds is an excessive high purity for layers and films. Information on impurities (type of an impurity, concentration, character of distribution) is important as for better understanding of the physical and chemical processes taking place in formed semiconductor structures and for the 'know-how' of devices on their basis. The object of this work is to develop radiochemical neutron activation technique for analysis of high purity gallium. Irradiation of 0.1 g of gallium sample in neutron flux of 5·10 13 cm -2 s -1 for 5 hours will result in induced activity of more than 10 8 Bq, due to 72 Ga radionuclide, half-life of which is 14.1 hours. Therefore to perform instrumental NAA of gallium long period (10 day) cooling is required, and high sensitive determination of elements producing short- and long-lived radionuclides (T 1/2 72 Ga. We have studied the behavior of gallium in extraction-chromatographic system 'TBP-HCl'. The experiments have shown that higher factor of distribution (D) and capacity on gallium can be achieved when 'TBP-4M HCl' system is used. However more than 10 trace elements have high D and thus they cannot be separated from 72 Ga. To resolve the problem and increase the number of separated trace elements we have used preliminary satisfaction of chromatographic column with tellurium, which has D higher than the most of elements in 'TBP-4M HCl' system and thus suppresses extraction of elements. Distribution profile of gallium along the column and elution curve of 25 trace elements have been measured. Chemical yields of separated elements measured by using radiotracers are more than 93%. On the basis of the carried out researches

Operational trials of single- and multi-element CR-39 dosemeters for the DIDO and PLUTO reactors at the Harwell Laboratory

International Nuclear Information System (INIS)

Gallacher, G.G.; Perks, C.A.

1993-01-01

Single- and multi-element CR-39 dosemeters, developed at the Harwell Laboratory, and a commercially available multi-element CR-39 dosemeter (obtained from Track Analysis Systems Ltd), were evaluated for their potential as neutron dosemeters for personnel working at Harwell Laboratory's research reactors. Owing to the angular dependence of the CR-39 (processed using electrochemical etching), the single-element dosemeter was found to be impractical. Consequently, a multi-element dosemeter was developed, which consisted of a cube of side 36 mm with CR-39 elements (also processed using electrochemical etching) attached to each of the sides. Although this dosemeter was technically suitable for this type of dosimetry, it was considered to be unacceptably bulky in personnel trials. The commercially available CR-39 dosemeter tested was much smaller (the CR-39 was only chemically etched) and this was considered to be acceptable as a personnel dosemeter. In addition, trials with personnel working at active handling glove boxes indicated that single-element dosemeters might be adequate, but further work would be needed to verify this. (author)

Finite Element Analysis and Optimization for the Multi-stage Deep Drawing of Molybdenum Sheet

International Nuclear Information System (INIS)

Kim, Heung-Kyu; Hong, Seok Kwan; Kang, Jeong Jin; Heo, Young-moo; Lee, Jong-Kil; Jeon, Byung-Hee

2005-01-01

Molybdenum, a bcc refractory metal with a melting point of about 2600 deg. C, has a high heat and electrical conductivity. In addition, it remains strong mechanically at high temperatures as well as at low temperatures. Therefore it is a technologically very important material for the applications operating at high temperatures. However, a multi-stage process is required due to the low drawability for making a deep drawn part from the molybdenum sheet. In this study, a multi-stage deep drawing process for a molybdenum circular cup was designed by combining the drawing with the ironing, which was effective for the low drawability materials. A parametric study by FE analysis for the multi-stage deep drawing was conducted for evaluation of the design variables effect. Based on the FE analysis result, the multi-stage deep drawing process was parameterized by the design variables, and an optimum process design was obtained by the process optimization based on the FE simulation at each stage

Quantitative and qualitative analysis of fluoride and multi elements of shark teeth by PIXE

International Nuclear Information System (INIS)

Sakurai, S.; Asakawa, R.; Hirota, F.; Sato, T.; Sera, K.; Itoh, J.

2008-01-01

Biomineralization has two types, biologically induced mineralization (BIM) and biologically controlled mineralization (BCM). Shark teeth is a typical representative of BCM. We have measured concentrations of fluorine and multi elements in shark teeth collected in the south of Japan. As a result, it was confirmed that the sample preparation method, which was established for the biological samples, is applicable to the shark teeth samples and the elemental concentration was obtained in good accuracy and reproducibility. Moreover, we clarified that the shark teeth is composed of Fluorapatite by the combination with X-ray Diffraction. Fluorine concentration is found to be 5500 μg/g in the shark teeth. We have 100 samples of Shark teeth and are planning on reporting the findings of a study with larger samples in the near future. (author)

Study of quantitative analysis of rare earth elements (Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) in soil samples by inductively couple plasma mass spectrometry

International Nuclear Information System (INIS)

Truong Duc Toan; Nguyen Giang; Vo Tran Quang Thai; Do Tam Nhan; Nguyen Le Anh; Nguyen Viet Duc; Luong Thi Tham; Truong Thi Phuong Mai

2015-01-01

Method for the determination of 16 rare earth elements (REEs) in soil samples without separating by inductively coupled plasma mass spectrometry (ICP-MS) has been studied at Dalat Nuclear Research Institute. The optimal conditions for ICP-MS NexION 300X with three modes: Standard, Collision (KED), and Reaction (DRC) have been studied on the Montana II soil reference material. The result analysis shows that: DRC mode only gives good analysis result for Sc, Y, La, Ce, Pr, Nd, Tm, Yb, and Lu; Standard mode exhibits good analysis results for all elements with error from 1.2 - 29.0% and KED mode is the best one with error less than 15%. The concentrations of elements in the soil samples of Cau Dat, Bao Loc, and Da Lat were determined, which concentrations of REEs in soil samples of Cau Dat are higher than that of the other areas in Lam Dong Province. (author)

Clustering of samples and elements based on multi-variable chemical data

International Nuclear Information System (INIS)

Op de Beeck, J.

1984-01-01

Clustering and classification are defined in the context of multivariable chemical analysis data. Classical multi-variate techniques, commonly used to interpret such data, are shown to be based on probabilistic and geometrical principles which are not justified for analytical data, since in that case one assumes or expects a system of more or less systematically related objects (samples) as defined by measurements on more or less systematically interdependent variables (elements). For the specific analytical problem of data set concerning a large number of trace elements determined in a large number of samples, a deterministic cluster analysis can be used to develop the underlying classification structure. Three main steps can be distinguished: diagnostic evaluation and preprocessing of the raw input data; computation of a symmetric matrix with pairwise standardized dissimilarity values between all possible pairs of samples and/or elements; and ultrametric clustering strategy to produce the final classification as a dendrogram. The software packages designed to perform these tasks are discussed and final results are given. Conclusions are formulated concerning the dangers of using multivariate, clustering and classification software packages as a black-box

Mass spectrometry a versatile aid to inorganic analysis

International Nuclear Information System (INIS)

Stefani, Rene

1976-01-01

Several hundred publications have appeared in the last three years that deal with applications of Mass Spectrometry to inorganic analysis. Bulk and localized trace analysis, surface and thin film characterization and microstructure examination are currently performed by Secondary Ion Mass Spectrometry, Spark Source Mass Spectrometry and the newly developed Laser Probe Mass Spectrometry. Suitable experimental procedures allow insulators, biologic materials and microsamples to be analysed. In spite of the classification by techniques this review is essentially devoted to the most significant papers in analytical applications but instrumental and basic features are sometimes introduced to support the discussions

Development of an accurate, sensitive, and robust isotope dilution laser ablation ICP-MS method for simultaneous multi-element analysis (chlorine, sulfur, and heavy metals) in coal samples

International Nuclear Information System (INIS)

Boulyga, Sergei F.; Heilmann, Jens; Heumann, Klaus G.; Prohaska, Thomas

2007-01-01

A method for the direct multi-element determination of Cl, S, Hg, Pb, Cd, U, Br, Cr, Cu, Fe, and Zn in powdered coal samples has been developed by applying inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) with laser-assisted introduction into the plasma. A sector-field ICP-MS with a mass resolution of 4,000 and a high-ablation rate laser ablation system provided significantly better sensitivity, detection limits, and accuracy compared to a conventional laser ablation system coupled with a quadrupole ICP-MS. The sensitivity ranges from about 590 cps for 35 Cl + to more than 6 x 10 5 cps for 238 U + for 1 μg of trace element per gram of coal sample. Detection limits vary from 450 ng g -1 for chlorine and 18 ng g -1 for sulfur to 9.5 pg g -1 for mercury and 0.3 pg g -1 for uranium. Analyses of minor and trace elements in four certified reference materials (BCR-180 Gas Coal, BCR-331 Steam Coal, SRM 1632c Trace Elements in Coal, SRM 1635 Trace Elements in Coal) yielded good agreement of usually not more than 5% deviation from the certified values and precisions of less than 10% relative standard deviation for most elements. Higher relative standard deviations were found for particular elements such as Hg and Cd caused by inhomogeneities due to associations of these elements within micro-inclusions in coal which was demonstrated for Hg in SRM 1635, SRM 1632c, and another standard reference material (SRM 2682b, Sulfur and Mercury in Coal). The developed LA-ICP-IDMS method with its simple sample pretreatment opens the possibility for accurate, fast, and highly sensitive determinations of environmentally critical contaminants in coal as well as of trace impurities in similar sample materials like graphite powder and activated charcoal on a routine basis. (orig.)

Development of an accurate, sensitive, and robust isotope dilution laser ablation ICP-MS method for simultaneous multi-element analysis (chlorine, sulfur, and heavy metals) in coal samples.

Science.gov (United States)

Boulyga, Sergei F; Heilmann, Jens; Prohaska, Thomas; Heumann, Klaus G

2007-10-01

A method for the direct multi-element determination of Cl, S, Hg, Pb, Cd, U, Br, Cr, Cu, Fe, and Zn in powdered coal samples has been developed by applying inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) with laser-assisted introduction into the plasma. A sector-field ICP-MS with a mass resolution of 4,000 and a high-ablation rate laser ablation system provided significantly better sensitivity, detection limits, and accuracy compared to a conventional laser ablation system coupled with a quadrupole ICP-MS. The sensitivity ranges from about 590 cps for (35)Cl+ to more than 6 x 10(5) cps for (238)U+ for 1 microg of trace element per gram of coal sample. Detection limits vary from 450 ng g(-1) for chlorine and 18 ng g(-1) for sulfur to 9.5 pg g(-1) for mercury and 0.3 pg g(-1) for uranium. Analyses of minor and trace elements in four certified reference materials (BCR-180 Gas Coal, BCR-331 Steam Coal, SRM 1632c Trace Elements in Coal, SRM 1635 Trace Elements in Coal) yielded good agreement of usually not more than 5% deviation from the certified values and precisions of less than 10% relative standard deviation for most elements. Higher relative standard deviations were found for particular elements such as Hg and Cd caused by inhomogeneities due to associations of these elements within micro-inclusions in coal which was demonstrated for Hg in SRM 1635, SRM 1632c, and another standard reference material (SRM 2682b, Sulfur and Mercury in Coal). The developed LA-ICP-IDMS method with its simple sample pretreatment opens the possibility for accurate, fast, and highly sensitive determinations of environmentally critical contaminants in coal as well as of trace impurities in similar sample materials like graphite powder and activated charcoal on a routine basis.

Multi-element isotope dilution analyses using ICP-MS

International Nuclear Information System (INIS)

Volpe, A.M.

1996-01-01

Presently, 37 elements ranging from light (Li,B) through transition metals, noble, rare earth and heavy elements, to actinides and transuranics (Pu, Am, Cm) are measured by isotope dilution at Lawrence Livermore National Laboratory. Projects range from geological and hydrological to biological. The research goal is to measure accurately many elements present in diverse matrices at trace (ppb) levels using isotope dilution methods. Major advantages of isotope dilution methods are accuracy, elimination of ion intensity calibration, and quantitation for samples that require chemical separation. Accuracy depends on tracer isotope calibration, tracer-sample isotopic equilibration, and appropriate background, isobaric and mass bias corrections. Propagation of isotope ratio error due to improper tracer isotope addition is a major concern with multi-element analyses when abundances vary widely. 11 refs., 3 figs

Application of energy dispersive XRF-spectrometry to analyse nutritional elements in relation to cancer

International Nuclear Information System (INIS)

Hota, P.K.; Vijayan, V.; Singh, L.P.

2001-01-01

Food is the principal media for intake of elements from environment to human body. Thus, it is felt important to determine the daily dietary intake of such elements in the field of toxicity and nutrition, the deficiency or sufficiency of which may lead to various diseases, disorders and allergies in human health. In this study, the elements present in commonly used cereals, pulses, noodles, some condiments/spices, tobacco products, some common leaves used in herbal medicine and tea leaves have been analyzed using EDXRF spectrometry technique. Elemental concentrations of K, Ca, Fe, Sr, Mn, Zn, Cu, Pb, As and Se are detected and quantified in all the samples using this method. The results are discussed in relation to cancer. (author)

Sampling strategy and analysis of trace element concentrations by inductively coupled plasma mass spectrometry on medieval human bones--the concept of chemical life history.

Science.gov (United States)

Skytte, Lilian; Rasmussen, Kaare Lund

2013-07-30

Medieval human bones have the potential to reveal diet, mobility and treatment of diseases in the past. During the last two decades trace element chemistry has been used extensively in archaeometric investigations revealing such data. Many studies have reported the trace element inventory in only one sample from each skeleton - usually from the femur or a tooth. It cannot a priori be assumed that all bones or teeth in a skeleton will have the same trace element concentrations. Six different bone and teeth samples from each individual were carefully decontaminated by mechanical means. Following dissolution of ca. 20 mg sample in nitric acid and hydrogen peroxide the assays were performed using inductively coupled plasma mass spectrometry (ICPMS) with quadropole detection. We describe the precise sampling technique as well as the analytical methods and parameters used for the ICPMS analysis. The places of sampling in the human skeleton did exhibit varying trace element concentrations. Although the samples are contaminated by Fe, Mn and Al from the surrounding soil where the bones have been residing for more than 500 years, other trace elements are intact within the bones. It is shown that the elemental ratios Sr/Ca and Ba/Ca can be used as indicators of provenance. The differences in trace element concentrations can be interpreted as indications of varying diet and provenance as a function of time in the life of the individual - a concept which can be termed chemical life history. A few examples of the results of such analyses are shown, which contains information about provenance and diagenesis. Copyright © 2013 John Wiley & Sons, Ltd.

Thirteenth ISMAS symposium cum workshop on spectrometry

International Nuclear Information System (INIS)

Aggarwal, S.K.; Jaison, P.G.; Alamelu, D.

2008-01-01

Mass spectrometry is an important analytical tool and finds applications in almost all branches of science and technology like Physics, Chemistry, Biology, Material Science, Geology, Nuclear Science, Industry, Oceanography, Environment etc. Innovations in the designs of mass spectrometers coupled with new ionization techniques have further strengthened the capabilities of mass spectrometry for analyzing all types of molecules including thermally labile and non-volatile at concentrations down to femto gram levels. The applications of mass spectrometry to the biomedical sciences have provided a unique, easy and fast approach to genomics, proteomics and metabolomics. The availability of different types of mass spectrometers for inorganic elemental and isotopic composition determination have strengthened the role of mass spectrometry for analyzing all elements starting from hydrogen onwards. It is now possible to carry out speciation analysis using electrospray mass spectrometry. The individual conference papers in the proceedings covers fundamentals of mass spectrometry, qualitative and quantitative aspects and data interpretation, maintenance of mass spectrometers, selection of mass spectrometer, and recent advances in the field. Papers relevant to INIS are indexed separately

The multi-element probabilistic collocation method (ME-PCM): Error analysis and applications

International Nuclear Information System (INIS)

Foo, Jasmine; Wan Xiaoliang; Karniadakis, George Em

2008-01-01

Stochastic spectral methods are numerical techniques for approximating solutions to partial differential equations with random parameters. In this work, we present and examine the multi-element probabilistic collocation method (ME-PCM), which is a generalized form of the probabilistic collocation method. In the ME-PCM, the parametric space is discretized and a collocation/cubature grid is prescribed on each element. Both full and sparse tensor product grids based on Gauss and Clenshaw-Curtis quadrature rules are considered. We prove analytically and observe in numerical tests that as the parameter space mesh is refined, the convergence rate of the solution depends on the quadrature rule of each element only through its degree of exactness. In addition, the L 2 error of the tensor product interpolant is examined and an adaptivity algorithm is provided. Numerical examples demonstrating adaptive ME-PCM are shown, including low-regularity problems and long-time integration. We test the ME-PCM on two-dimensional Navier-Stokes examples and a stochastic diffusion problem with various random input distributions and up to 50 dimensions. While the convergence rate of ME-PCM deteriorates in 50 dimensions, the error in the mean and variance is two orders of magnitude lower than the error obtained with the Monte Carlo method using only a small number of samples (e.g., 100). The computational cost of ME-PCM is found to be favorable when compared to the cost of other methods including stochastic Galerkin, Monte Carlo and quasi-random sequence methods

Error analysis of isotope dilution mass spectrometry method with internal standard

International Nuclear Information System (INIS)

Rizhinskii, M.W.; Vitinskii, M.Y.

1989-02-01

The computation algorithms of the normalized isotopic ratios and element concentration by isotope dilution mass spectrometry with internal standard are presented. A procedure based on the Monte-Carlo calculation is proposed for predicting the magnitude of the errors to be expected. The estimation of systematic and random errors is carried out in the case of the certification of uranium and plutonium reference materials as well as for the use of those reference materials in the analysis of irradiated nuclear fuels. 4 refs, 11 figs, 2 tabs

Multi-elemental imaging of paraffin-embedded human samples by laser-induced breakdown spectroscopy

Science.gov (United States)

Moncayo, S.; Trichard, F.; Busser, B.; Sabatier-Vincent, M.; Pelascini, F.; Pinel, N.; Templier, I.; Charles, J.; Sancey, L.; Motto-Ros, V.

2017-07-01

Chemical elements play central roles for physiological homeostasis in human cells, and their dysregulation might lead to a certain number of pathologies. Novel imaging techniques that improve the work of pathologists for tissue analysis and diagnostics are continuously sought. We report the use of Laser-Induced Breakdown Spectroscopy (LIBS) to perform multi-elemental images of human paraffin-embedded skin samples on the entire biopsy scale in a complementary and compatible way with microscope histopathological examination. A specific instrumental configuration is proposed in order to detect most of the elements of medical interest (i.e. P, Al, Mg, Na, Zn, Si, Fe, and Cu). As an example of medical application, we selected and analysed skin biopsies, including healthy skin tissue, cutaneous metastasis of melanoma, Merkel-cell carcinoma and squamous cell carcinoma. Clear distinctions in the distribution of chemical elements are observed from the different samples investigated. This study demonstrates the high complementarity of LIBS elemental imaging with conventional histopathology, opening new opportunities for any medical application involving metals.

Quantitating subcellular metabolism with multi-isotope imaging mass spectrometry

Science.gov (United States)

Steinhauser, Matthew L.; Bailey, Andrew; Senyo, Samuel E.; Guillermier, Christelle; Perlstein, Todd S.; Gould, Alex P.; Lee, Richard T.; Lechene, Claude P.

2011-01-01

Mass spectrometry with stable isotope labels has been seminal in discovering the dynamic state of living matter1,2 but is limited to bulk tissues or cells. We developed multi-isotope imaging mass spectrometry (MIMS) that allowed us to view and measure stable isotope incorporation with sub-micron resolution3,4. Here we apply MIMS to diverse organisms, including Drosophila, mice, and humans. We test the “immortal strand hypothesis,” which predicts that during asymmetric stem cell division chromosomes containing older template DNA are segregated to the daughter destined to remain a stem cell, thus insuring lifetime genetic stability. After labeling mice with 15N-thymidine from gestation through post-natal week 8, we find no 15N label retention by dividing small intestinal crypt cells after 4wk chase. In adult mice administered 15N-thymidine pulse-chase, we find that proliferating crypt cells dilute label consistent with random strand segregation. We demonstrate the broad utility of MIMS with proof-of-principle studies of lipid turnover in Drosophila and translation to the human hematopoietic system. These studies show that MIMS provides high-resolution quantitation of stable isotope labels that cannot be obtained using other techniques and that is broadly applicable to biological and medical research. PMID:22246326

Use of alpha spectrometry for analysis of U-isotopes in some granite samples

International Nuclear Information System (INIS)

El-Galy, M.M.; Desouky, O.A.; Khattab, M.R.; Issa, F.A.

2011-01-01

The present study aims to use the α-spectrometry, at NMA. A radiochemical technique for analysis of U-isotopes was carried out for some granite samples from Gabal Gattar and El Missikat localities and also for some reference soil samples of IAEA. Several steps of sample preparation, radiochemical separation, and source preparation were performed before analysis. The concerned sample was leached by HNO 3 , HF and H 2 O 2 acids after ashing. The ashed sample was spiked with uranium tracer ( 232 U) for chemical yield and activity calculation. Then uranium was extracted from the matrix elements with trioctylphosphine oxide (TOPO) and stripped with 1 M NH 4 F/0.1 M HCl solution. The uranium fraction was purified by co-precipitation with LaF 3 to ensure complete removal of thorium and traces of resolution degrading elements. This was followed by a final clean-up step using an anion exchange. The pure uranium fraction was electrodeposited on a stainless steel disc from HCl/oxalate solution. The obtained results from the soil reference samples indicate general similarities between the techniques of α-spectrometers of NMA, EAEA and IAEA for analysis of U-isotopes. The U-isotopes in the granite samples of high radioactivity levels need more attempts after dilution process to be in the limit detection of α-spectrometry. (author)

Pump radiation distribution in multi-element first cladding laser fibres

International Nuclear Information System (INIS)

Mel'kumov, Mikhail A; Bufetov, Igor' A; Bubnov, M M; Shubin, Aleksei V; Semenov, S L; Dianov, Evgenii M

2005-01-01

Pump radiation transfer is studied experimentally in multi-element first cladding laser fibres. A model of this process is proposed, which is in good agreement with experimental results. An all-fibre single-mode cw ytterbium laser based on a three-element first cladding fibre with an output power of 100W is fabricated. (lasers)

Development of isotope dilution gamma-ray spectrometry for plutonium analysis

Energy Technology Data Exchange (ETDEWEB)

Li, T.K.; Parker, J.L. (Los Alamos National Lab., NM (United States)); Kuno, Y.; Sato, S.; Kurosawa, A.; Akiyama, T. (Power Reactor and Nuclear Fuel Development Corp., Tokai, Ibaraki (Japan))

1991-01-01

We are studying the feasibility of determining the plutonium concentration and isotopic distribution of highly radioactive, spent-fuel dissolver solutions by employing high-resolution gamma-ray spectrometry. The study involves gamma-ray plutonium isotopic analysis for both dissolver and spiked dissolver solution samples, after plutonium is eluted through an ion-exchange column and absorbed in a small resin bead bag. The spike is well characterized, dry plutonium containing {approximately}98% of {sup 239}Pu. By using measured isotopic information, the concentration of elemental plutonium in the dissolver solution can be determined. Both the plutonium concentration and the isotopic composition of the dissolver solution obtained from this study agree well with values obtained by traditional isotope dilution mass spectrometry (IDMS). Because it is rapid, easy to operate and maintain, and costs less, this new technique could be an alternative method to IDMS for input accountability and verification measurements in reprocessing plants. 7 refs., 4 figs., 4 tabs.

Hydrothermal analysis in engineering using control volume finite element method

CERN Document Server

Sheikholeslami, Mohsen

2015-01-01

Control volume finite element methods (CVFEM) bridge the gap between finite difference and finite element methods, using the advantages of both methods for simulation of multi-physics problems in complex geometries. In Hydrothermal Analysis in Engineering Using Control Volume Finite Element Method, CVFEM is covered in detail and applied to key areas of thermal engineering. Examples, exercises, and extensive references are used to show the use of the technique to model key engineering problems such as heat transfer in nanofluids (to enhance performance and compactness of energy systems),

Multi-class, multi-residue analysis of pesticides, polychlorinated biphenyls, polycyclic aromatic hydrocarbons, polybrominated diphenyl ethers and novel flame retardants in fish using fast, low-pressure gas chromatography–tandem mass spectrometry

International Nuclear Information System (INIS)

Sapozhnikova, Yelena; Lehotay, Steven J.

2013-01-01

Highlights: ► A method for analysis of POPs and novel flame retardants in catfish was developed. ► The method is based on a QuEChERS extraction, d-SPE clean-up and low pressure GC/MS–MS. ► The method validation demonstrated good recoveries and low detection limits. ► The method was successfully applied for analysis of catfish samples from the market. - Abstract: A multi-class, multi-residue method for the analysis of 13 novel flame retardants, 18 representative pesticides, 14 polychlorinated biphenyl (PCB) congeners, 16 polycyclic aromatic hydrocarbons (PAHs), and 7 polybrominated diphenyl ether (PBDE) congeners in catfish muscle was developed and evaluated using fast low pressure gas chromatography triple quadrupole tandem mass spectrometry (LP-GC/MS–MS). The method was based on a QuEChERS (quick, easy, cheap, effective, rugged, safe) extraction with acetonitrile and dispersive solid-phase extraction (d-SPE) clean-up with zirconium-based sorbent prior to LP-GC/MS–MS analysis. The developed method was evaluated at 4 spiking levels and further validated by analysis of NIST Standard Reference Materials (SRMs) 1974B and 1947. Sample preparation for a batch of 10 homogenized samples took about 1 h/analyst, and LP-GC/MS–MS analysis provided fast separation of multiple analytes within 9 min achieving high throughput. With the use of isotopically labeled internal standards, recoveries of all but one analyte were between 70 and 120% with relative standard deviations less than 20% (n = 5). The measured values for both SRMs agreed with certified/reference values (72–119% accuracy) for the majority of analytes. The detection limits were 0.1–0.5 ng g −1 for PCBs, 0.5–10 ng g −1 for PBDEs, 0.5–5 ng g −1 for select pesticides and PAHs and 1–10 ng g −1 for flame retardants. The developed method was successfully applied for analysis of catfish samples from the market.

The use of synchrotron radiation for trace element analysis and element mapping by scanning X-ray fluorescence

International Nuclear Information System (INIS)

Davies, S.T.

1983-01-01

Synchrotron Radiation excited X-Ray Fluorescence is a potentially powerful tool for the routine quantitative chemical analysis of materials, with minimum detection limits typically of the order of a tenth of a ppm, and with the added advantages of simultaneous multi-element detection capability, spatial resolution on a micron scale, large signal to noise ratios and short analysis times. This paper presents a brief review of the use of Synchrotron Radiation in Trace Element Analysis and discusses the requirements for a microprobe for chemical analysis utilising SR. Data obtained at the Synchrotron Radiation Source, Daresbury Laboratory include XRF spectra of standard reference materials and an application of the technique to the study of ion implanted layers in semiconductors is outlined. (author)

Principle of neutron activation analysis and its use for determination of trace elements in sediment

International Nuclear Information System (INIS)

Verma, Rakesh

2012-01-01

Neutron Activation analysis (NAA) is a multi element analysis technique, often non-destructive in nature where approximately 75 elements can be measured with the detection limits ranging from 10 -6 to 10 -12 g of element in a sample. Typical sample sizes range from 1 mg to 1 g, however in principle much larger samples can be activated and the size is only limited by the capacity of the neutron irradiation facility. In NAA, a sample (solid or liquid or gas) is exposed to neutrons and radiations emitted by the radioactive products, formed during the nuclear reaction, are measured using a suitable detector. The energy of the emitted radiation is a characteristic of a radioisotope whereas the intensity of the emitted radiation is proportional to the mass of the analyte. NAA can be carried out by measurement of (i) prompt gamma rays emitted by compound nucleus, called prompt gamma ray NAA (PGNAA) and (ii) β rays emitted from radioactive product or delayed gamma rays emitted subsequent to β decay, called conventional NAA or simply NAA. PGNAA is an online measurement method. PGNAA is complementary to conventional NAA in terms of analyzing low Z elements. Conventional NAA is an offline method and is easy to perform. Depending upon the nature of matrix and analyte to be determined, three approaches are possible in NAA namely, (i) instrumental neutron activation analysis (INAA), (ii) radiochemical neutron activation analysis (RNAA), and (iii) chemical neutron activation analysis (CNAA). Quantification is accomplished by any of the three standardisation methodologies namely (i) absolute method (ii) relative method and (iii) single comparator method. The relative method is most precise and simple to perform. Natural processes responsible for the formation of bottom sediments can be altered by anthropogenic activities. Bottom sediments are a sink as well as a source of contaminants in the aquatic environment. Analysis of-sediments provides environmentally significant

Evaluasi Ketidakpastian Pengukuran Multi-Unsur Dalam Mineral Zirkon Dengan Metode Analisis Aktivasi Neutron

Directory of Open Access Journals (Sweden)

Sukirno

2015-05-01

Full Text Available The evaluation of multi-elements analysis has been carried out with calculation of element uncertainy in the zircon mineral from Sampit (Central Kalimantan dan Bangka has been evaluated by the Neutron Activation Analysis (NAA method. The purpose of this research is determination of composition and value of multi-elements uncertainty in the mineral of zircon to fulfil the requirements of ISO/IEC guide 17025-2008 that applied at NAA laboratory. The result of analysis using gamma spectrometry with a HPGe detector showed of 21 detected elements, divided into three groups (major, minor, and trace. Evaluation of uncertainty estimation should be done to increase quality and confidence rate of analysis results. The result of testing are not mean without calculation of uncertainty. Therefore, it was assessed the uncertainty measurement of all elements analysis in zircon mineral. The results of quantitative analysis is Zr with the highest concentration value of 38.986% and value of uncertainty is 0.331% so that value of real concentration is 38.986 ± 0.331%. In the form of oxide (ZrO2 has concentration of 52.661±0.45%. Sb element is the lowest element detected with value of concentration and uncertainty is 7±0,3 µg/g. In the form of oxide (Sb2O3 has concentration is 17±0.9 µg/g. The oxide composition and the must important of chemicals in the zircon sand mineral more significant from Sampit which quantitative composition areZrO2+HfO2 (53-55%, F2O3 (5-6%, TiO2 (13-14%, Al2O3 (1.5-2% and SiO2. Elements ofSi(SiO2 can not be determined by NAA method because Si cross-sections is verysmall.

Beyond the ridge pattern: multi-informative analysis of latent fingermarks by MALDI mass spectrometry.

Science.gov (United States)

Francese, S; Bradshaw, R; Ferguson, L S; Wolstenholme, R; Clench, M R; Bleay, S

2013-08-07

After over a century, fingerprints are still one of the most powerful means of biometric identification. The conventional forensic workflow for suspect identification consists of (i) recovering latent marks from crime scenes using the appropriate enhancement technique and (ii) obtaining an image of the mark to compare either against known suspect prints and/or to search in a Fingerprint Database. The suspect is identified through matching the ridge pattern and local characteristics of the ridge pattern (minutiae). However successful, there are a number of scenarios in which this process may fail; they include the recovery of partial, distorted or smudged marks, poor quality of the image resulting from inadequacy of the enhancement technique applied, extensive scarring/abrasion of the fingertips or absence of suspect's fingerprint records in the database. In all of these instances it would be very desirable to have a technology able to provide additional information from a fingermark exploiting its endogenous and exogenous chemical content. This opportunity could potentially provide new investigative leads, especially when the fingermark comparison and match process fails. We have demonstrated that Matrix Assisted Laser Desorption Ionisation Mass Spectrometry and Mass Spectrometry Imaging (MALDI MSI) can provide multiple images of the same fingermark in one analysis simultaneous with additional intelligence. Here, a review on the pioneering use and development of MALDI MSI for the analysis of latent fingermarks is presented along with the latest achievements on the forensic intelligence retrievable.

Quantitative determination of minor and trace elements in rocks and soils by spark source mass spectrometry

International Nuclear Information System (INIS)

Ure, A.M.; Bacon, J.R.

1978-01-01

Experimental details are given of the quantitative determination of minor and trace elements in rocks and soils by spark source mass spectrometry. The effects of interfering species, and corrections that can be applied, are discussed. (U.K.)

Neutron activation analysis of rare earths and some other elements in material of geochemical interest

International Nuclear Information System (INIS)

Brunfelt, A.O.

1975-01-01

ngle-element methods for the determination by neutron activation analysis of antimony, chromium, phosphorus, selenium and silver in international geochemical standard rocks, and the determination of rare earth elements i in standard rocks and apatites are described and discussed in twelve previously published papers, and in an eighteen page summary. Chemical separationtechniques are also discussed and the results are compared with previously obtained results with the same standard rocks. The accuracy of neutron activation analysis is discussed in comparison with isotope dilution mass spectroscopy, atomic absorption, gas chromatography and spark source mass spectrometry. (JIW)

Chemical elements in the environment: multi-element geochemical datasets from continental to national scale surveys on four continents

Science.gov (United States)

Caritat, Patrice de; Reimann, Clemens; Smith, David; Wang, Xueqiu

2017-01-01

During the last 10-20 years, Geological Surveys around the world have undertaken a major effort towards delivering fully harmonized and tightly quality-controlled low-density multi-element soil geochemical maps and datasets of vast regions including up to whole continents. Concentrations of between 45 and 60 elements commonly have been determined in a variety of different regolith types (e.g., sediment, soil). The multi-element datasets are published as complete geochemical atlases and made available to the general public. Several other geochemical datasets covering smaller areas but generally at a higher spatial density are also available. These datasets may, however, not be found by superficial internet-based searches because the elements are not mentioned individually either in the title or in the keyword lists of the original references. This publication attempts to increase the visibility and discoverability of these fundamental background datasets covering large areas up to whole continents.

Spectrometer system using a modular echelle spectrograph and a laser-driven continuum source for simultaneous multi-element determination by graphite furnace absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Geisler, Sebastian; Okruss, Michael; Becker-Ross, Helmut; Huang, Mao Dong, E-mail: huang@isas.de; Esser, Norbert; Florek, Stefan

2015-05-01

A multi-element absorption spectrometer system has been developed based on a laser-driven xenon continuum source and a modular simultaneous echelle spectrograph (MOSES), which is characterized by a minimized number of optical components resulting in high optical throughput, high transmittance and high image quality. The main feature of the new optical design is the multifunction usage of a Littrow prism, which is attached on a rotation stage. It operates as an order-sorter for the echelle grating in a double-pass mode, as a fine positioning device moving the echelle spectrum on the detector, and as a forwarder to address different optical components, e.g., echelle gratings, in the setup. Using different prisms, which are mounted back to back on the rotation stage, a multitude of different spectroscopic modes like broad-range panorama observations, specific UV–VIS and NIR studies or high resolution zoom investigations of variable spectral channels can be realized. In the UV panorama mode applied in this work, MOSES has simultaneously detectable wavelength coverage from 193 nm to 390 nm with a spectral resolution λ/Δλ of 55,000 (3-pixel criterion). In the zoom mode the latter can be further increased by a factor of about two for a selectable section of the full wavelength range. The applicability and the analytical performance of the system were tested by simultaneous element determination in a graphite furnace, using eight different elements. Compared to an instrument operating in the optimized single line mode, the achieved analytical sensitivity using the panorama mode was typically a factor of two lower. Using the zoom mode for selected elements, comparable sensitivities were obtained. The results confirm the influence of the different spectral resolutions. - Highlights: • Echelle spectrometer with a full frame CCD array detector • High and variable spectral resolution from λ/Δλ of 55,000 to 95,000 • Laser-driven continuum light source �

Compton suppression spectrometry for analysis of short-lived neutron activation products in foods

International Nuclear Information System (INIS)

Anderson, D.L.; Cunningham, W.C.

2008-01-01

Compton suppression spectrometry was used to analyze foods for elements with short-lived neutron activation products (half-lives of about 2 minutes to 1.5 days). Analysis conditions were optimized to provide quality assurance analyses for iodine in FDA's Total Diet Study. Iodine mass fractions (0.075 to 2.03 mg/kg) were measured in 19 of 42 foods analyzed, with limits of detection (LODs) ranging from 0.03 to 1.4 mg/kg, mostly depending on NaCl content. LODs were lowered by up to a factor of 2 for 16 elements. Suppression factors ranged from about 2 to 8 over the energy range 400 to 3200 keV. (author)

Principal component analysis of normalized full spectrum mass spectrometry data in multiMS-toolbox: An effective tool to identify important factors for classification of different metabolic patterns and bacterial strains.

Science.gov (United States)

Cejnar, Pavel; Kuckova, Stepanka; Prochazka, Ales; Karamonova, Ludmila; Svobodova, Barbora

2018-06-15

Explorative statistical analysis of mass spectrometry data is still a time-consuming step. We analyzed critical factors for application of principal component analysis (PCA) in mass spectrometry and focused on two whole spectrum based normalization techniques and their application in the analysis of registered peak data and, in comparison, in full spectrum data analysis. We used this technique to identify different metabolic patterns in the bacterial culture of Cronobacter sakazakii, an important foodborne pathogen. Two software utilities, the ms-alone, a python-based utility for mass spectrometry data preprocessing and peak extraction, and the multiMS-toolbox, an R software tool for advanced peak registration and detailed explorative statistical analysis, were implemented. The bacterial culture of Cronobacter sakazakii was cultivated on Enterobacter sakazakii Isolation Agar, Blood Agar Base and Tryptone Soya Agar for 24 h and 48 h and applied by the smear method on an Autoflex speed MALDI-TOF mass spectrometer. For three tested cultivation media only two different metabolic patterns of Cronobacter sakazakii were identified using PCA applied on data normalized by two different normalization techniques. Results from matched peak data and subsequent detailed full spectrum analysis identified only two different metabolic patterns - a cultivation on Enterobacter sakazakii Isolation Agar showed significant differences to the cultivation on the other two tested media. The metabolic patterns for all tested cultivation media also proved the dependence on cultivation time. Both whole spectrum based normalization techniques together with the full spectrum PCA allow identification of important discriminative factors in experiments with several variable condition factors avoiding any problems with improper identification of peaks or emphasis on bellow threshold peak data. The amounts of processed data remain still manageable. Both implemented software utilities are available

Determination of trace and ultra-trace elements in Dergaon meteorite by inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Balaram, V.; Gnaneswara Rao, T.; Anjaiah, K.V.; Phukon, N.; Majumdar, A.C.

2003-01-01

In this paper, a detailed methodology for high precision measurement of several trace and ultra-trace elements including REE and PGE have been presented using effective sample preparation techniques and inductively coupled plasma mass spectrometry. Discussion is focussed on aspects, such as total dissolution and recovery of all elements, minimization of oxide and doubly-charged and other polyatomic ion interferences, calibration by matrix matching standards, accuracy and precision

Investigation of Elemental Mass Spectrometry in Pharmacology for Peptide Quantitation at Femtomolar Levels.

Directory of Open Access Journals (Sweden)

Emmanuelle Cordeau

Full Text Available In the search of new robust and environmental-friendly analytical methods able to answer quantitative issues in pharmacology, we explore liquid chromatography (LC associated with elemental mass spectrometry (ICP-MS to monitor peptides in such complex biological matrices. The novelty is to use mass spectrometry to replace radiolabelling and radioactivity measurements, which represent up-to now the gold standard to measure organic compound concentrations in life science. As a proof of concept, we choose the vasopressin (AVP/V1A receptor system for model pharmacological assays. The capacity of ICP-MS to provide highly sensitive quantitation of metallic and hetero elements, whatever the sample medium, prompted us to investigate this technique in combination with appropriate labelling of the peptide of interest. Selenium, that is scarcely present in biological media, was selected as a good compromise between ICP-MS response, covalent tagging ability using conventional sulfur chemistry and peptide detection specificity. Applying selenium monitoring by elemental mass spectrometry in pharmacology is challenging due to the very high salt content and organic material complexity of the samples that produces polyatomic aggregates and thus potentially mass interferences with selenium detection. Hyphenation with a chromatographic separation was found compulsory. Noteworthy, we aimed to develop a straightforward quantitative protocol that can be performed in any laboratory equipped with a standard macrobore LC-ICP-MS system, in order to avoid time-consuming sample treatment or special implementation of instrumental set-up, while allowing efficient suppression of all mass interferences to reach the targeted sensitivity. Significantly, a quantification limit of 57 ng Se L-1 (72 femtomoles of injected Se was achieved, the samples issued from the pharmacological assays being directly introduced into the LC-ICP-MS system. The established method was successfully

Simple procedure for nutrient analysis of coffee plant with energy dispersive X-ray fluorescence spectrometry (EDXRF)

Energy Technology Data Exchange (ETDEWEB)

Tezotto, Tiago; Favarin, Jose Laercio; Neto, Ana Paula; Azevedo, Ricardo Antunes, E-mail: tiago.tezotto@usp.br [Escola Superior de Agricultura Luiz de Queiroz (ESALQ/USP), Piracicaba, SP (Brazil); Gratao, Priscila Lupino [Universidade Estadual Paulista Julio de Mesquita Filho (UNESP/ FCAV), Jaboticabal, SP (Brazil). Dept. de Biologia Aplicada a Agropecuaria; Mazzafera, Paulo [Universidade Estadual de Campinas (UNICAMP/IB), SP (Brazil). Dept. Biologia Vegetal

2013-07-15

Nutrient analysis is used to estimate nutrient content of crop plants to manage fertilizer application for sustained crop production. Direct solid analysis of agricultural and environmental samples by energy dispersive X-ray fluorescence spectrometry (EDXRF) was chosen as alternative technique to evaluate the simultaneous multielemental quantification of the most important essential elements in coffee (Coffea arabica L.) plants. Inductively coupled plasma atomic emission spectrometry and certified reference materials made from leaves were used to calibrate and check the trueness of EDXRF method for the determination of the concentration of several nutrients in coffee leaves and branches. Fluorescence spectrometry proved to be advantageous and presented low cost as loose powder samples could be used. Samples collected from a field experiment where coffee plants were treated with excess of Ni and Zn were used to verify the practical application of the method. Good relationships were achieved between certified values and data obtained by EDXRF, with recoveries ranging from 82 to 117 %.(author)

Mass spectrographic analysis of selected chemical elements by microbial leaching of zircon

International Nuclear Information System (INIS)

Becker, S.; Dietze, H.J.; Bullmann, M.; Iske, U.

1986-01-01

Spark source mass spectrometry is a useful method for chemical element analysis of geological and biological samples. This sensitive technique (detection limit down to the ppb-range) is used to analyze leaching processes by means of several microorganisms. The problem of microbial leaching of chemical resistent materials was tested under laboratory conditions with regard to possible analytical and technical applications. Leaching of metals with chemolithotrophic and heterotrophic, organic acids producing microorganisms has been investigated with zircon from the Baltic Shield containing 0.7% rare earth elements and 1.67% hafnium. When zircon is leached with strains of thiobacillus ferrooxidans about 80% of the rare earth elements, Hf, Th and U can be recovered. (orig.) [de

Quantification of trace amounts of rare earth elements in high purity gadolinium oxide by sector field inductively coupled plasma mass spectrometry (ICP-MS)

International Nuclear Information System (INIS)

Pedreira, W.R.; Silva Queiroz, C.A. da; Abrao, A.; Pimentel, M.M.

2004-01-01

In recent years, rare earth elements (REEs) have received much attention in the fields of geochemistry and industry. Gadolinium oxide is used for many different high technology applications such as infrared absorbing automotive glass, petroleum cracking catalyst, gadolinium-yttrium garnets, microwave applications, and color TV tube phosphors. It can also be used in optical glass manufacturing and in the electronic industry. Rapid and accurate determinations of the rare earth elements are increasingly required as industrial demands expand. In general, the inductively coupled plasma mass spectrometry (ICP-MS) presents some advantages for trace element analysis, due to high sensitivity and resolution, when compared with other analytical techniques. In this work, sector field inductively coupled plasma mass spectrometry was used. Sixteen elements (Sc, Y, and 14 lanthanides) were determined selectively with the ICP-MS system using a concentration gradient method. The detection limits with the ICP-MS system were about 0.2-8 pg ml -1 . The recovery percentage ranged from 95 to 100% for different rare earth elements. The %R.S.D. of the methods varying between 1.5 and 2.5% for a set of five (n=5) replicates was found for the IPEN's material and for the certificate reference sample. Determination of trace REEs in two high pure gadolinium oxides samples (IPEN and JMC) was performed. IPEN's material is highly pure (>99.99%) and was successfully analyzed without spectral interference

Particle induced X-ray emission for quantitative trace-element analysis using the Eindhoven cyclotron

International Nuclear Information System (INIS)

Kivits, H.

1980-01-01

Development of a multi-elemental trace analysis technique using PIXE (Particle Induced X-ray Emission), was started almost five years ago at the Eindhoven University of Technology, in the Cyclotron Applications Group of the Physics Department. The aim of the work presented is to improve the quantitative aspects of trace-element analysis with PIXE, as well as versatility, speed and simplicity. (Auth.)

Determination of rare earth elements by liquid chromatography/inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

Yoshida, K.; Haraguchi, H.

1984-01-01

Inductively coupled plasma atomic emission spectrometry (ICP-AES) interfaced with high-performance liquid chromatography (HPLC) has been applied to the determination of rare earth elements. ICP-AES was used as an element-selective detector for HPLC. The separation of rare earth elements with HPLC helped to avoid erroneous analytical results due to spectral interferences. Fifteen rare earth elements (Y and 14 lanthanides) were determined selectively with the HPLC/ICP-AES system using a concentration gradient method. The detection limits with the present HPLC/ICP-AES system were about 0.001-0.3 μg/mL with a 100-μL sample injection. The calibration curves obtained by the peak height measurements showed linear relationships in the concentration range below 500 μg/mL for all rare earth elements. A USGS rock standard sample, rare earth ores, and high-purity lanthanide reagents (>99.9%) were successfully analyzed without spectral interferences

Total and species-specific quantitative analyses of trace elements in sediment by isotope dilution inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Inagaki, Kazumi; Takatsu, Akiko; Yarita, Takashi; Okamoto, Kensaku; Chiba, Koichi

2009-01-01

Isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS) is one of the reliable methods for total and species-specific quantitative analysis of trace elements. However, several technical problems (e.g. spectral interference caused from sample constituents) should be overcome to obtain reliable analytical results when environmental samples are analyzed by ID-ICP-MS. In our laboratory, various methods based on ID-ICP-MS have been investigated for reliable quantitative analyses of trace elements in environmental samples. In this paper, coprecipitate separation/ID-ICP-MS for the determination of trace elements in sediment, cation exchange disk filtration/ID-ICP-MS for the determination of selenium in sediment, species-specific ID-ICP-MS using 118 Sn/labeled organotin compounds for the determination of butyltins and phenyltins, and the application of the ID-ICP-MS methods to the certification of sediment reference materials are described. (author)

Hybrid quadrupole-orbitrap mass spectrometry analysis with accurate-mass database and parallel reaction monitoring for high-throughput screening and quantification of multi-xenobiotics in honey.

Science.gov (United States)

Li, Yi; Zhang, Jinzhen; Jin, Yue; Wang, Lin; Zhao, Wen; Zhang, Wenwen; Zhai, Lifei; Zhang, Yaping; Zhang, Yongxin; Zhou, Jinhui

2016-01-15

This study reports a rapid, automated screening and quantification method for the determination of multi-xenobiotic residues in honey using ultra-high performance liquid chromatography-hybrid quadrupole-Orbitrap mass spectrometry (UHPLC-Q-Orbitrap) with a user-built accurate-mass database plus parallel reaction monitoring (PRM). The database contains multi-xenobiotic information including formulas, adduct types, theoretical exact mass and retention time, characteristic fragment ions, ion ratios, and mass accuracies. A simple sample preparation method was developed to reduce xenobiotic loss in the honey samples. The screening method was validated based on retention time deviation, mass accuracy via full scan-data-dependent MS/MS (full scan-ddMS2), multi-isotope ratio, characteristic ion ratio, sensitivity, and positive/negative switching performance between the spiked sample and corresponding standard solution. The quantification method based on the PRM mode is a promising new quantitative tool which we validated in terms of selectivity, linearity, recovery (accuracy), repeatability (precision), decision limit (CCα), detection capability (CCβ), matrix effects, and carry-over. The optimized methods proposed in this study enable the automated screening and quantification of 157 compounds in less than 15 min in honey. The results of this study, as they represent a convenient protocol for large-scale screening and quantification, also provide a research approach for analysis of various contaminants in other matrices. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of isotope ratios of metals (and metalloids) by means of inductively coupled plasma-mass spectrometry for provenancing purposes - A review

International Nuclear Information System (INIS)

Balcaen, L.; Moens, L.; Vanhaecke, F.

2010-01-01

Since considerable time, isotopic analysis of different elements present in a sample, material or object (such as the 'light' elements H, C, N, O and S and 'heavy' elements, such as Sr and Pb), has been used in provenancing studies, as several factors - defined by 'the environment' or origin of the sample - can lead to measurable differences in their isotopic composition. For the light elements, traditionally, (gas source) isotope ratio mass spectrometry (IR-MS) is used, while for a long period of time, thermal ionization mass spectrometry (TIMS) was considered as the only technique capable of detecting subtle variations in the isotopic composition of the 'heavier' elements. However, since the introduction of the first inductively coupled plasma mass spectrometers (ICP-MS), considerable attention has been devoted to the development of methodologies and strategies to perform isotopic analysis by means of ICP-MS. While the relatively modest isotope ratio precision offered by single-collector ICP-MS may already be fit-for-purpose under some circumstances, especially the introduction of multi-collector ICP-MS instruments, equipped with an array of Faraday detectors instead of a single electron multiplier, has lead to tremendous improvements in the field of isotopic analysis. As a result, MC-ICP-MS can be seen as a very strong competitor of TIMS nowadays, while it even provides information on the small isotopic variations shown by some elements, that are not or hardly accessible by means of TIMS (e.g., elements with a high ionization energy). Owing to these new instrumental developments, the application field of isotopic analysis by means of ICP-MS is continuously growing, also in the field of provenance determination. This paper is intended as a review of the developments in and the recent applications of isotopic analysis by means of ICP-MS in this specific research field.

Analysis of Hair Trace Elements in Children with Autism Spectrum Disorders and Communication Disorders.

Science.gov (United States)

Skalny, Anatoly V; Simashkova, Natalia V; Klyushnik, Tatiana P; Grabeklis, Andrei R; Radysh, Ivan V; Skalnaya, Margarita G; Tinkov, Alexey A

2017-06-01

The primary objective of the present study is analysis of hair trace elements content in children with communication disorder (CD) and autism spectrum disorder (ASD). A total of 99 children from control, CD, and ASD groups (n = 33) were examined. All children were additionally divided into two subgroups according to age. Hair levels of trace elements were assessed using inductively coupled plasma mass spectrometry. The difference was considered significant at p elements including the toxic ones, it can be proposed that children suffering from ASD are characterized by more profound alteration of metal handling and excretion in comparison to CD.

Numerical solution of multi group-Two dimensional- Adjoint equation with finite element method

International Nuclear Information System (INIS)

Poursalehi, N.; Khalafi, H.; Shahriari, M.; Minoochehr

2008-01-01

Adjoint equation is used for perturbation theory in nuclear reactor design. For numerical solution of adjoint equation, usually two methods are applied. These are Finite Element and Finite Difference procedures. Usually Finite Element Procedure is chosen for solving of adjoint equation, because it is more use able in variety of geometries. In this article, Galerkin Finite Element method is discussed. This method is applied for numerical solving multi group, multi region and two dimensional (X, Y) adjoint equation. Typical reactor geometry is partitioned with triangular meshes and boundary condition for adjoint flux is considered zero. Finally, for a case of defined parameters, Finite Element Code was applied and results were compared with Citation Code

Coupling between chip based isotachophoresis and multi-collector inductively coupled plasma mass spectrometry for separation and measurement of lanthanides

International Nuclear Information System (INIS)

Vio, Laurent; Cretier, Gerard; Rocca, Jean-Louis; Chartier, Frederic; Geertsen, Valerie; Gourgiotis, Alkiviadis; Isnard, Helene; Morin, Pierre

2012-01-01

This paper presents the conception and fabrication of a micro-system for lanthanides separation and its coupling with a multi-collector inductively coupled plasma mass spectrometer for isotope ratio measurements. The lanthanides separation is based on the isotachophoresis technique and the micro-system conception has been adapted in order to fit with glove box limitations in view of future spent nuclear fuels analysis. The micro-device was tested by using a mixture of standard solutions of natural elements and the separation of 13 lanthanides was successfully performed. The micro-device was then coupled to a multi-collector inductively coupled plasma mass spectrometer for the on-line measurements of Nd and Sm isotope ratios. The isotopes of Nd and Sm were acquired online in multi-collection mode after separation of the two elements with an injection amount of 5 ng. Results obtained on the Nd and Sm isotope ratio measurements on transient signals are presented and discussed. (authors)

[Inductively coupled plasma mass spectrometry for the simultaneous determination of thirty metals and metalloids elements in blood samples].

Science.gov (United States)

Ding, Chun-guang; Zhu, Chun; Liu, De-ye; Dong, Ming; Zhang, Ai-hua; Pan, Ya-juan; Yan, Hui-fang

2012-08-01

To establish an inductively coupled plasma mass spectrometry(ICP-MS) method for determination of 30 trace elements including As, Ba, Be, Bi, Ni, Cd, Co, Cr, Cs, Cu, Ga, Mn, Pb, Sr, Tl, V, Ge, Mo, Nb, Ti, W, Te, Se, Zr, In, Sb, Hg, Ce, La, and Sm in human blood. The blood samples were analyzed by ICP-MS after diluted 1/10 with 0.01% Triton-X-100 and 0.5% nitric acid solution. Y, Rh and Lu were selected as internal standard in order to correct the matrix interference of Cr, As, Se, and Hg by a hex pole-based collision-reaction cell. Other elements were determined with standard method. The limits of detection, precision and accuracy of the method were evaluated. The accuracy was validated by the determination of the whole blood reference material. All the 30 trace elements have good linearity in their determination range, with the correlation coefficient > 0.9999. The limits of detection of the 30 trace elements were in the range of 1.19 - 2.15 µg/L and the intra-precision and inter-precision (relative standard deviation, RSD) were less than 14.3% (except Hg RSD < 21.2%, and Ni RSD < 15.4%). The spiked recovery for all elements fell within 59.3% - 119.2%. Among the 13 whole blood reference materials, V, Cr, Mn, Co, Ni, Cu, As, Se, Cd, Te, and Pb (1.45, 1.19, 18.40, 0.18, 1.57, 591.00, 2.97, 61.00, 0.35, 1.86, and 9.70 µg/L respectively) fell within the acceptable range and the detection results of Hg (0.59 µg/L) and Mo (1.59 µg/L) were slightly beyond the range. This method was simple, fast and effective. It can be used to monitor the multi-elementary concentration in human blood.

Analysis of antibiotics from liquid sample using electrospray ionization-ion mobility spectrometry

International Nuclear Information System (INIS)

Li Shu; Jia Jian; Gao Xiaoguang; He Xiuli; Li Jianping

2012-01-01

Highlights: ► The reduced mobilities of 18 antibiotics are determined. ► Establishing antibiotic mass-mobility correlation using (12,4) potential model. ► Multi-component characteristics of antibiotics can be revealed using ESI-IMS. ► Most mixtures of antibiotics can be analyzed using ESI-IMS. ► The detection limit of amoxicillin is 70 pg. - Abstract: The recent findings of antibiotic residues in aquatic environment at trace level have gained much concern for the detrimental effect on ecological and human health due to bacterial resistance. Here, the feasibility of using electrospray ionization ion mobility spectrometry (ESI-IMS) for analysis antibiotics in liquid sample is demonstrated. Reduced mobilities and collision cross sections of 18 antibiotics are experimentally measured and compared with theoretical values according to mass-mobility correlation. Gentamicin is used as an example to investigate the capability of ESI-IMS for multi-component analysis of antibiotics. Mixtures of antibiotics at different concentrations are analyzed. The estimated detection limit for amoxicillin is 0.7 mg L −1 (70 pg) and the linear range of response maintains over two orders. This method will be a potential technique for the analysis of antibiotics in aquatic environment.

Neutron Activation Analysis with k0 standardisation

International Nuclear Information System (INIS)

Pomme, S.

1998-01-01

The objectives of the research are: (1) to develop and implement the k0 standardisation method for neutron activation analysis in close collaboration with scientific partners; (2) to exploit fully the inherent qualities of NAA such as accuracy, traceability, and multi-element offer complete services in health-physics measurements according to international quality standards, (2) to improve continuously these measurement techniques and to follow up international recommendations and legislation concerning the surveillance of workers; (3) to support and advise nuclear and non-nuclear industry on problems of radioactive contamination. Achievements in 1997 related to gamma spectrometry, whole-body counting, beta and alpha spectrometry, dosimetry, radon measurements, calibration, instrumentation, and neutron activation analysis are described

[Principal component analysis and cluster analysis of inorganic elements in sea cucumber Apostichopus japonicus].

Science.gov (United States)

Liu, Xiao-Fang; Xue, Chang-Hu; Wang, Yu-Ming; Li, Zhao-Jie; Xue, Yong; Xu, Jie

2011-11-01

The present study is to investigate the feasibility of multi-elements analysis in determination of the geographical origin of sea cucumber Apostichopus japonicus, and to make choice of the effective tracers in sea cucumber Apostichopus japonicus geographical origin assessment. The content of the elements such as Al, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Mo, Cd, Hg and Pb in sea cucumber Apostichopus japonicus samples from seven places of geographical origin were determined by means of ICP-MS. The results were used for the development of elements database. Cluster analysis(CA) and principal component analysis (PCA) were applied to differentiate the sea cucumber Apostichopus japonicus geographical origin. Three principal components which accounted for over 89% of the total variance were extracted from the standardized data. The results of Q-type cluster analysis showed that the 26 samples could be clustered reasonably into five groups, the classification results were significantly associated with the marine distribution of the sea cucumber Apostichopus japonicus samples. The CA and PCA were the effective methods for elements analysis of sea cucumber Apostichopus japonicus samples. The content of the mineral elements in sea cucumber Apostichopus japonicus samples was good chemical descriptors for differentiating their geographical origins.

The Study of Titanium and Zirconium Ions in Water by MPT-LTQ Mass Spectrometry in Negative Mode.

Science.gov (United States)

Yang, Junqing; Zheng, Mei; Liu, Qiuju; Yang, Meiling Zhu Chushan; Zhang, Yan; Zhu, Zhiqiang

2017-09-26

Microwave plasma torches (MPTs) can be used as simple and low power-consumption ambient ion sources. When MPT-mass spectrometry (MPT-MS) is applied in the detection of some metal elements, the metallic ions exhibit some novel features which are significantly different with those obtained by the traditional inductively coupled plasma (ICP)-mass spectrometry (ICP-MS) and may be helpful for metal element analysis. As the representative elements of group IVA, titanium and zirconium are both of importance and value in modern industry, and they have impacts on human health. Here, we first provide a study on the complex anions of titanium and zirconium in water by using the MPT as ion source and a linear ion trap mass spectrometer (LTQ-MS). These complex anions were produced in the plasma flame by an aqueous solution flowing through the central tube of the MPT, and were introduced into the inlet of the mass spectrometry working in negative ion mode to get the feature mass spectrometric signals. Moreover, the feature fragment patterns of these ions in multi-step collision- induced dissociation processes have been explained. Under the optimized conditions, the limit of detection (LOD) using the MS² (the second tandem mass spectrometry) procedure was estimated to be at the level of 10μg/L for titanium and 20 μg/L for zirconium with linear dynamics ranges that cover at least two orders of magnitude, i.e., between 0-500 μg/L and 20-200 μg/L, respectively. These experimental data demonstrated that the MPT-MS is a promising and useful tool in field analysis of titanium and zirconium ions in water, and can be applied in many fields, such as environmental control, hydrogeology, and water quality inspection. In addition, MPT-MS could also be used as a supplement of ICP-MS for the rapid and on-site analysis of metal ions.

Multielement determination of rare earth elements in rock sample by liquid chromatography / inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Hamanaka, Tadashi; Itoh, Akihide; Itoh, Shinya; Sawatari, Hideyuki; Haraguchi, Hiroki.

1995-01-01

Rare earth elements in geological standard rock sample JG-1 (granodiolite)issued from the Geological Survey of Japan have been determined by a combined system of liquid chromatography and inductively coupled plasma mass spectrometry. (author)

Food authenticity studies via multi-elemental and isotopic pattern using inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Katona, R.; Brunner, M.; Abranko, L.; Prohaska, T.; Stefanka, Z.

2009-01-01

Full text: The aim of our study has been the development of an analytical method based on Sr isotope and elemental fingerprint analysis for discriminating food samples from different geographical origin. Several types of foods were involved in the investigation representing different stages of food processing such as pulverized spicy paprika (sparsely processed food product) and wine samples (processed product). Independent inorganic mass spectrometric techniques like ICP-SFMS, ICP-CCMS, and MC-ICPMS were used for method validation and investigation of the geographical origin. The advantage and limitations of the developed methods are discussed critically. (author)

Microwave-assisted versus conventional decomposition procedures applied to a ceramic potsherd standard reference material by inductively coupled plasma atomic emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Papadopoulou, D.N.; Zachariadis, G.A.; Anthemidis, A.N.; Tsirliganis, N.C.; Stratis, J.A

2004-03-03

Inductively coupled plasma atomic emission spectrometry (ICP-AES) is a powerful, sensitive analytical technique with numerous applications in chemical characterization including that of ancient pottery, mainly due to its multi-element character, and the relatively short time required for the analysis. A critical step in characterization studies of ancient pottery is the selection of a suitable decomposition procedure for the ceramic matrix. The current work presents the results of a comparative study of six decomposition procedures applied on a standard ceramic potsherd reference material, SARM 69. The investigated decomposition procedures included three microwave-assisted decomposition procedures, one wet decomposition (WD) procedure by conventional heating, one combined microwave-assisted and conventional heating WD procedure, and one fusion procedure. Chemical analysis was carried out by ICP-AES. Five major (Si, Al, Fe, Ca, Mg), three minor (Mn, Ba, Ti) and two trace (Cu, Co) elements were determined and compared with their certified values. Quantitation was performed at two different spectral lines for each element and multi-element matrix-matched calibration standards were used. The recovery values for the six decomposition procedures ranged between 75 and 110% with a few notable exceptions. Data were processed statistically in order to evaluate the investigated decomposition procedures in terms of recovery, accuracy and precision, and eventually select the most appropriate one for ancient pottery analysis.

Determination of uranium isotopes (235U, 238U) and trace elements (Cd, Pb, Cu and As) in bottled drinking water by Icp-SFMS

International Nuclear Information System (INIS)

Lara A, N.; Hernandez M, H.; Romero G, E. T.; Kuri de la C, A.; Perez B, M. A.

2016-09-01

In the present work we propose an optimized method for the quantification of uranium isotopes ( 235 U, 2 38 U) and the elements Cd, Pb, Cu and As in bottled water for drinking at trace levels of concentration. Based on the multi-element detection capability, the high sensitivity and resolution that the Mass Spectrometry with Magnetic Sector with Inductively Coupled Plasma Source (Icp-SFMS) technique offers; the high, medium and low resolution analysis conditions for the elements under study were established and optimized using and Element 2/Xr equipment and the 23 multi-elemental Certified Reference Material (CRM). The analysis method was validated using the standard reference material Nist 1643d and CRM mono-elemental s as external standards for the quantification of the analytes. Samples, targets and CRM were acidified with 2% of HNO 3 and analyzed without pretreatment under the established analysis conditions. The results obtained show concentrations of 235 U, 238 U, 111 Cd, 208 Pb, 63 Cu and 75 As in the range of μg L -1 , the linearity obtained from the calibration curves for each element has correlation coefficients < 0.99 in all cases, the accuracy of the method in terms of percent relative standard deviation (RSD %) was less than 5%, the mean recovery rate of Nist 1643d ranged from 96.46% to 101.12%. The optimization of the method guarantees the stability and calibration of the equipment throughout the analysis, as well as the ability to resolve interferences. In conclusion, the method proposed using Icp-SFMS offers the advantages of being fast and simple for the multi-elemental analysis in water at trace levels, with low limits of quantification and detection, with good linearity, accuracy, precision and reproducibility to a degree of reliability of 95%. (Author)

In-Situ Sampling Analysis of a Jupiter Trojan Asteroid by High Resolution Mass Spectrometry in the Solar Power Sail Mission

Science.gov (United States)

Kebukawa, Y.; Aoki, J.; Ito, M.; Kawai, Y.; Okada, T.; Matsumoto, J.; Yano, H.; Yurimoto, H.; Terada, K.; Toyoda, M.; Yabuta, H.; Nakamura, R.; Cottin, H.; Grand, N.; Mori, O.

2017-12-01

The Solar Power Sail (SPS) mission is one of candidates for the upcoming strategic middle-class space exploration to demonstrate the first outer Solar System journey of Japan. The mission concept includes in-situ sampling analysis of the surface and subsurface (up to 1 m) materials of a Jupiter Trojan asteroid using high resolution mass spectrometry (HRMS). The candidates for the HRMS are multi-turn time-of-flight mass spectrometer (MULTUM) type and Cosmorbitrap type. We plan to analyze isotopic and elemental compositions of volatile materials from organic matter, hydrated minerals, and ice (if any), in order to understand origin and evolution of the Jupiter Trojan asteroids. It will provide insights into planet formation/migration theories, evolution and distribution of volatiles in the Solar System, and missing link between asteroids and comets on evolutional. The HRMS system allows to measure H, N, C, O isotopic compositions and elemental compositions of molecules prepared by various pre-MS procedures including stepwise heating up to 600ºC, gas chromatography (GC), and high-temperature pyrolysis with catalyst to decompose the samples into simple gaseous molecules (e.g., H2, CO, and N2) for isotopic ratio analysis. The required mass resolution should be at least 30,000 for analyzing isotopic ratios for simple gaseous molecules. For elemental compositions, mass accuracy of 10 ppm is required to determine elemental compositions for molecules with m/z up to 300 (as well as compound specific isotopic compositions for smaller molecules). Our planned analytical sequences consist of three runs for both surface and subsurface samples. In addition, `sniff mode' which simply introduces environmental gaseous molecules into a HRMS will be done by the system.

Carbon Nanotube Fiber Ionization Mass Spectrometry: A Fundamental Study of a Multi-Walled Carbon Nanotube Functionalized Corona Discharge Pin for Polycyclic Aromatic Hydrocarbons Analysis

Science.gov (United States)

Nahan, Keaton S.; Alvarez, Noe; Shanov, Vesselin; Vonderheide, Anne

2017-09-01

Mass spectrometry continues to tackle many complicated tasks, and ongoing research seeks to simplify its instrumentation as well as sampling. The desorption electrospray ionization (DESI) source was the first ambient ionization source to function without extensive gas requirements and chromatography. Electrospray techniques generally have low efficiency for ionization of nonpolar analytes and some researchers have resorted to methods such as direct analysis in real time (DART) or desorption atmospheric pressure chemical ionization (DAPCI) for their analysis. In this work, a carbon nanotube fiber ionization (nanoCFI) source was developed and was found to be capable of solid phase microextraction (SPME) of nonpolar analytes as well as ionization and sampling similar to that of direct probe atmospheric pressure chemical ionization (DP-APCI). Conductivity and adsorption were maintained by utilizing a corona pin functionalized with a multi-walled carbon nanotube (MWCNT) thread. Quantitative work with the nanoCFI source with a designed corona discharge pin insert demonstrated linearity up to 0.97 (R2) of three target PAHs with phenanthrene internal standard. [Figure not available: see fulltext.

Determination of multi-element in marine sediment samples collected in Angola by the k0-NAA technique

International Nuclear Information System (INIS)

Teixeira, M.C.P.; Ho Manh Dung; Cao Dong Vu; Nguyen Thi Sy; Nguyen Thanh Binh; Vuong Huu Tan

2006-01-01

The marine sediment samples were designed to collect in Angola for marine environmental pollution study. The k 0 -standardization method of neutron activation analysis (k 0 -NAA) on Dalat research reactor has been developed to determine of multi-element in the Angola marine sediment samples. The samples were irradiated in cell 7-1 for short- and middle-lived nuclides and rotary specimen rack for long-lived nuclides. The irradiation facilities were characterized for neutron spectrum parameters and post-activated samples were measured on the calibrated gamma-ray spectrometers using HPGe detectors. The analytical results for 9 marine sediment samples with 27 elements: Al, As, Br, Ca, Ce,Cl, Co, Cs, Dy, Fe, Hf, I, K, Mg, Mn, Na, Rb, Sb, Sc, Se, Sm, Th, Ti, U, V and Zn in term of mean concentration, standard deviation and their content range are shown in the report. The analytical quality assurance was done by analysis of a Japan's certified reference material namely marine sediment NMIJ-CRM-7302a. These preliminary results revealed that the k 0 -NAA technique on the Dalat research reactor is a good analytical technique for determination of multi-element in the marine sediment samples. Some heavy metals and trace elements determined in this work possibly connected to the human activities at the sampling region. (author)

Elemental concentration analysis in the brain of young and old Wistar rats by total reflection X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Serpa, Renata F.B.; Jesus, Edgar F.O. de; Lopes, Ricardo T.; Anjos, Marcelino J. dos; Carmo, Maria G.T. do; Rocha, Monica S.; Moreira, Silvana; Martinez, Ana M.B.

2007-01-01

It is well known that aging is associated with neurobehavioral deficits. The aging process of human brain is characterized by progressive neuronal loss. Furthermore, certain brain areas are more vulnerable to neuronal degeneration than others, reflecting an altered resistance to stress of the tissue itself and/or the lack of adequate immunological defense mechanisms in these regions. About the elemental levels in the brain, it is known that the excess ou deficiency of some elements are toxic for human healthy, being also related to several neurodegenerative diseases. In this way, the main goal of this work was to determine the elemental concentration in the hippocampus of young and old male (n = 10) and female (n = 10) Wistar rats by total reflection X-ray fluorescence spectrometry with synchrotron radiation (SR-TXRF). These measurements were carried out at XRF beam line at Light Synchrotron Brazilian Laboratory, Campinas, Brazil. About the results, we could observe that Al, Fe, Cu, Zn and Br levels were higher in the hippocampus of the old female rats than the young ones. On the other hand, only Cu levels were higher in the hippocampus of the old male rats than the young ones. Therefore, the aging of the hippocampus of the female rats can be characterized by an accumulate for Al, Fe, Cu, Zn and Br. The excess in these elements levels are also associated with several neurodegenerative disorders, such as Alzheimer' disease, Parkinson's disease and Huntington's disease. (author)

Analysis of mass spectrometry data in proteomics

DEFF Research Database (Denmark)

Matthiesen, Rune; Jensen, Ole N

2008-01-01

The systematic study of proteins and protein networks, that is, proteomics, calls for qualitative and quantitative analysis of proteins and peptides. Mass spectrometry (MS) is a key analytical technology in current proteomics and modern mass spectrometers generate large amounts of high-quality data...... that in turn allow protein identification, annotation of secondary modifications, and determination of the absolute or relative abundance of individual proteins. Advances in mass spectrometry-driven proteomics rely on robust bioinformatics tools that enable large-scale data analysis. This chapter describes...... some of the basic concepts and current approaches to the analysis of MS and MS/MS data in proteomics....

Development of an accurate, sensitive, and robust isotope dilution laser ablation ICP-MS method for simultaneous multi-element analysis (chlorine, sulfur, and heavy metals) in coal samples

Energy Technology Data Exchange (ETDEWEB)

Boulyga, Sergei F. [University of Natural Resources and Applied Life Sciences, Department of Chemistry, Division of Analytical Chemistry-VIRIS Laboratory, Vienna (Austria); Johannes Gutenberg-University, Institute of Inorganic Chemistry and Analytical Chemistry, Mainz (Germany); Heilmann, Jens; Heumann, Klaus G. [Johannes Gutenberg-University, Institute of Inorganic Chemistry and Analytical Chemistry, Mainz (Germany); Prohaska, Thomas [University of Natural Resources and Applied Life Sciences, Department of Chemistry, Division of Analytical Chemistry-VIRIS Laboratory, Vienna (Austria)

2007-10-15

A method for the direct multi-element determination of Cl, S, Hg, Pb, Cd, U, Br, Cr, Cu, Fe, and Zn in powdered coal samples has been developed by applying inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) with laser-assisted introduction into the plasma. A sector-field ICP-MS with a mass resolution of 4,000 and a high-ablation rate laser ablation system provided significantly better sensitivity, detection limits, and accuracy compared to a conventional laser ablation system coupled with a quadrupole ICP-MS. The sensitivity ranges from about 590 cps for {sup 35}Cl{sup +} to more than 6 x 10{sup 5} cps for {sup 238}U{sup +} for 1 {mu}g of trace element per gram of coal sample. Detection limits vary from 450 ng g{sup -1} for chlorine and 18 ng g{sup -1} for sulfur to 9.5 pg g{sup -1} for mercury and 0.3 pg g{sup -1} for uranium. Analyses of minor and trace elements in four certified reference materials (BCR-180 Gas Coal, BCR-331 Steam Coal, SRM 1632c Trace Elements in Coal, SRM 1635 Trace Elements in Coal) yielded good agreement of usually not more than 5% deviation from the certified values and precisions of less than 10% relative standard deviation for most elements. Higher relative standard deviations were found for particular elements such as Hg and Cd caused by inhomogeneities due to associations of these elements within micro-inclusions in coal which was demonstrated for Hg in SRM 1635, SRM 1632c, and another standard reference material (SRM 2682b, Sulfur and Mercury in Coal). The developed LA-ICP-IDMS method with its simple sample pretreatment opens the possibility for accurate, fast, and highly sensitive determinations of environmentally critical contaminants in coal as well as of trace impurities in similar sample materials like graphite powder and activated charcoal on a routine basis. (orig.)

SAFE-AXISYM, Stress Analysis of Axisymmetric Composite Structure by Finite Elements Method

International Nuclear Information System (INIS)

Cornell, D.C.

1967-01-01

1 - Nature of physical problem solved: SAFE-AXISYM is a program for the analysis of multi-material axisymmetric composite structures. It is designed for the analysis of heterogeneous structures such as reinforced and/or prestressed concrete vessels. The structure is assumed to be linearly elastic, and only bodies of revolution subjected to axisymmetric loading can be treated. 2 - Method of solution: SAFE-AXISYM uses a finite element method with a modified Gauss-Seidel iteration scheme. A reference grid subdivides the structure into ring-like small, finite elements, the vertices of which are called nodes. The grid may be generated by hand, by the computer or by a combination of the two methods. Each node has two degrees of freedom, translation in the and in the axial direction. Both zero and non-zero fixed displacement constraints may be assumed, and the loading condition may be mechanical and/or thermal. 3 - Restrictions on the complexity of the problem: Multi-material structures with varying rigidities converge very slowly. Not valid for incompressible materials. Maximum number of nodes = 475. Maximum number of elements = 1100

Analysis of iron-base alloys by low-wattage glow discharge emission spectrometry

International Nuclear Information System (INIS)

Wagatsuma, K.; Hirokawa, K.

1984-01-01

Several iron-base alloys were investigated by low-wattage glow discharge emission spectrometry. The emission intensity principally depended on the sputtering parameters of constituent elements in the alloy. However, in the case of chromium, stable and firm oxides formed on the surface influencing the yield of ejected atoms. This paper discusses the relation between the sputtering parameters in Fe-Ni, Fe-Cr, and Fe-Co alloys and their relative emission intensities. Additionally, quantitative analysis was performed for some ternary iron-base alloys and commercial stainless steels with the calibration factors of binary alloy systems

Elemental analysis of sub-hourly ambient aerosol collections

Energy Technology Data Exchange (ETDEWEB)

Kidwell, C.B.; Ondov, J.M. [University of Maryland, College Park, MD (USA). Dept. of Chemical & Biochemistry

2004-03-01

Simultaneous multielement graphite furnace atomic absorption spectrometry was used to determine Al, As, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Sb, Se, and Zn in ambient air sampled at 170 L.min{sup -1} for 30 min and collected as a slurry after dynamic preconcentration. Analyses of slurries of NIST SRM 1648, Urban Particulate Matter, were typically within 10% of expected values for all elements except Al, Cr, and Fe, elements for which deviations were mostly due to difficulties in transferring large particles. This problem will be reduced for urban fine particulate matter samples (PM2.5). Trends in the concentrations of elemental source markers were readily correlated with wind direction and other meteorological factors to identify the influences of local industrial emissions, including motor vehicle traffic, coal- and oil-fired power plants, and municipal incinerators. Factor analysis was applied to the 88-sample data set to extract 7 factors: urban dust, meteorological factors, incinerators, coal- fired power plants, Tour Bus emission, unknown As source, and oil-fired power plants. Factor analysis was also applied to an 18-sample data set representing 2.5 h averages of the 30 min data to simulate the effect of longer sample collection times. Only 6 factors were extracted from this data set, which shows that increased temporal resolution enhances the power of factor analysis to resolve sources. These results indicate that a wealth of detailed information is revealed at this level of temporal resolution.

Multi-element analysis of the rat hippocampus by proton induced x-ray emission spectroscopy (phosphorus, sulfur, chlorine, potassium, calcium, iron, zinc, copper, lead, bromine, and rubidium)

Energy Technology Data Exchange (ETDEWEB)

Kemp, K.; Danscher, G.

1979-01-22

A technique for multi-element analysis of brain tissue by proton induced x-ray emission spectroscopy (PIXE) is described and data from analysis of fixed and unfixed samples from rat hippocampus, neocortex, amygdala, and spinal cord are presented and commented on. The atoms present in the tissue are bombarded with protons which cause the ejection of electrons from the inner shells. When the holes are refilled with electrons from outer shells, x-ray quanta characteristic for each element are emitted. Using a high resolution energy dispersive detector, a complete x-ray spectrum of the specimen can be recorded in a single measurement. Detection limits less than or approximately 5 ppM of dry matter are obtained for most elements with atomic number greater than 14 (silicon). Around 13 elements were found in concentrations above the detection limits. The grand means for non-fixed hippocampi were e.g., for Zn-120 ppM; Rb-20 ppM; Fe-150 ppM; Pb-3 ppM; Ni-5 ppM.

MULTI-DIMENSIONAL MASS SPECTROMETRY-BASED SHOTGUN LIPIDOMICS AND NOVEL STRATEGIES FOR LIPIDOMIC ANALYSES

Science.gov (United States)

Han, Xianlin; Yang, Kui; Gross, Richard W.

2011-01-01

Since our last comprehensive review on multi-dimensional mass spectrometry-based shotgun lipidomics (Mass Spectrom. Rev. 24 (2005), 367), many new developments in the field of lipidomics have occurred. These developments include new strategies and refinements for shotgun lipidomic approaches that use direct infusion, including novel fragmentation strategies, identification of multiple new informative dimensions for mass spectrometric interrogation, and the development of new bioinformatic approaches for enhanced identification and quantitation of the individual molecular constituents that comprise each cell’s lipidome. Concurrently, advances in liquid chromatography-based platforms and novel strategies for quantitative matrix-assisted laser desorption/ionization mass spectrometry for lipidomic analyses have been developed. Through the synergistic use of this repertoire of new mass spectrometric approaches, the power and scope of lipidomics has been greatly expanded to accelerate progress toward the comprehensive understanding of the pleiotropic roles of lipids in biological systems. PMID:21755525

The determination of trace elements in uranium ores by x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

De Villiers, W. van Z.

1983-11-01

The determination of 17 trace elements (As, Ba, Co, Cr, Cu, Mo, Nb, Ni, Pb, Rb, Sr, Th, U, V, Y, Zn and Zr) in uranium ores by x-ray fluorescence spectrometry was investigated in this study. The determination of major elements was also necessary for the calculation of mass absorption coefficients. Initially a method was developed for the determination of the elements of interest in unmineralised silicates. Correction for absorption of radiation by the sample were made by means of mass absorption coefficients which were obtained from the relation between the inverse of the mass absorption coefficient and the intensity of the Compton scattering peak. The Feather and Willis method was used for determining the background intensity at the peak positions as well as for mass absorption coefficients. It was observed that the background intensity in the region of the uranium lines increases with increasing uranium content of the sample

Trace element analysis by EPMA in geosciences: detection limit, precision and accuracy

Science.gov (United States)

Batanova, V. G.; Sobolev, A. V.; Magnin, V.

2018-01-01

Use of the electron probe microanalyser (EPMA) for trace element analysis has increased over the last decade, mainly because of improved stability of spectrometers and the electron column when operated at high probe current; development of new large-area crystal monochromators and ultra-high count rate spectrometers; full integration of energy-dispersive / wavelength-dispersive X-ray spectrometry (EDS/WDS) signals; and the development of powerful software packages. For phases that are stable under a dense electron beam, the detection limit and precision can be decreased to the ppm level by using high acceleration voltage and beam current combined with long counting time. Data on 10 elements (Na, Al, P, Ca, Ti, Cr, Mn, Co, Ni, Zn) in olivine obtained on a JEOL JXA-8230 microprobe with tungsten filament show that the detection limit decreases proportionally to the square root of counting time and probe current. For all elements equal or heavier than phosphorus (Z = 15), the detection limit decreases with increasing accelerating voltage. The analytical precision for minor and trace elements analysed in olivine at 25 kV accelerating voltage and 900 nA beam current is 4 - 18 ppm (2 standard deviations of repeated measurements of the olivine reference sample) and is similar to the detection limit of corresponding elements. To analyse trace elements accurately requires careful estimation of background, and consideration of sample damage under the beam and secondary fluorescence from phase boundaries. The development and use of matrix reference samples with well-characterised trace elements of interest is important for monitoring and improving of the accuracy. An evaluation of the accuracy of trace element analyses in olivine has been made by comparing EPMA data for new reference samples with data obtained by different in-situ and bulk analytical methods in six different laboratories worldwide. For all elements, the measured concentrations in the olivine reference sample

Determination of the elemental composition of ferromanganese formations certified reference materials by mass-spectrometry with inductively coupled plasma

Directory of Open Access Journals (Sweden)

N. V. Zarubina

2014-01-01

Full Text Available Contents of 41 elements in the Russian standard samples of ferromanganese nodules OOPE 601, OOPE 602, OOPE 603 and ore crust OOPE 604 were identified by mass-spectrometry with inductively-coupled plasma. Content of W was firstly presented in the sample OOPE-603. Relative standard deviation for most elements was in the range of 3-10%. A description of ICP-MS technique including sample preparation procedure and other instrumental parameters were given as well as analysis of ferromanganese nodules standard samples NOD-A-1 and NOD-P-1 of U.S. Geological Survey was demonstrated for validation. Normalized to chondrite distribution curves of REE in the studied samples were shown as an indicator of the internal consistency offound concentrations. The available literature data on the content of a wide range of elements and its comparison with the matter obtained by us was produced. Measured contents of elements in the established CRM may be useful in the analytical practice to evaluate precision of results. There is a lack of relevant information on a variety of geochemically important elements in the Russian standard samples of OOPE series and the new data can be taken into account in their certification.

Statistical Methods in Assembly Quality Management of Multi-Element Products on Automatic Rotor Lines

Science.gov (United States)

Pries, V. V.; Proskuriakov, N. E.

2018-04-01

To control the assembly quality of multi-element mass-produced products on automatic rotor lines, control methods with operational feedback are required. However, due to possible failures in the operation of the devices and systems of automatic rotor line, there is always a real probability of getting defective (incomplete) products into the output process stream. Therefore, a continuous sampling control of the products completeness, based on the use of statistical methods, remains an important element in managing the quality of assembly of multi-element mass products on automatic rotor lines. The feature of continuous sampling control of the multi-element products completeness in the assembly process is its breaking sort, which excludes the possibility of returning component parts after sampling control to the process stream and leads to a decrease in the actual productivity of the assembly equipment. Therefore, the use of statistical procedures for continuous sampling control of the multi-element products completeness when assembled on automatic rotor lines requires the use of such sampling plans that ensure a minimum size of control samples. Comparison of the values of the limit of the average output defect level for the continuous sampling plan (CSP) and for the automated continuous sampling plan (ACSP) shows the possibility of providing lower limit values for the average output defects level using the ACSP-1. Also, the average sample size when using the ACSP-1 plan is less than when using the CSP-1 plan. Thus, the application of statistical methods in the assembly quality management of multi-element products on automatic rotor lines, involving the use of proposed plans and methods for continuous selective control, will allow to automating sampling control procedures and the required level of quality of assembled products while minimizing sample size.

Measurements of environmental gamma-ray spectra using a multi-element TL dosemeter

International Nuclear Information System (INIS)

Furuta, Sadaaki; Boetter-Jensen, L.; Nielsen, S.P.

1986-12-01

A method to estimate the energy distribution and dose of environmental gamma radiation was developed using a multielement TL dosemeter. Experimentally obtained energy responses from a multi-element TL dosemeter with different kinds of filters were used to calculate the energy distribution and related dose by the SAND-II computer code. The code was originally developed to estimate the neutron flux using a multiple foil activation method. Measurements were made at several locations with the multi-element TL dosemeter and comparisons were made with results from a NaI(Tl) scintillation detector and a high-pressure ionization chamber. (author)

Characterization of chemical elements in soil submitted to different systems use and management by energy dispersive x-ray fluorescence spectrometry (EDXRF)

International Nuclear Information System (INIS)

Wastowski, Arci Dirceu; Rosa, Genesio Mario da; Cherubin, Mauricio Roberto; Rigon, Joao Paulo Gonsiorkiewicz

2010-01-01

This study aimed to evaluate the chemical elements levels in soil, submitted to different management systems and use by the Energy Dispersive X-Ray Fluorescence Spectrometry - EDXRF. The systems were T1 - agroforestry (SAF), T2 - native field (CN), T3 - native forest (NM), T4 - tillage forest (PF); T5 - conventional tillage system (SPC) and T6 - system tillage (NT). Samples were collected at 0-10 and 10-20 cm, dried and ground for analysis in EDX-720. The soil showed no difference in the average concentrations of chemical elements analyzed in the profiles, but the systems presented different concentrations of metal elements, and T3 had the highest K, Ca and Zn at 0-10 cm and higher contents of K, Ca, Cu, Zn and Mn in the layer of 10-20 cm. (author)

Separation of interfering elements in the neutron activation analysis of lanthanides in geological materials

International Nuclear Information System (INIS)

Saiki, M.

1988-01-01

A chemical procedure has been developed for the separation of U, Th, Fe, Sc, Na,Ta, and Mo which interfere in the neutron activation analysis of the lanthanide elements in geological materials. This procedure is based on the solvent extraction of interferents using a solution of tetracycline in benzyl alcohol. The lanthanide elements remaining in the aqueous phase are coprecipitated on calcium oxalate or ferric hydroxide for irradiation and subsequent determination by gamma ray spectrometry. The chemical separation procedure was applied in the analysis of lanthanides in two international geological reference materials GSP-1 (USGS), GS-N (CRPG) and in the analysis of a volcanic rock from Pocos de Caldas, MG, Brazil. The sensitivities for all the lanthanides were determined. (author) [pt

Analysis of humic colloid borne trace elements by flow field-flow fractionation, gel permeation chromatography and icp-mass spectrometry

International Nuclear Information System (INIS)

Ngo, Manh Thang; Beck, H.P; Geckeis, H.; Kim, J.I.

1999-01-01

Groundwater samples containing aquatic humic substances are analyzed by flow field- flow fractionation (FFFF) and gel permeation chromatography (GPC). Natural concentrations of U, Th and rare earth elements (REE) in a size-fractionated groundwater sample are analyzed by on-line coupling of inductively coupled plasma-mass spectrometry (ICP-MS) to either FFFF or GPC. The uranium, thorium, and REE are found to be quantitatively attached to colloidal species in the investigated groundwater sample. Their distribution in different colloid size fractions, however, is quite heterogeneous. Both, FFFF and GPC reveal that Th and REE are preferentially located in the size fraction > 50 kDalton. U is also attached to low molecular weight humic acid, similar to Fe and Al. This finding could be qualitatively reproduced by sequential ultrafiltration. The results are interpreted in terms of different binding mechanisms for the individual elements in the heterogeneous humic macromolecules. The inclusion of actinides into larger aggregates of aquatic humic acid might explain the considerable kinetic hindrance of actinide-humic acid dissociation reactions described in the literature. (authors)

Solving the Einstein constraint equations on multi-block triangulations using finite element methods

Energy Technology Data Exchange (ETDEWEB)

Korobkin, Oleg; Pazos, Enrique [Department of Physics and Astronomy, Louisiana State University, Baton Rouge, LA 70803 (United States); Aksoylu, Burak [Center for Computation and Technology, Louisiana State University, Baton Rouge, LA 70803 (United States); Holst, Michael [Department of Mathematics, University of California at San Diego 9500 Gilman Drive La Jolla, CA 92093-0112 (United States); Tiglio, Manuel [Department of Physics, University of Maryland, College Park, MD 20742 (United States)

2009-07-21

In order to generate initial data for nonlinear relativistic simulations, one needs to solve the Einstein constraints, which can be cast into a coupled set of nonlinear elliptic equations. Here we present an approach for solving these equations on three-dimensional multi-block domains using finite element methods. We illustrate our approach on a simple example of Brill wave initial data, with the constraints reducing to a single linear elliptic equation for the conformal factor psi. We use quadratic Lagrange elements on semi-structured simplicial meshes, obtained by triangulation of multi-block grids. In the case of uniform refinement the scheme is superconvergent at most mesh vertices, due to local symmetry of the finite element basis with respect to local spatial inversions. We show that in the superconvergent case subsequent unstructured mesh refinements do not improve the quality of our initial data. As proof of concept that this approach is feasible for generating multi-block initial data in three dimensions, after constructing the initial data we evolve them in time using a high-order finite-differencing multi-block approach and extract the gravitational waves from the numerical solution.

Solving the Einstein constraint equations on multi-block triangulations using finite element methods

International Nuclear Information System (INIS)

Korobkin, Oleg; Pazos, Enrique; Aksoylu, Burak; Holst, Michael; Tiglio, Manuel

2009-01-01

In order to generate initial data for nonlinear relativistic simulations, one needs to solve the Einstein constraints, which can be cast into a coupled set of nonlinear elliptic equations. Here we present an approach for solving these equations on three-dimensional multi-block domains using finite element methods. We illustrate our approach on a simple example of Brill wave initial data, with the constraints reducing to a single linear elliptic equation for the conformal factor ψ. We use quadratic Lagrange elements on semi-structured simplicial meshes, obtained by triangulation of multi-block grids. In the case of uniform refinement the scheme is superconvergent at most mesh vertices, due to local symmetry of the finite element basis with respect to local spatial inversions. We show that in the superconvergent case subsequent unstructured mesh refinements do not improve the quality of our initial data. As proof of concept that this approach is feasible for generating multi-block initial data in three dimensions, after constructing the initial data we evolve them in time using a high-order finite-differencing multi-block approach and extract the gravitational waves from the numerical solution.

Methods for analysis of uranium-plutonium mixed fuel and transplutonium elements at RIAR (Preprint no. IT-25)

International Nuclear Information System (INIS)

Timofeev, G.A.

1991-02-01

Different methods for analysis of the uranium-plutonium mixed nuclear fuel and transplutonium elements are briefly discussed in this paper: coulometry, radiometric techniques, emission spectrography, mass-spectrometry, chromatography, spectrophotometry. The main analytical characteristics of the methods developed are given. (author). 30 refs., 2 tabs

Identification of Se trace element in the soybean using neutron activation analysis

International Nuclear Information System (INIS)

Sihombing, E.; Sri Wardani; Hamzah, A.

1999-01-01

Neutron Activation Analysis method has been developed as a fast analysis method with high sensitivity, accuracy and precision in determining distribution of element content of various types of seed food materials. In this research the element content of Se was determined by irradiating sample of black and white soybean that can be bought in the market. For determining the content of long decay time element of Se, a samples of 1.3 - 2.3 grams of seed was irradiated within 45 minutes where as for short decay time of Se, the 1,2 - 2,2 grams of seed was irradiated within 30 minutes in the reactor wall. The activated sample, then, was analyzed using gamma spectrometry method. The gamma spectrum was acquired with Hp Ge detector with counting time within 2 - 60 minutes. The results showed that there is a small deviation on Se's quantity of contents with vary between 154,2 and 165,8 ppb

XRF analysis of portland cement for major and trace elements

International Nuclear Information System (INIS)

Abdunnabi, A. R.

2012-12-01

Libyan portland cement produced in several factories around the country, in Lip tis, Zoltan, Souq-Elkamis, Dernah and El-Fatach, were analyzed for quantitative major and trace elements and mineral content, which were compered with those imported from Spain, Romania, Cyprus, and Egypt. X-ray fluorescence spectro X lab 2000 spectrometer equipped with Rh-and X-ray tube was used for the analysis of various samples. The detector Si(Li) with a resolution of 148 eV at Mn K-a=5.9 keV facilitates the determination of a wide range of elements from sodium to uranium, with a detection limit at sub levels. Cement samples in the powder form were analyzed using the pellet-technique. The pellets were prepared by mixing 4g of the cement powder with 0.9 g of binder (HWC) and pressed at high pressure. A ful analysis including, background counting, matrix correction and all relevant corrections were achieved automatically by XLAB 2000 software package. For major and trace elements X RF results were higher for most of the elements than those analyzed with atomic absorption spectrometry. The mineral content showed that Libyan cement is comparable to the imported ones, also the Libyan cement meets the requirements of the international specifications of the portland cement. (Author)

MULTI ELEMENT SI SENSOR WITH READOUT ASIC FOR EXAFS SPECTROSCOPY.

Energy Technology Data Exchange (ETDEWEB)

DE GERONIMO,G.; O CONNOR,P.; BEUTTENMULLER,R.H.; LI,Z.; KUCZEWSKI,A.J.; SIDDONS,D.P.

2002-09-09

Extended X-ray Absorption Fine Structure (EXAFS) experiments impose stringent requirements on a detection system, due to the need for processing ionizing events at a high rate, typically above of 10Mcps/cm{sup 2}, and with a high resolution, typically better than 300eV. The detection system here presented is being developed targeting these stringent requirements. It is the result of a cooperation between the Instrumentation Division and the National Synchrotron Light Source (NSLS) of the Brookhaven National Laboratory (BNL). The system is composed of a multi-element Si sensor with dedicated per pixel electronics. The combination of high rate, high resolution and moderate complexity makes this system attractive when compared to other multi-element solutions. In sections 2, 3 and 4 the sensor, the interconnect and the electronics are briefly described. Section 5 reports on the first experimental results.

Mass spectrometry for real-time quantitative breath analysis

Czech Academy of Sciences Publication Activity Database

Smith, D.; Španěl, Patrik; Herbig, J.; Beauchamp, J.

2014-01-01

Roč. 8, č. 2 (2014), 027101 ISSN 1752-7155 Institutional support: RVO:61388955 Keywords : breath analysis * proton transfer reaction mass spectrometry * selected ion flow tube mass spectrometry Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 4.631, year: 2014

Biosorption of Metals from Multi-Component Bacterial Solutions

CERN Document Server

Tsertsvadze, L A; Petriashvili, Sh G; Chutkerashvili, D G; Kirkesali, E I; Frontasyeva, M V; Pavlov, S S; Gundorina, S F

2002-01-01

The method of extraction of metals from industrial solutions by means of economical and easy to apply biosorbents in subtropics such as products of tea manufacturing, moss, microorganisms is described. The multi-component solutions obtained in the process of leaching of ores, rocks and industrial wastes by peat suspension were used in the experiments. The element composition of sorbent biomass and solutions was investigated by epithermal neutron activation analysis and by atomic absorption spectrometry. The results obtained evidence that the used biosorbents are applicable for extraction of the whole set of heavy metals and actinides (U, Th, Cu, Mn, Fe, Pb, Li, Rb, Sr, Cd, As, Co and others) from industrial solutions.

Studies of the source complex behaviour and of the ultrasound radiation of contact flexible multi-element transducers; Etudes du comportement complexe de source et du rayonnement ultrasonore des traducteurs multi-elements flexibles au contact

Energy Technology Data Exchange (ETDEWEB)

Amory, V

2007-12-15

This work deals with the ultrasonic nondestructive testing of parts with complex geometries using soft multi-element sensors. The different types of contact control configurations are presented first. Then, the difficulties encountered with conventional contact transducers are explained and the multi-element piezoelectric transducers technology, developed to meet these difficulties, is presented. The second chapter presents the results of finite-element calculations showing the complexity of a transducer in a condition of testing utilization. In a same configuration, the radiated far field calculated by finite-elements is compared to the measurement in order to validate the way the source behaviour is calculated. However, despite the efficiency of the finite-elements simulation, this tool is numerically too costly and cannot be used to optimize a full multi-element transducer. Therefore, a realistic source model is built and implemented in a radiation code based on high-frequency asymptotic approximations where only L and T volume waves are calculated. The incapacity of this model to reproduce the behaviour of T waves in some directions of propagation has led to give a particular attention to the fore-waves, neglected in the radiation calculation. Chapter 3 treats of the building of an exact radiation model taking into consideration the fore-waves contribution emitted by a contact transducer exerting a random space-time distribution constraint at the surface of the considered medium. A radiation model, based on the calculation of exact Green functions of the Lamb problem is proposed. The exact model is particularly interesting in the case of sensor geometries with a long length with respect to other dimensions (2D case). Field calculation results are shown for an element of the matrix network (3D case) and for a linear element (2D case). A study of different existing approached models is carried out as well. The last chapter presents some results of the field

Spectral response of multi-element silicon detectors

Energy Technology Data Exchange (ETDEWEB)

Ludewigt, B.A.; Rossington, C.S.; Chapman, K. [Univ. of California, Berkeley, CA (United States)

1997-04-01

Multi-element silicon strip detectors, in conjunction with integrated circuit pulse-processing electronics, offer an attractive alternative to conventional lithium-drifted silicon Si(Li) and high purity germanium detectors (HPGe) for high count rate, low noise synchrotron x-ray fluorescence applications. One of the major differences between the segmented Si detectors and the commercially available single-element Si(Li) or HPGe detectors is that hundreds of elements can be fabricated on a single Si substrate using standard silicon processing technologies. The segmentation of the detector substrate into many small elements results in very low noise performance at or near, room temperature, and the count rate of the detector is increased many-fold due to the multiplication in the total number of detectors. Traditionally, a single channel of detector with electronics can handle {approximately}100 kHz count rates while maintaining good energy resolution; the segmented detectors can operate at greater than MHz count rates merely due to the multiplication in the number of channels. One of the most critical aspects in the development of the segmented detectors is characterizing the charge sharing and charge loss that occur between the individual detector strips, and determining how these affect the spectral response of the detectors.

MultiSIMNRA: A computational tool for self-consistent ion beam analysis using SIMNRA

International Nuclear Information System (INIS)

Silva, T.F.; Rodrigues, C.L.; Mayer, M.; Moro, M.V.; Trindade, G.F.; Aguirre, F.R.; Added, N.; Rizzutto, M.A.; Tabacniks, M.H.

2016-01-01

Highlights: • MultiSIMNRA enables the self-consistent analysis of multiple ion beam techniques. • Self-consistent analysis enables unequivocal and reliable modeling of the sample. • Four different computational algorithms available for model optimizations. • Definition of constraints enables to include prior knowledge into the analysis. - Abstract: SIMNRA is widely adopted by the scientific community of ion beam analysis for the simulation and interpretation of nuclear scattering techniques for material characterization. Taking advantage of its recognized reliability and quality of the simulations, we developed a computer program that uses multiple parallel sessions of SIMNRA to perform self-consistent analysis of data obtained by different ion beam techniques or in different experimental conditions of a given sample. In this paper, we present a result using MultiSIMNRA for a self-consistent multi-elemental analysis of a thin film produced by magnetron sputtering. The results demonstrate the potentialities of the self-consistent analysis and its feasibility using MultiSIMNRA.

Analysis of antibiotics from liquid sample using electrospray ionization-ion mobility spectrometry

Energy Technology Data Exchange (ETDEWEB)

Shu, Li; Jian, Jia; Xiaoguang, Gao; Xiuli, He [State Key Laboratory of Transducer Technology, Institute of Electronics, Chinese Academy of Sciences, Beijing 100190 (China); Li Jianping, E-mail: jpli@mail.ie.ac.cn [State Key Laboratory of Transducer Technology, Institute of Electronics, Chinese Academy of Sciences, Beijing 100190 (China)

2012-03-30

Highlights: Black-Right-Pointing-Pointer The reduced mobilities of 18 antibiotics are determined. Black-Right-Pointing-Pointer Establishing antibiotic mass-mobility correlation using (12,4) potential model. Black-Right-Pointing-Pointer Multi-component characteristics of antibiotics can be revealed using ESI-IMS. Black-Right-Pointing-Pointer Most mixtures of antibiotics can be analyzed using ESI-IMS. Black-Right-Pointing-Pointer The detection limit of amoxicillin is 70 pg. - Abstract: The recent findings of antibiotic residues in aquatic environment at trace level have gained much concern for the detrimental effect on ecological and human health due to bacterial resistance. Here, the feasibility of using electrospray ionization ion mobility spectrometry (ESI-IMS) for analysis antibiotics in liquid sample is demonstrated. Reduced mobilities and collision cross sections of 18 antibiotics are experimentally measured and compared with theoretical values according to mass-mobility correlation. Gentamicin is used as an example to investigate the capability of ESI-IMS for multi-component analysis of antibiotics. Mixtures of antibiotics at different concentrations are analyzed. The estimated detection limit for amoxicillin is 0.7 mg L{sup -1} (70 pg) and the linear range of response maintains over two orders. This method will be a potential technique for the analysis of antibiotics in aquatic environment.

Phylogenetic Analysis Using Protein Mass Spectrometry.

Science.gov (United States)

Ma, Shiyong; Downard, Kevin M; Wong, Jason W H

2017-01-01

Through advances in molecular biology, comparative analysis of DNA sequences is currently the cornerstone in the study of molecular evolution and phylogenetics. Nevertheless, protein mass spectrometry offers some unique opportunities to enable phylogenetic analyses in organisms where DNA may be difficult or costly to obtain. To date, the methods of phylogenetic analysis using protein mass spectrometry can be classified into three categories: (1) de novo protein sequencing followed by classical phylogenetic reconstruction, (2) direct phylogenetic reconstruction using proteolytic peptide mass maps, and (3) mapping of mass spectral data onto classical phylogenetic trees. In this chapter, we provide a brief description of the three methods and the protocol for each method along with relevant tools and algorithms.

Analysis of aluminium by atomic absorption spectrometry and analysis of thorium and uranium by alpha spectrometry in the black sand of Egypt

International Nuclear Information System (INIS)

Hannachi, Dhouha; Mathlouthi, Nadia

2008-01-01

Throughout the period of our project of end of study carried out in the Center ; main road Sciences and Nuclear Engineering's CNSTN in one is tallied took one Egypt black sand simple with an aim has of knowing the activities of the existing radio elements and especially Uranium and Thorium. In the same mining, we try to take another Egypt black sand simple an aim has knowing the mass of aluminum by using a techniques in Atomique Absorption Spectrophotometer. After the radio chemical and Spectrometry analysis of the black sand sample we found the results following: - Egypt black sand is contains isotopes of Uranium such as 234 U and 238 U; - The Egypt black sand is contains isotopes of Thorium such as 230 Th and 232 Th. - L' Aluminum is a major. (Author)

Determination of rare-earth elements in rocks by isotope-excited X-ray fluorescence spectrometry

DEFF Research Database (Denmark)

Kunzendorf, Helmar; Wollenberg, H.A.

1970-01-01

Isotope-excited X-ray fluorescence spectrometry furnishes a rapid determination of rare-earth elements in unprepared rock samples. The samples are excited by 241Am γ-rays, generating X-ray spectra on a multichannel pulse-height analyser. Gaussian peaks of the Kα and Kβ X-ray energies are treated......-ray spectrometric scan of a longitudinally sliced drill core showed a close correlation between rare-earth abundances and appropriate minerals....

STUDIES OF CHOSEN TOXIC ELEMENTS CONCENTRATION IN MULTIFLOWER BEE HONEY

Directory of Open Access Journals (Sweden)

Ewa Popiela

2011-04-01

Full Text Available 72 544x376 Normal 0 21 false false false  The aim of the study was to determine the bioaccumulation level of chosen toxic elements (Zn, Cu, Pb, As and Cd in multiflower honey collected from Brzeg area. Biological material (honey was mineralized using the microwave technique at an elevated pressure in the microprocessor station of pressure in the type Mars 5. Quantitative analysis of elements (As, Cd, Cu, Pb and Zn was performed by plasma spectrometry method using a Varian ICP-AES apparatus. The presence of toxic elements was determined in examined biological materials. The elements fallowed the fallowing decreasing order with respect to their content of honey: Zn>Cu>Pb>As>Cd. The average concentrations of studied elements observed in multi-flower honey were as follows: 6.24 mg.kg-1 of zinc, 2.75 mg.kg-1 of copper, 0.53, 0.071, 0.042 mg.kg-1of lead, arsenic and cadmium, respectively. Lead was the most problematic in bee honey because its average content exceeded the maximum acceptable concentration. Additionally, this metal concentration was 60% higher in studied samples than allowable standard of lead content.doi:10.5219/134 

A framework for developing finite element codes for multi-disciplinary applications.

OpenAIRE

Dadvand, Pooyan

2007-01-01

The world of computing simulation has experienced great progresses in recent years and requires more exigent multidisciplinary challenges to satisfy the new upcoming demands. Increasing the importance of solving multi-disciplinary problems makes developers put more attention to these problems and deal with difficulties involved in developing software in this area. Conventional finite element codes have several difficulties in dealing with multi-disciplinary problems. Many of these codes are d...

Simultaneous acquisition of X-ray spectra using a multi-wire, position-sensitive gas flow detector

International Nuclear Information System (INIS)

Beaven, Peter A.; Marmotti, Mauro; Kampmann, Reinhard; Knoth, Joachim; Schwenke, Heinrich

2003-01-01

A multi-wire, gas-filled position-sensitive detector has been developed for the simultaneous recording of wavelength-dispersed X-ray signals that enables X-ray fluorescence spectrometry with a limited multi-element capability in the low Z element range. Details of the modular construction of the detector are given. The detector performance was characterized using Al-Kα radiation and a variable slit system. The detector has been applied in a laboratory spectrometer equipped with an electron source and a double multilayer mirror device as the wavelength-dispersing element. Spectra from Al and Si obtained in the simultaneous acquisition mode show good agreement with calculations performed using a ray-tracing model

Process recognition in multi-element soil and stream-sediment geochemical data

Science.gov (United States)

Grunsky, E.C.; Drew, L.J.; Sutphin, D.M.

2009-01-01

Stream-sediment and soil geochemical data from the Upper and Lower Coastal Plains of South Carolina (USA) were studied to determine relationships between soils and stream sediments. From multi-element associations, characteristic compositions were determined for both media. Primary associations of elements reflect mineralogy, including heavy minerals, carbonates and clays, and the effects of groundwater. The effects of groundwater on element concentrations are more evident in soils than stream sediments. A "winnowing index" was created using ratios of Th to Al that revealed differing erosional and depositional environments. Both soils and stream sediments from the Upper and Lower Coastal Plains show derivation from similar materials and subsequent similar multi-element relationships, but have some distinct differences. In the Lower Coastal Plain, soils have high values of elements concentrated in heavy minerals (Ce, Y, Th) that grade into high values of elements concentrated into finer-grain-size, lower-density materials, primarily comprised of carbonates and feldspar minerals (Mg, Ca, Na, K, Al). These gradational trends in mineralogy and geochemistry are inferred to reflect reworking of materials during marine transgressions and regressions. Upper Coastal Plain stream-sediment geochemistry shows a higher winnowing index relative to soil geochemistry. A comparison of the 4 media (Upper Coastal Plain soils and stream sediments and Lower Coastal Plain soils and stream sediments) shows that Upper Coastal Plain stream sediments have a higher winnowing index and a higher concentration of elements contained within heavy minerals, whereas Lower Coastal Plain stream sediments show a strong correlation between elements typically contained within clays. It is not possible to calculate a functional relationship between stream sediment-soil compositions for all elements due to the complex history of weathering, deposition, reworking and re-deposition. However, depending on

Multi-Stage Mass Spectrometry Analysis of Sugar-Conjugated β-Turn Structures to be Used as Probes in Autoimmune Diseases.

Science.gov (United States)

Giangrande, Chiara; Auberger, Nicolas; Rentier, Cédric; Papini, Anna Maria; Mallet, Jean-Maurice; Lavielle, Solange; Vinh, Joëlle

2016-04-01

Synthetic sugar-modified peptides were identified as antigenic probes in the context of autoimmune diseases. The aim of this work is to provide a mechanistic study on the fragmentation of different glycosylated analogs of a synthetic antigenic probe able to detect antibodies in a subpopulation of multiple sclerosis patients. In particular the N-glucosylated type I' β-turn peptide structure called CSF114(Glc) was used as a model to find signature fragmentations exploring the potential of multi-stage mass spectrometry by MALDI-LTQ Orbitrap. Here we compare the fragmentation of the glucosylated form of the synthetic peptide CSF114(Glc), bearing a glucose moiety on an asparagine residue, with less or non- immunoreactive forms, bearing different sugar-modifications, such as CSF114(GlcNAc), modified with a residue of N-acetylglucosamine, and CSF114[Lys(7)(1-deoxyfructopyranosyl)], this last one modified with a 1-deoxyfructopyranosyl moiety on a lysine at position 7. The analysis was set up using a synthetic compound specifically deuterated on the C-1 to compare its fragmentation with the fragmentation of the undeuterated form, and thus ascertain with confidence the presence on an Asn(Glc) within a peptide sequence. At the end of the study, our analysis led to the identification of signature neutral losses inside the sugar moieties to characterize the different types of glycosylation/glycation. The interest of this study lies in the possibility of applyimg this approach to the discovery of biomarkers and in the diagnosis of autoimmune diseases. Graphical Abstract GRAPHICAL ABSTRACT TEXT HERE] -->.

Analysis of elemental composition of porcelains unearthed from Waguantan kiln site by PIXE-RBS

Science.gov (United States)

Zhou, Z.; Zhang, K.; Xia, C. D.; Liu, M. T.; Zhu, J. J.; An, Z.; Bai, B.

2015-03-01

A method combining proton-induced X-ray emission spectrometry (PIXE) and Rutherford backscattering spectrometry (RBS) was used to determine the composition of 61 porcelain shards from the Yuan Dynasty (1271-1368 A.D.) unearthed from the Waguantan kiln site at Tianzhu County in Guizhou Province, China. Based on our previous experimental setup, an electron gun device with a LaB6 crystal cathode was installed to solve the problem created when the incident proton beams generated electric charge accumulations on the surfaces of the insulating porcelain samples, which induced a large bremsstrahlung background. The use of the electron gun has largely eliminated the large bremsstrahlung background and has therefore improved the detection limits for elements, especially for trace elements, and made it possible to determine the origin of the porcelains based on the trace elements. Major and trace elemental compositions of the porcelain bodies and glazes measured by PIXE and RBS were analyzed by the factor analysis method. The factor analysis showed that a few pieces of porcelain with a style similar to the porcelain of the Longquan kiln among the unearthed porcelains from the Waguantan kiln site did not have obvious differences in elemental compositions from other remaining porcelains unearthed from the Waguantan kiln site, indicating that the pieces of unearthed porcelain with the Longquan kiln style did in fact belong to the product fired locally by imitating the model of the Longquan celadon with local raw materials. This result therefore indicated that the Longquan kiln technology that originated from the Five Dynasties (907-960 A.D.) had been propagated to the Waguantan kiln site of Guizhou Province in the Yuan Dynasty.

Biomonitoring of air pollution through trace element analysis

International Nuclear Information System (INIS)

Akoto Bamford, Samuel; Osae, E.K.; Serfor-Armah, Y.; Nyarko, B.; Ofosu, F.; Aboh, I.J.; Odamtten, G.T.

2001-01-01

Research work is currently going on to determine the suitability in the use of local lichen species for biomonitoring air pollution in Ghana. The study areas being investigated are the gold-mining areas situated in the Moist Evergreen and Semi-Deciduous forests in Ghana. The nuclear analytical techniques being used in this work are instrumental neutron activation analysis and tube-excited x-ray fluorescence spectrometry. The present report covers results of quality control exercise carried out to validate the quantitative methods being used. This includes our participation in an intercomparison exercise carried out among participants of the IAEA coordinated research project. The samples analyzed were two lichen samples from two completely different areas using neutron activation analysis. Only short- and medium-lived irradiations were carried out. Satisfactory results were obtained for most of the elements identified and quantified. (author)

Application of Internal Standard Method for Several 3d-Transition Metallic Elements in Flame Atomic Absorption Spectrometry Using a Multi-wavelength High-resolution Spectrometer.

Science.gov (United States)

Toya, Yusuke; Itagaki, Toshiko; Wagatsuma, Kazuaki

2017-01-01

We investigated a simultaneous internal standard method in flame atomic absorption spectrometry (FAAS), in order to better the analytical precision of 3d-transition metals contained in steel materials. For this purpose, a new spectrometer system for FAAS, comprising a bright xenon lamp as the primary radiation source and a high-resolution Echelle monochromator, was employed to measure several absorption lines at a wavelength width of ca. 0.3 nm at the same time, which enables the absorbances of an analytical line and also an internal standard line to be estimated. In considering several criteria for selecting an internal standard element and the absorption line, it could be suggested that platinum-group elements: ruthenium, rhodium, or palladium, were suitable for an internal standard element to determine the 3d-transition metal elements, such as titanium, iron, and nickel, by measuring an appropriate pair of these absorption lines simultaneously. Several variances of the absorption signal, such as a variation in aspirated amounts of sample solution and a short-period drift of the primary light source, would be corrected and thus reduced, when the absorbance ratio of the analytical line to the internal standard line was measured. In Ti-Pd, Ni-Rh, and Fe-Ru systems chosen as typical test samples, the repeatability of the signal respnses was investigated with/without the internal standard method, resulting in better precision when the internal standard method was applied in the FAAS with a nitrous oxide-acetylene flame rather than an air-acetylene flame.

Analysis of elemental composition of porcelains unearthed from Waguantan kiln site by PIXE–RBS

International Nuclear Information System (INIS)

Zhou, Z.; Zhang, K.; Xia, C.D.; Liu, M.T.; Zhu, J.J.; An, Z.; Bai, B.

2015-01-01

Highlights: •We analyzed 61 unearthed porcelain shards in Yuan Dynasty by PIXE–RBS. •An electron gun was installed to solve the electric charge accumulations. •The factor analysis was performed for the element compositions. •The “exotic group” porcelain samples unearthed were produced locally. -- Abstract: A method combining proton-induced X-ray emission spectrometry (PIXE) and Rutherford backscattering spectrometry (RBS) was used to determine the composition of 61 porcelain shards from the Yuan Dynasty (1271–1368 A.D.) unearthed from the Waguantan kiln site at Tianzhu County in Guizhou Province, China. Based on our previous experimental setup, an electron gun device with a LaB 6 crystal cathode was installed to solve the problem created when the incident proton beams generated electric charge accumulations on the surfaces of the insulating porcelain samples, which induced a large bremsstrahlung background. The use of the electron gun has largely eliminated the large bremsstrahlung background and has therefore improved the detection limits for elements, especially for trace elements, and made it possible to determine the origin of the porcelains based on the trace elements. Major and trace elemental compositions of the porcelain bodies and glazes measured by PIXE and RBS were analyzed by the factor analysis method. The factor analysis showed that a few pieces of porcelain with a style similar to the porcelain of the Longquan kiln among the unearthed porcelains from the Waguantan kiln site did not have obvious differences in elemental compositions from other remaining porcelains unearthed from the Waguantan kiln site, indicating that the pieces of unearthed porcelain with the Longquan kiln style did in fact belong to the product fired locally by imitating the model of the Longquan celadon with local raw materials. This result therefore indicated that the Longquan kiln technology that originated from the Five Dynasties (907–960 A.D.) had been

Analysis of elemental composition of porcelains unearthed from Waguantan kiln site by PIXE–RBS

Energy Technology Data Exchange (ETDEWEB)

Zhou, Z. [Key Laboratory of Radiation Physics and Technology of Ministry of Education, Institute of Nuclear Science and Technology, Sichuan University, Chengdu 610064 (China); Zhang, K. [School of History and Culture, Sichuan University, Chengdu 610064 (China); Xia, C.D.; Liu, M.T.; Zhu, J.J. [Key Laboratory of Radiation Physics and Technology of Ministry of Education, Institute of Nuclear Science and Technology, Sichuan University, Chengdu 610064 (China); An, Z., E-mail: anzhu@scu.edu.cn [Key Laboratory of Radiation Physics and Technology of Ministry of Education, Institute of Nuclear Science and Technology, Sichuan University, Chengdu 610064 (China); Bai, B., E-mail: baibin@scu.edu.cn [School of History and Culture, Sichuan University, Chengdu 610064 (China)

2015-03-01

Highlights: •We analyzed 61 unearthed porcelain shards in Yuan Dynasty by PIXE–RBS. •An electron gun was installed to solve the electric charge accumulations. •The factor analysis was performed for the element compositions. •The “exotic group” porcelain samples unearthed were produced locally. -- Abstract: A method combining proton-induced X-ray emission spectrometry (PIXE) and Rutherford backscattering spectrometry (RBS) was used to determine the composition of 61 porcelain shards from the Yuan Dynasty (1271–1368 A.D.) unearthed from the Waguantan kiln site at Tianzhu County in Guizhou Province, China. Based on our previous experimental setup, an electron gun device with a LaB{sub 6} crystal cathode was installed to solve the problem created when the incident proton beams generated electric charge accumulations on the surfaces of the insulating porcelain samples, which induced a large bremsstrahlung background. The use of the electron gun has largely eliminated the large bremsstrahlung background and has therefore improved the detection limits for elements, especially for trace elements, and made it possible to determine the origin of the porcelains based on the trace elements. Major and trace elemental compositions of the porcelain bodies and glazes measured by PIXE and RBS were analyzed by the factor analysis method. The factor analysis showed that a few pieces of porcelain with a style similar to the porcelain of the Longquan kiln among the unearthed porcelains from the Waguantan kiln site did not have obvious differences in elemental compositions from other remaining porcelains unearthed from the Waguantan kiln site, indicating that the pieces of unearthed porcelain with the Longquan kiln style did in fact belong to the product fired locally by imitating the model of the Longquan celadon with local raw materials. This result therefore indicated that the Longquan kiln technology that originated from the Five Dynasties (907–960 A.D.) had been

Concentration of 17 Elements in Subcellular Fractions of Beef Heart Tissue Determined by Neutron Activation Analysis

Energy Technology Data Exchange (ETDEWEB)

Wester, P O

1964-12-15

Subcellular fractions of beef heart tissue are investigated, by means of neutron activation analysis, with respect to their concentration of 17 different elements. A recently developed ion-exchange technique combined with gamma spectrometry is used. The homogeneity of the subcellular fractions is examined electron microscopically. The following elements are determined: As, Ba, Br, Cas Co, Cs, Cu, Fe, Hg, La, Mo, P, Rb, Se, Sm, W and Zn. The determination of Ag, Au, Cd, Ce, Cr, Sb and Sc is omitted, in view of contamination. Reproducible and characteristic patterns of distribution are obtained for all elements studied.

Concentration of 17 Elements in Subcellular Fractions of Beef Heart Tissue Determined by Neutron Activation Analysis

International Nuclear Information System (INIS)

Wester, P.O.

1964-12-01

Subcellular fractions of beef heart tissue are investigated, by means of neutron activation analysis, with respect to their concentration of 17 different elements. A recently developed ion-exchange technique combined with gamma spectrometry is used. The homogeneity of the subcellular fractions is examined electron microscopically. The following elements are determined: As, Ba, Br, Cas Co, Cs, Cu, Fe, Hg, La, Mo, P, Rb, Se, Sm, W and Zn. The determination of Ag, Au, Cd, Ce, Cr, Sb and Sc is omitted, in view of contamination. Reproducible and characteristic patterns of distribution are obtained for all elements studied

Statistical analysis of proteomics, metabolomics, and lipidomics data using mass spectrometry

CERN Document Server

Mertens, Bart

2017-01-01

This book presents an overview of computational and statistical design and analysis of mass spectrometry-based proteomics, metabolomics, and lipidomics data. This contributed volume provides an introduction to the special aspects of statistical design and analysis with mass spectrometry data for the new omic sciences. The text discusses common aspects of design and analysis between and across all (or most) forms of mass spectrometry, while also providing special examples of application with the most common forms of mass spectrometry. Also covered are applications of computational mass spectrometry not only in clinical study but also in the interpretation of omics data in plant biology studies. Omics research fields are expected to revolutionize biomolecular research by the ability to simultaneously profile many compounds within either patient blood, urine, tissue, or other biological samples. Mass spectrometry is one of the key analytical techniques used in these new omic sciences. Liquid chromatography mass ...

Multielement determination of rare earth elements by liquid chromatography/inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

Sawatari, Hideyuki; Asano, Takaaki; Hu, Xincheng; Saizuka, Tomoo; Itoh, Akihide; Hirose, Akio; Haraguchi, Hiroki

1995-01-01

The rapid determination of rare earth elements (REEs) has been investigated by an on-line system of high performance liquid chromatography/multichannel inductively coupled plasma atomic emission spectrometry. In the present system, all REEs could be detected simultaneously in a single chromatographic measurement without spectral interferences. Utilizing a cation exchange column and 2-hydroxy-2-methylpropanoic acid aqueous solution as the mobile phase, the detection limits of 0.4-30 ng ml -1 for all REEs were obtained. The system was applied to the determination of REEs in geological standard rock samples and rare earth impurities in high purity rare earth oxides. The REEs in standard rocks could be determined by the present HPLC/ICP-AES system without pretreatment after acid digestion, although the detection limits were not sufficient for the analysis of rare earth oxides. (author)

Bioimaging mass spectrometry of trace elements – recent advance and applications of LA-ICP-MS: A review

Energy Technology Data Exchange (ETDEWEB)

Becker, J.Sabine, E-mail: s.becker@fz-juelich.de [Central Institute for Engineering, Electronics and Analytics (ZEA-3), Forschungszentrum Jülich, Jülich D-52425 (Germany); Matusch, Andreas, E-mail: a.matusch@fz-juelich.de [Institute for Neuroscience and Medicine (INM-2), Forschungszentrum Jülich, Jülich D-52425 (Germany); Wu, Bei, E-mail: b.wu@fz-juelich.de [Central Institute for Engineering, Electronics and Analytics (ZEA-3), Forschungszentrum Jülich, Jülich D-52425 (Germany)

2014-07-04

Highlights: • Bioimaging LA-ICP-MS is established for trace metals within biomedical specimens. • Trace metal imaging allows to study brain function and neurodegenerative diseases. • Laser microdissection ICP-MS was applied to mouse brain hippocampus and wheat root. - Abstract: Bioimaging using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) offers the capability to quantify trace elements and isotopes within tissue sections with a spatial resolution ranging about 10–100 μm. Distribution analysis adds to clarifying basic questions of biomedical research and enables bioaccumulation and bioavailability studies for ecological and toxicological risk assessment in humans, animals and plants. Major application fields of mass spectrometry imaging (MSI) and metallomics have been in brain and cancer research, animal model validation, drug development and plant science. Here we give an overview of latest achievements in methods and applications. Recent improvements in ablation systems, operation and cell design enabled progressively better spatial resolutions down to 1 μm. Meanwhile, a body of research has accumulated covering basic principles of the element architecture in animals and plants that could consistently be reproduced by several laboratories such as the distribution of Fe, Cu, Zn in rodent brain. Several studies investigated the distribution and delivery of metallo-drugs in animals. Hyper-accumulating plants and pollution indicator organisms have been the key topics in environmental science. Increasingly, larger series of samples are analyzed, may it be in the frame of comparisons between intervention and control groups, of time kinetics or of three-dimensional atlas approaches.

Application of the total reflection X-ray fluorescence method to the elemental analysis of brain tumors of different types and grades of malignancy

International Nuclear Information System (INIS)

Lankosz, M.W.; Grzelak, M.; Ostachowicz, B.; Wandzilak, A.; Szczerbowska-Boruchowska, M.; Wrobel, P.; Radwanska, E.; Adamek, D.

2014-01-01

The process of carcinogenesis may influence normal biochemical reactions leading to alterations in the elemental composition of the tissue. Total reflection X-ray fluorescence analysis (TXRF) was applied to the elemental analysis of different brain tumors. The following elements were present in all the neoplastic tissues analyzed: K, Ca, Fe, Cu, Zn and Rb. The results of the analysis showed that the elemental composition of a relatively small fragment of tissue represents satisfactorily the biochemical “signature” of a cancer. On the basis of the element concentrations determined, it was possible to differentiate between some types of brain tumors. - Highlights: • Elemental composition represents the biochemical signature of brain cancer. • The element levels differentiate some types of brain tumors. • TXRF spectrometry is a useful tool for elemental trace analysis of brain cancer

Multi-capillary column-ion mobility spectrometry: a potential screening system to differentiate virgin olive oils.

Science.gov (United States)

Garrido-Delgado, Rocío; Arce, Lourdes; Valcárcel, Miguel

2012-01-01

The potential of a headspace device coupled to multi-capillary column-ion mobility spectrometry has been studied as a screening system to differentiate virgin olive oils ("lampante," "virgin," and "extra virgin" olive oil). The last two types are virgin olive oil samples of very similar characteristics, which were very difficult to distinguish with the existing analytical method. The procedure involves the direct introduction of the virgin olive oil sample into a vial, headspace generation, and automatic injection of the volatiles into a gas chromatograph-ion mobility spectrometer. The data obtained after the analysis by duplicate of 98 samples of three different categories of virgin olive oils, were preprocessed and submitted to a detailed chemometric treatment to classify the virgin olive oil samples according to their sensory quality. The same virgin olive oil samples were also analyzed by an expert's panel to establish their category and use these data as reference values to check the potential of this new screening system. This comparison confirms the potential of the results presented here. The model was able to classify 97% of virgin olive oil samples in their corresponding group. Finally, the chemometric method was validated obtaining a percentage of prediction of 87%. These results provide promising perspectives for the use of ion mobility spectrometry to differentiate virgin olive oil samples according to their quality instead of using the classical analytical procedure.

Grammar-Based Multi-Frontal Solver for One Dimensional Isogeometric Analysis with Multiple Right-Hand-Sides

KAUST Repository

Kuźnik, Krzysztof

2013-06-01

This paper introduces a grammar-based model for developing a multi-thread multi-frontal parallel direct solver for one- dimensional isogeometric finite element method. The model includes the integration of B-splines for construction of the element local matrices and the multi-frontal solver algorithm. The integration and the solver algorithm are partitioned into basic indivisible tasks, namely the grammar productions, that can be executed squentially. The partial order of execution of the basic tasks is analyzed to provide the scheduling for the execution of the concurrent integration and multi-frontal solver algo- rithm. This graph grammar analysis allows for optimal concurrent execution of all tasks. The model has been implemented and tested on NVIDIA CUDA GPU, delivering logarithmic execution time for linear, quadratic, cubic and higher order B-splines. Thus, the CUDA implementation delivers the optimal performance predicted by our graph grammar analysis. We utilize the solver for multiple right hand sides related to the solution of non-stationary or inverse problems.

An analysis of the electromagnetic field in multi-polar linear induction system

International Nuclear Information System (INIS)

Chervenkova, Todorka; Chervenkov, Atanas

2002-01-01

In this paper a new method for determination of the electromagnetic field vectors in a multi-polar linear induction system (LIS) is described. The analysis of the electromagnetic field has been done by four dimensional electromagnetic potentials in conjunction with theory of the magnetic loops . The electromagnetic field vectors are determined in the Minkovski's space as elements of the Maxwell's tensor. The results obtained are compared with those got from the analysis made by the finite elements method (FEM).With the method represented in this paper one can determine the electromagnetic field vectors in the multi-polar linear induction system using four-dimensional potential. A priority of this method is the obtaining of analytical results for the electromagnetic field vectors. These results are also valid for linear media. The dependencies are valid also at high speeds of movement. The results of the investigated linear induction system are comparable to those got by the finite elements method. The investigations may be continued in the determination of other characteristics such as drag force, levitation force, etc. The method proposed in this paper for an analysis of linear induction system can be used for optimization calculations. (Author)

Determination of trace elements in freshwater rotifers and ciliates by total reflection X-ray fluorescence spectrometry

Science.gov (United States)

Woelfl, S.; Óvári, M.; Nimptsch, J.; Neu, T. R.; Mages, M.

2016-02-01

Element determination in plankton is important for the assessment of metal contamination of aquatic environments. Until recently, it has been difficult to determine elemental content in rotifers or ciliates derived from natural plankton samples because of the difficulty in handling and separation of these fragile organisms. The aim of this study was to evaluate methods for separation of rotifers and large ciliates from natural plankton samples (μg range dry weight) and subsequent analysis of their elemental content using total-reflection X-ray fluorescence spectrometry (TXRF). Plankton samples were collected from different aquatic environments (three lakes, one river) in Chile, Argentina and Hungary. From one to eighty specimens of five rotifer species (Brachionus calyciflorus, Brachionus falcatus, Asplanchna sieboldii, Asplanchna sp., Philodina sp.) and four to twelve specimens of one large ciliate (Stentor amethystinus) were prepared according to the dry method originally developed for microcrustaceans, and analysed by TRXF following in situ microdigestion. Our results demonstrated that it possible to process these small and fragile organisms (individual dry mass: 0.17-9.39 μg ind- 1) via careful washing and preparation procedures. We found species-dependent differences of the element mass fractions for some of the elements studied (Cr, Mn, Fe, Ni, Cu, Zn, As, Pb), especially for Cu, Fe and Mn. One large rotifer species (A. sieboldii) also showed a negative correlation between individual dry weight and the element content for Pb, Ni and Cr. We conclude that our application of the in situ microdigestion-TRXF method is suitable even for rotifers and ciliates, greatly expanding the possibilities for use of plankton in biomonitoring of metal contamination in aquatic environments.

Determination of trace elements in fisheries samples by instrumental neutron and photon activation analysis

International Nuclear Information System (INIS)

Chattopadhyay, A.; Ellis, K.M.; Nimalasiri Desilva, K.

1979-01-01

An instrumental neutron activation analysis (INAA) method has been developed for the simultaneous determination of trace concentrations of up to 23 elements in fisheries samples. The INAA method consists of irradiations of wet and lyophilized cod muscle and liver samples for three different periods at a flux density of 5x10 11 n.cm -2 .s -1 and subsequent measurements after four different decay periods using high-resolution Ge(Li) gamma-ray spectrometry. Concentrations of several essential and toxic elements have been determined. Loss of certain elements during lyophilization has been studied. Elemental distribution in muscles and livers as a function of the age of fish has been investigated. Precision and accuracy of the INAA method have been evaluated by analysing replicate samples, National Bureau of Standards' bovine liver standard reference material, and an intercalibration fish flour sample provided by the International Council for the Exploration of the Sea. A few fish samples have also been analysed by an alternative method, namely instrumental photon activation analysis (IPAA). Elemental concentrations determined by both INAA and IPAA methods are reported here. (author)

ED-XRF spectrometry-based trace element composition of genetically engineered rhizoclones vis-a-vis natural roots of a multi-medicinal plant, butterfly pea (Clitoria ternatea L.)

International Nuclear Information System (INIS)

Swain, S.S.; Chand, P.K.

2012-01-01

The energy dispersive X-ray fluorescence set-up incorporating a molybdenum secondary exciter was used for quantitative determination of major and minor elements in genetically transformed root somaclones (rhizoclones) of butterfly pea (Clitoria ternatea L.) which had been established via explant co-cultivation with Agrobacterium rhizogenes. The multi-elemental composition of these transformed rhizoclones was compared with that of the naturally grown in vivo donor plant. Trace elements namely Cr, Mn, Fe, Co, Ni, Cu, Zn, Se, Rb, Sr and Pb in addition to two macro-elements K and Ca were identified and quantified in root tissues of both sources. The elemental content of transformed root cultures was found to be at par with that of the natural roots of in vivo grown plants of the same species. These findings are implicated on the context of utilization of such Agrobacterium-mediated genetically transformed root cultures as a viable alternative to natural roots, the former being a fast-proliferating renewable resource of medicinally useful minerals essential for designing of effective drugs, besides providing an ex situ means for plant conservation. (author)

Determination of Heavy Metals in Meat, Intestine, Liver, Eggs, and Chicken Using Neutron Activation Analysis and Atomic Absorption Spectrometry

Energy Technology Data Exchange (ETDEWEB)

Surtipanti, S; Suwirma, S; Yumiarti, S; Mellawati, Yune [National Atomic Energy Agency, Jakarta (Indonesia), Center for the Application of Isotopes Radiation

1995-01-01

The elements As, Cd, Co, Cr, Fe, Hg, Ni, Pb, Sb, se and Zn in meat, intestine, and liver of cow and goat, as well as in broiler, local breed chicken and eggs have been determined using Neutron Activation Analysis and Atomic Absorption Spectrometry. Mercury was determined after being separated radiochemically. The results showed that concentration of the essential elements studied i.e. Cr, Cu, Fe, Zn, Co, and Ni were higher in liver and intestine than in the meat, but still in the normal range, while toxic elements As, Cd, and Pb were undetectable in all samples. (author). 8 refs., 6 tabs.

Determination of Heavy Metals in Meat, Intestine, Liver, Eggs, and Chicken Using Neutron Activation Analysis and Atomic Absorption Spectrometry

International Nuclear Information System (INIS)

Surtipanti, S.; Suwirma, S.; Yumiarti, S.; Mellawati, Yune

1995-01-01

The elements As, Cd, Co, Cr, Fe, Hg, Ni, Pb, Sb, se and Zn in meat, intestine, and liver of cow and goat, as well as in broiler, local breed chicken and eggs have been determined using Neutron Activation Analysis and Atomic Absorption Spectrometry. Mercury was determined after being separated radiochemically. The results showed that concentration of the essential elements studied i.e. Cr, Cu, Fe, Zn, Co, and Ni were higher in liver and intestine than in the meat, but still in the normal range, while toxic elements As, Cd, and Pb were undetectable in all samples. (author). 8 refs., 6 tabs

Indigenous instrumentation for mass spectrometry. PD-5-1

International Nuclear Information System (INIS)

Handu, V.K.

2007-01-01

Mass Spectrometry is a powerful analytical technique due to its high sensitivity, specificity, selectivity, and wide field of applications in elemental analysis, especially in the determination of trace and ultra trace elements, precise and accurate isotopic ratio measurements. Due to these excellent features, it is a crucial analytical tool for number of Department of Atomic Energy's (DAE) programs. BARC, over the years, has developed several mass spectrometers suitable for needs of a number of programs in DAE and, in this process, technologies have been developed in HV/UHV systems, precision mechanical engineering and fabrication, design and fabrication of electromagnets, ion optics, ultra stable analog and digital electronics, data systems etc. A large number of these mass spectrometers are being used regularly in various units of DAE. Since users are demanding TIMS mass spectrometer with better specifications, efforts are being made in house to develop TIMS with improved specifications. Efforts are also under way to develop a multi collector, plasma source mass spectrometer (MC-ICP-MS) with magnetic sector mass analyzer, since such instrument is increasingly being used to measure isotopic ratios with high precision

Studies on absorption coefficient near edge of multi elements

International Nuclear Information System (INIS)

Eisa, M.H.; Shen, H.; Yao, H.Y.; Mi, Y.; Zhou, Z.Y.; Hu, T.D.; Xie, Y.N.

2005-01-01

X-ray absorption near edge structure (XANES) was used to study the near edge mass-absorption coefficients of seven elements, such as, Ti, V, Fe, Co, Ni, Cu and Zn. It is well known that, on the near edge absorption of element, when incident X-ray a few eV change can make the absorption coefficient an order magnitude alteration. So that, there are only a few points mass-absorption coefficient at the near edge absorption and that always average value in published table. Our results showed a wide range of data, the total measured data of mass-absorption coefficient of the seven elements was about 505. The investigation confirmed that XANES is useful technique for multi-element absorption coefficient measurement. Details of experimental methods and results are given and discussed. The experimental work has been performed at Beijing Synchrotron Radiation Facility. The measured values were compared with the published data. Good agreement between experimental results and published data is obtained

Studies on absorption coefficient near edge of multi elements

Science.gov (United States)

Eisa, M. H.; Shen, H.; Yao, H. Y.; Mi, Y.; Zhou, Z. Y.; Hu, T. D.; Xie, Y. N.

2005-12-01

X-ray absorption near edge structure (XANES) was used to study the near edge mass-absorption coefficients of seven elements, such as, Ti, V, Fe, Co, Ni, Cu and Zn. It is well known that, on the near edge absorption of element, when incident X-ray a few eV change can make the absorption coefficient an order magnitude alteration. So that, there are only a few points mass-absorption coefficient at the near edge absorption and that always average value in published table. Our results showed a wide range of data, the total measured data of mass-absorption coefficient of the seven elements was about 505. The investigation confirmed that XANES is useful technique for multi-element absorption coefficient measurement. Details of experimental methods and results are given and discussed. The experimental work has been performed at Beijing Synchrotron Radiation Facility. The measured values were compared with the published data. Good agreement between experimental results and published data is obtained.

Analysis and synthesis of multi-qubit, multi-mode quantum devices

Energy Technology Data Exchange (ETDEWEB)

Solgun, Firat

2015-03-27

In this thesis we propose new methods in multi-qubit multi-mode circuit quantum electrodynamics (circuit-QED) architectures. First we describe a direct parity measurement method for three qubits, which can be realized in 2D circuit-QED with a possible extension to four qubits in a 3D circuit-QED setup for the implementation of the surface code. In Chapter 3 we show how to derive Hamiltonians and compute relaxation rates of the multi-mode superconducting microwave circuits consisting of single Josephson junctions using an exact impedance synthesis technique (the Brune synthesis) and applying previous formalisms for lumped element circuit quantization. In the rest of the thesis we extend our method to multi-junction (multi-qubit) multi-mode circuits through the use of state-space descriptions which allows us to quantize any multiport microwave superconducting circuit with a reciprocal lossy impedance response.

Elemental analysis of Oum er Rbia Moroccan river-water using TXRF

International Nuclear Information System (INIS)

Zahry, F.; Bounakhla, M.; El Hamdaoui, A.; Labraimi, M.

2000-01-01

The x-ray fluorescence analysis of water and suspended particulate matter (SPM) from Oum er Rbia Moroccan river for the content of 17 elements has been performed utilizing the energy dispersive x-ray fluorescence spectrometer and total reflection excitation. SPM samples were dissolved in nitric acid. For all samples direct measurements are feasible by spiking a few ml of the sample with Ga as internal standard element, and drying an aliquot of 20 μl on a quartz glass carrier. The detection limits of 10 to 20 ppb are sufficient for most of the elements to be determined. Results were assessed for accuracy by the analysis of the 15474 ICP multi-elemental standard I. Some results were also compared with AAS and ICP-AES. The results for most of the elements obtained by TXRF were accurate to about 2-15 %. The objectives of the analysis were to determine the geo-chemical areas on this river, to explain the mechanism of sediment transport and to assess the pollution of the river by human activities. 36 samples had been collected along the river between its source in Middle Atlas and the Atlantic ocean at Azemour city. (author)

Determination of geographic provenance of cotton fibres using multi-isotope profiles and multivariate statistical analysis

Science.gov (United States)

Daeid, N. Nic; Meier-Augenstein, W.; Kemp, H. F.

2012-04-01

The analysis of cotton fibres can be particularly challenging within a forensic science context where discrimination of one fibre from another is of importance. Normally cotton fibre analysis examines the morphological structure of the recovered material and compares this with that of a known fibre from a particular source of interest. However, the conventional microscopic and chemical analysis of fibres and any associated dyes is generally unsuccessful because of the similar morphology of the fibres. Analysis of the dyes which may have been applied to the cotton fibre can also be undertaken though this can be difficult and unproductive in terms of discriminating one fibre from another. In the study presented here we have explored the potential for Isotope Ratio Mass Spectrometry (IRMS) to be utilised as an additional tool for cotton fibre analysis in an attempt to reveal further discriminatory information. This work has concentrated on un-dyed cotton fibres of known origin in order to expose the potential of the analytical technique. We report the results of a pilot study aimed at testing the hypothesis that multi-element stable isotope analysis of cotton fibres in conjunction with multivariate statistical analysis of the resulting isotopic abundance data using well established chemometric techniques permits sample provenancing based on the determination of where the cotton was grown and as such will facilitate sample discrimination. To date there is no recorded literature of this type of application of IRMS to cotton samples, which may be of forensic science relevance.

Multi-isotope imaging mass spectrometry quantifies stem cell division and metabolism.

Science.gov (United States)

Steinhauser, Matthew L; Bailey, Andrew P; Senyo, Samuel E; Guillermier, Christelle; Perlstein, Todd S; Gould, Alex P; Lee, Richard T; Lechene, Claude P

2012-01-15

Mass spectrometry with stable isotope labels has been seminal in discovering the dynamic state of living matter, but is limited to bulk tissues or cells. We developed multi-isotope imaging mass spectrometry (MIMS) that allowed us to view and measure stable isotope incorporation with submicrometre resolution. Here we apply MIMS to diverse organisms, including Drosophila, mice and humans. We test the 'immortal strand hypothesis', which predicts that during asymmetric stem cell division chromosomes containing older template DNA are segregated to the daughter destined to remain a stem cell, thus insuring lifetime genetic stability. After labelling mice with (15)N-thymidine from gestation until post-natal week 8, we find no (15)N label retention by dividing small intestinal crypt cells after a four-week chase. In adult mice administered (15)N-thymidine pulse-chase, we find that proliferating crypt cells dilute the (15)N label, consistent with random strand segregation. We demonstrate the broad utility of MIMS with proof-of-principle studies of lipid turnover in Drosophila and translation to the human haematopoietic system. These studies show that MIMS provides high-resolution quantification of stable isotope labels that cannot be obtained using other techniques and that is broadly applicable to biological and medical research.

Feasibility of X-ray analysis of multi-layer thin films at a single beam voltage

International Nuclear Information System (INIS)

Statham, P J

2010-01-01

Multi-layer analysis using electron beam excitation and X-ray spectrometry is a powerful tool for characterising layers down to 1 nm thickness and with typically 1 μm lateral resolution but does not always work. Most published applications have used WDS with many measurements at different beam voltages and considerable experience has been needed to choose lines and voltages particularly for complex multi-layer problems. A new objective mathematical approach is described which demonstrates whether X-ray analysis can obtain reliable results for an arbitrary multi-layer problem. A new algorithm embodied in 'ThinFilmID' software produces a single plot that shows feasibility of achieving results with a single EDS spectrum and suggests the optimal beam voltage. Synthesis of EDS spectra allows the precision in results to be estimated and acquisition conditions modified before wasting valuable instrument time. Thus, practicality of multi-layer thin film analysis at a single beam voltage can now be established without the extensive experimentation that was previously required by a microanalysis expert. Examples are shown where the algorithm discovers viable single-voltage conditions for applications that experts previously thought could only be addressed using measurements at more than one beam voltage.

The application of energy-dispersive x-ray fluorescence spectrometry (EDXRF) to the analysis of cosmetic evidence in Indian nail polishes

International Nuclear Information System (INIS)

Misra, G.; Sawhney, K.J.S.; Lodha, G.S.; Mittal, V.K.; Sahota, H.S.

1992-01-01

The application of energy-dispersive x-ray fluorescence (EDXRF) spectrometry in the quantitative analysis of samples of Indian nail polishes of apparently similar shades from different manufacturers has been examined by evaluating the possibility of detecting spurious material which is marketed under the guise of a popular brand. On the basis of the number of elements detected, and from the ratios of particular elements [Fe/Ti,Fe/Cu,Ti/Cu] the results are very encouraging. (author)

The application of energy-dispersive x-ray fluorescence spectrometry (EDXRF) to the analysis of cosmetic evidence in Indian nail polishes

Energy Technology Data Exchange (ETDEWEB)

Misra, G. (Forensic Science Lab., Chandigarh (India)); Sawhney, K.J.S.; Lodha, G.S. (Nuclear Research Lab., Srinagar (India)); Mittal, V.K.; Sahota, H.S. (Punjabi Univ., Patiala (India). Dept. of Physics)

1992-05-01

The application of energy-dispersive x-ray fluorescence (EDXRF) spectrometry in the quantitative analysis of samples of Indian nail polishes of apparently similar shades from different manufacturers has been examined by evaluating the possibility of detecting spurious material which is marketed under the guise of a popular brand. On the basis of the number of elements detected, and from the ratios of particular elements (Fe/Ti,Fe/Cu,Ti/Cu) the results are very encouraging. (author).

Finite element method for radiation heat transfer in multi-dimensional graded index medium

International Nuclear Information System (INIS)

Liu, L.H.; Zhang, L.; Tan, H.P.

2006-01-01

In graded index medium, ray goes along a curved path determined by Fermat principle, and curved ray-tracing is very difficult and complex. To avoid the complicated and time-consuming computation of curved ray trajectories, a finite element method based on discrete ordinate equation is developed to solve the radiative transfer problem in a multi-dimensional semitransparent graded index medium. Two particular test problems of radiative transfer are taken as examples to verify this finite element method. The predicted dimensionless net radiative heat fluxes are determined by the proposed method and compared with the results obtained by finite volume method. The results show that the finite element method presented in this paper has a good accuracy in solving the multi-dimensional radiative transfer problem in semitransparent graded index medium

Quantification of 2D elemental distribution maps of intermediate-thick biological sections by low energy synchrotron μ-X-ray fluorescence spectrometry

Science.gov (United States)

Kump, P.; Vogel-Mikuš, K.

2018-05-01

Two fundamental-parameter (FP) based models for quantification of 2D elemental distribution maps of intermediate-thick biological samples by synchrotron low energy μ-X-ray fluorescence spectrometry (SR-μ-XRF) are presented and applied to the elemental analysis in experiments with monochromatic focused photon beam excitation at two low energy X-ray fluorescence beamlines—TwinMic, Elettra Sincrotrone Trieste, Italy, and ID21, ESRF, Grenoble, France. The models assume intermediate-thick biological samples composed of measured elements, the sources of the measurable spectral lines, and by the residual matrix, which affects the measured intensities through absorption. In the first model a fixed residual matrix of the sample is assumed, while in the second model the residual matrix is obtained by the iteration refinement of elemental concentrations and an adjusted residual matrix. The absorption of the incident focused beam in the biological sample at each scanned pixel position, determined from the output of a photodiode or a CCD camera, is applied as a control in the iteration procedure of quantification.

[Analysis of X-Ray Fluorescence Spectroscopy and Plasma Mass Spectrometry of Pangxidong Composite Granitoid Pluton and Its Implications for Magmatic Differentiation].

Science.gov (United States)

Zeng, Chang-yu; Ding, Ru-xin; Li, Hong-zhong; Zhou, Yong-zhang; Niu, Jia; Zhang, Jie-tang

2015-11-01

Pangxidong composite granitoid pluton located in the southwestern margin of Yunkai massif. The metamorphic grade of this pluton increases from outside to inside, that is, banded-augen granitic gneisses, gneissoid granites and granites distribute in order from edge to core. X-Ray Fluorescence Spectroscopy and Plasma Mass Spectrometry are conducted to study the geochemical characteristics of the three types of rocks. The result shows that all the three types of rocks are peraluminous rocks and their contents of main elements and rare earth elements change gradually. From granitic gneisses to granites, the contents of Al₂O₃, CaO, MgO, TiO₂, total rare earth elements and light rare earth elements increase, but the contents of SiO₂ and heavy rare earth elements decrease. It is suggested that the phylogenetic relationship exists between granitic gneisses, gneissoid granites and granites during the multi-stage tectonic evolution process. Furthermore, the remelting of metamorphosed supracrustal rocks in Yunkai massif is probably an important cause of granitoid rocks forming. The evolutionary mechanism is probably that SiO₂ and heavy rare earth elements were melt out from the protolith and gradually enriched upward, but Al₂O₃, CaO, MgO, TiO₂ and light rare earth elements enriched downward.

Elemental Analysis of Galium incanum SM subsp Centrale Ehrend ...

African Journals Online (AJOL)

. centrale Ehrend. Methods: The air-dried aerial parts of the plant material were used and its water extract (2 % w/v infusion) was analysed for trace elements using x-ray fluorescence (XRF ) spectrometry. Results: The aqueous extract depicted ...

Mass spectrometry in clinical chemistry

International Nuclear Information System (INIS)

Pettersen, J.E.

1977-01-01

A brief description is given of the functional elements of a mass spectrometer and of some currently employed mass spectrometric techniques, such as combined gas chromatography-mass spectrometry, mass chromatography, and selected ion monitoring. Various areas of application of mass spectrometry in clinical chemistry are discussed, such as inborn errors of metabolism and other metabolic disorders, intoxications, quantitative determinations of drugs, hormones, gases, and trace elements, and the use of isotope dilution mass spectrometry as a definitive method for the establishment of true values for concentrations of various compounds in reference sera. It is concluded that mass spectrometry is of great value in clinical chemistry. (Auth.)

Elemental Composition Analysis to Investigate NOx Effects on Secondary Organic Aerosol from α-Pinene Using Ultrahigh Resolution Mass Spectrometry

Science.gov (United States)

Lim, H. J.; Park, J. H.; Babar, Z.

2015-12-01

Secondary organic aerosol (SOA) accounts for 20-70% of atmospheric fine aerosol. NOx plays crucial roles in SOA formation and consequently affects the composition and yield of SOA. SOA component speciation is incomplete due to its complex composition of polar oxygenated and multifunctional species. In this study, ultrahigh resolution mass spectrometry (UHR MS) was applied to improve the understanding of NOx effects on biogenic SOA formation by identifying the elemental composition of SOA. Additional research aim was to investigate oligomer components that are considered as a driving force for SOA formation and growth. In this study α-pinene SOA from photochemical reaction was examined. SOA formation was performed in the absence and presence of NOx at dry condition (grant funded by the Korea government (MEST) (No. 2011-01350000).

ED-XRF spectrometric analysis of comparative elemental composition of in vivo and in vitro roots of Andrographis paniculata (Burm.f.) Wall. ex Nees-a multi-medicinal herb

Energy Technology Data Exchange (ETDEWEB)

Behera, P.R., E-mail: priyaranjan2004@gmail.co [Plant Cell and Tissue culture Facility, Post-Graduate Department of Botany, Utkal University, Vani Vihar, Bhubaneswar 751004, Orissa (India); Plant Biotechnology Lab, Institute of Minerals and Materials Technology (CSIR), Bhubaneswar 751013, Orissa (India); Nayak, P [Plant Cell and Tissue culture Facility, Post-Graduate Department of Botany, Utkal University, Vani Vihar, Bhubaneswar 751004, Orissa (India); Plant Biotechnology Lab, Institute of Minerals and Materials Technology (CSIR), Bhubaneswar 751013, Orissa (India); Barik, D.P., E-mail: barikdp@yahoo.co [Plant Cell and Tissue culture Facility, Post-Graduate Department of Botany, Utkal University, Vani Vihar, Bhubaneswar 751004, Orissa (India); Rautray, T.R., E-mail: trrautray@gmail.co [Ion Beam Laboratory, Institute of Physics, Bhubaneswar 751013, Orissa (India); Thirunavoukkarasu, M [Plant Biotechnology Lab, Institute of Minerals and Materials Technology (CSIR), Bhubaneswar 751013, Orissa (India); Chand, P.K., E-mail: pkchanduubot@yahoo.co.i [Plant Cell and Tissue culture Facility, Post-Graduate Department of Botany, Utkal University, Vani Vihar, Bhubaneswar 751004, Orissa (India)

2010-12-15

The multi-elemental composition of in vitro-proliferated root tissues of Andrographis paniculata (Burm.f.) Wall. ex Nees was compared with that of the naturally grown in vivo plants. Trace elements namely Cr, Mn, Fe, Co, Ni, Cu, Zn, Se, Rb, Sr and Pb in addition to two macro-elements K and Ca were identified and quantified in root tissues of both sources using the energy dispersive X-ray fluorescence (ED-XRF) technique. ED-XRF analysis was performed using Mo K X-rays generated from a secondary molybdenum target. The elemental content of in vitro roots was found to be at par with that of naturally grown plants of the same species. This opens up a possibility of exploiting in vitro root cultures as a viable, alternative and renewable source of phytochemicals of relevance, besides providing a means for conservation of the valuable natural resources.

ED-XRF spectrometric analysis of comparative elemental composition of in vivo and in vitro roots of Andrographis paniculata (Burm.f.) Wall. ex Nees-a multi-medicinal herb

International Nuclear Information System (INIS)

Behera, P.R.; Nayak, P.; Barik, D.P.; Rautray, T.R.; Thirunavoukkarasu, M.; Chand, P.K.

2010-01-01

The multi-elemental composition of in vitro-proliferated root tissues of Andrographis paniculata (Burm.f.) Wall. ex Nees was compared with that of the naturally grown in vivo plants. Trace elements namely Cr, Mn, Fe, Co, Ni, Cu, Zn, Se, Rb, Sr and Pb in addition to two macro-elements K and Ca were identified and quantified in root tissues of both sources using the energy dispersive X-ray fluorescence (ED-XRF) technique. ED-XRF analysis was performed using Mo K X-rays generated from a secondary molybdenum target. The elemental content of in vitro roots was found to be at par with that of naturally grown plants of the same species. This opens up a possibility of exploiting in vitro root cultures as a viable, alternative and renewable source of phytochemicals of relevance, besides providing a means for conservation of the valuable natural resources.

Chemical analysis of refractories by plasma spectrometry

International Nuclear Information System (INIS)

Coutinho, C.A.

1990-01-01

X-ray spectrometry has been, since the last two or three decades, the traditional procedure for the chemical analysis of refractories, due to its high degree of accuracy and speed to produce analytical results. An interesting alternative to X-ray fluorescence is provided by the Inductively Coupled Plasma Spectrometry technique, for those laboratories where wet chemistry facilities are already available or process control is not required at high speed, or investiment costs have to be low. This paper presents results obtained by plasma spectroscopy for the analysis of silico - aluminous refractories, showing calibration curves, precion and detection limits. Considerations and comparisons with X-ray fluorescence are also made. (author) [pt

An x ray scatter approach for non-destructive chemical analysis of low atomic numbered elements