WorldWideScience

Sample records for spectrometry ii determination

  1. Separation/preconcentration of trace Pb(II and Cd(II with 2-mercaptobenzothiazole impregnated Amberlite XAD-1180 resin and their determination by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Şerife Tokalıoğlu

    2017-01-01

    Full Text Available A new chelating resin, 2-mercaptobenzothiazole loaded Amberlite XAD-1180 was prepared and used for separation and preconcentration of Cd(II and Pb(II ions prior to their determinations by flame atomic absorption spectrometry. The optimum pH for simultaneous retention of the elements and the best elution means for their simultaneous elution were 9.5 and 2 mol L−1 HNO3, respectively. The detection limits for Cd(II and Pb(II were 0.35 and 5.0 μg L−1, respectively. The accuracy of the method was confırmed both by analyzing the certified reference material (RM 8704 Buffalo river sediment and performing recovery studies.

  2. Determination of lead in water by electrothermal atomic absorption spectrometry with a nickel(II)-ammonium tartrate modifier

    International Nuclear Information System (INIS)

    Sekerka, I.; Lechner, J.F.

    1991-01-01

    A method is described for the determination of low concentrations of lead in water samples. Atomic absorption spectrometry is used with a tungsten ribbon furnace and Zeeman background correction. Interferences are eliminated by the addition of ammonium tartrate and nickel(II) nitrate to the samples to act as a matrix modifier and adjust the pH. The results show the superior performance of this modifier over other types used conventionally. The detection limit is 1 μg l -1 relative standard deviation of -1 can be obtained. The instrumentation is simple and the method is efficient for the determination of lead in various water samples. 25 refs.; 7 figs.; 6 tabs

  3. X-Ray Fluorescence Spectrometry. II. Determination of Uranium in ores

    International Nuclear Information System (INIS)

    Bermudez Polonio, J.; Crus Castillo, F. de la; Fernandez Cellini, R.

    1961-01-01

    A method of analysis of uranium in ores by X-ray spectrometry was developed, using the internal standard technique. Strontium was found to be the most suitable internal standard for general use. A Norelco Philips X-ray fluorescent spectrometer was used in this work, equipped with a lithium fluoride crystal acting as a diffraction grating analyzer. The intensity of the uranium-L α 1 spectral line is calculated and related to corresponding strontium-K α spectral line, both detected with a Scintillation Counter. (Author) 31 refs

  4. A solid phase extraction procedure for the determination of Cd(II) and Pb(II) ions in food and water samples by flame atomic absorption spectrometry.

    Science.gov (United States)

    Daşbaşı, Teslima; Saçmacı, Şerife; Ülgen, Ahmet; Kartal, Şenol

    2015-05-01

    A relatively rapid, accurate and precise solid phase extraction method is presented for the determination of cadmium(II) and lead(II) in various food and water samples. Quantitation is carried out by flame atomic absorption spectrometry (FAAS). The method is based on the retention of the trace metal ions on Dowex Marathon C, a strong acid cation exchange resin. Some important parameters affecting the analytical performance of the method such as pH, flow rate and volume of the sample solution; type, concentration, volume, flow rate of the eluent; and matrix effects on the retention of the metal ions were investigated. Common coexisting ions did not interfere on the separation and determination of the analytes. The detection limits (3 σb) for Cd(II) and Pb(II) were found as 0.13 and 0.18 μg L(-1), respectively, while the limit of quantification values (10 σb) were computed as 0.43 and 0.60 μg L(-1) for the same sequence of the analytes. The precision (as relative standard deviation was lower than 4% at 5 μg L(-1) Cd(II) and 10 μg L(-1) Pb(II) levels, and the preconcentration factor was found to be 250. The accuracy of the proposed procedure was verified by analysing the certified reference materials, SPS-WW2 Batch 108 wastewater level 2 and INCT-TL-1 tea leaves, with the satisfactory results. In addition, for the accuracy of the method the recovery studies (⩾ 95%) were carried out. The method was applied to the determination of the analytes in the various natural waters (lake water, tap water, waste water with boric acid, waste water with H2SO4) and food samples (pomegranate flower, organic pear, radish leaf, lamb meat, etc.), and good results were obtained. While the food samples almost do not contain cadmium, they have included lead at low levels of 0.13-1.12 μg g(-1). Copyright © 2014 Elsevier Ltd. All rights reserved.

  5. Determination of cadmium(II), cobalt(II), nickel(II), lead(II), zinc(II), and copper(II) in water samples using dual-cloud point extraction and inductively coupled plasma emission spectrometry.

    Science.gov (United States)

    Zhao, Lingling; Zhong, Shuxian; Fang, Keming; Qian, Zhaosheng; Chen, Jianrong

    2012-11-15

    A dual-cloud point extraction (d-CPE) procedure has been developed for simultaneous pre-concentration and separation of heavy metal ions (Cd2+, Co2+, Ni2+, Pb2+, Zn2+, and Cu2+ ion) in water samples by inductively coupled plasma optical emission spectrometry (ICP-OES). The procedure is based on forming complexes of metal ion with 8-hydroxyquinoline (8-HQ) into the as-formed Triton X-114 surfactant rich phase. Instead of direct injection or analysis, the surfactant rich phase containing the complexes was treated by nitric acid, and the detected ions were back extracted again into aqueous phase at the second cloud point extraction stage, and finally determined by ICP-OES. Under the optimum conditions (pH=7.0, Triton X-114=0.05% (w/v), 8-HQ=2.0×10(-4) mol L(-1), HNO3=0.8 mol L(-1)), the detection limits for Cd2+, Co2+, Ni2+, Pb2+, Zn2+, and Cu2+ ions were 0.01, 0.04, 0.01, 0.34, 0.05, and 0.04 μg L(-1), respectively. Relative standard deviation (RSD) values for 10 replicates at 100 μg L(-1) were lower than 6.0%. The proposed method could be successfully applied to the determination of Cd2+, Co2+, Ni2+, Pb2+, Zn2+, and Cu2+ ion in water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  6. Preconcentration, Separation and Determination of lead(II) with Methyl Thymol Blue Adsorbed on Activated Carbon Using Flame Atomic Absorption Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ensafi, Ali A.; Ghaderi, Ali R. [Isfahan University of Technology, Isfahan (Iran, Islamic Republic of)

    2008-02-15

    An on-line system for preconcentration and separation of lead(II) is presented. The method is based on the complex formation of Pb(II) with adsorbed Methyl thymol blue on activated carbon. The conditions of preparing the solid phase reagent and of quantitative recovery of Pb(II) from diluted solutions, such as acidity of aqueous phase, solid phase capacity, and flow variables were studied as well as effect of potential interfering ions. After preconcentration step, the metal ions are eluted automatically by 5 ml of 0.5 M HNO{sub 3} solution and the lead ions content was determined by flame atomic absorption spectrometry. Under the optimum conditions, the lead ions in aqueous samples were separated and preconcentrated about 1000-fold by the column. The detection limit was 0.001 μg mL{sup -1}. Lead has been determined in river and tap water samples, with recovery of 98 to 102%.

  7. Determination of cadmium(II), cobalt(II), nickel(II), lead(II), zinc(II), and copper(II) in water samples using dual-cloud point extraction and inductively coupled plasma emission spectrometry

    International Nuclear Information System (INIS)

    Zhao, Lingling; Zhong, Shuxian; Fang, Keming; Qian, Zhaosheng; Chen, Jianrong

    2012-01-01

    Highlights: ► A dual-cloud point extraction (d-CPE) procedure was firstly developed for simultaneous pre-concentration and separation of trace metal ions combining with ICP-OES. ► The developed d-CPE can significantly eliminate the surfactant of Triton X-114 and successfully extend to the determination of water samples with good performance. ► The designed method is simple, high efficient, low cost, and in accordance with the green chemistry concept. - Abstract: A dual-cloud point extraction (d-CPE) procedure has been developed for simultaneous pre-concentration and separation of heavy metal ions (Cd 2+ , Co 2+ , Ni 2+ , Pb 2+ , Zn 2+ , and Cu 2+ ion) in water samples by inductively coupled plasma optical emission spectrometry (ICP-OES). The procedure is based on forming complexes of metal ion with 8-hydroxyquinoline (8-HQ) into the as-formed Triton X-114 surfactant rich phase. Instead of direct injection or analysis, the surfactant rich phase containing the complexes was treated by nitric acid, and the detected ions were back extracted again into aqueous phase at the second cloud point extraction stage, and finally determined by ICP-OES. Under the optimum conditions (pH = 7.0, Triton X-114 = 0.05% (w/v), 8-HQ = 2.0 × 10 −4 mol L −1 , HNO 3 = 0.8 mol L −1 ), the detection limits for Cd 2+ , Co 2+ , Ni 2+ , Pb 2+ , Zn 2+ , and Cu 2+ ions were 0.01, 0.04, 0.01, 0.34, 0.05, and 0.04 μg L −1 , respectively. Relative standard deviation (RSD) values for 10 replicates at 100 μg L −1 were lower than 6.0%. The proposed method could be successfully applied to the determination of Cd 2+ , Co 2+ , Ni 2+ , Pb 2+ , Zn 2+ , and Cu 2+ ion in water samples.

  8. Determination of cadmium(II), cobalt(II), nickel(II), lead(II), zinc(II), and copper(II) in water samples using dual-cloud point extraction and inductively coupled plasma emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Lingling; Zhong, Shuxian; Fang, Keming; Qian, Zhaosheng [College of Chemistry and Life Sciences, Zhejiang Normal University, Jinhua 321004 (China); Chen, Jianrong, E-mail: cjr@zjnu.cn [College of Chemistry and Life Sciences, Zhejiang Normal University, Jinhua 321004 (China); College of Geography and Environmental Sciences, Zhejiang Normal University, Jinhua 321004 (China)

    2012-11-15

    Highlights: Black-Right-Pointing-Pointer A dual-cloud point extraction (d-CPE) procedure was firstly developed for simultaneous pre-concentration and separation of trace metal ions combining with ICP-OES. Black-Right-Pointing-Pointer The developed d-CPE can significantly eliminate the surfactant of Triton X-114 and successfully extend to the determination of water samples with good performance. Black-Right-Pointing-Pointer The designed method is simple, high efficient, low cost, and in accordance with the green chemistry concept. - Abstract: A dual-cloud point extraction (d-CPE) procedure has been developed for simultaneous pre-concentration and separation of heavy metal ions (Cd{sup 2+}, Co{sup 2+}, Ni{sup 2+}, Pb{sup 2+}, Zn{sup 2+}, and Cu{sup 2+} ion) in water samples by inductively coupled plasma optical emission spectrometry (ICP-OES). The procedure is based on forming complexes of metal ion with 8-hydroxyquinoline (8-HQ) into the as-formed Triton X-114 surfactant rich phase. Instead of direct injection or analysis, the surfactant rich phase containing the complexes was treated by nitric acid, and the detected ions were back extracted again into aqueous phase at the second cloud point extraction stage, and finally determined by ICP-OES. Under the optimum conditions (pH = 7.0, Triton X-114 = 0.05% (w/v), 8-HQ = 2.0 Multiplication-Sign 10{sup -4} mol L{sup -1}, HNO{sub 3} = 0.8 mol L{sup -1}), the detection limits for Cd{sup 2+}, Co{sup 2+}, Ni{sup 2+}, Pb{sup 2+}, Zn{sup 2+}, and Cu{sup 2+} ions were 0.01, 0.04, 0.01, 0.34, 0.05, and 0.04 {mu}g L{sup -1}, respectively. Relative standard deviation (RSD) values for 10 replicates at 100 {mu}g L{sup -1} were lower than 6.0%. The proposed method could be successfully applied to the determination of Cd{sup 2+}, Co{sup 2+}, Ni{sup 2+}, Pb{sup 2+}, Zn{sup 2+}, and Cu{sup 2+} ion in water samples.

  9. A dispersive liquid--liquid microextraction methodology for copper (II) in environmental samples prior to determination using microsample injection flame atomic absorption spectrometry.

    Science.gov (United States)

    Alothman, Zeid A; Habila, Mohamed; Yilmaz, Erkan; Soylak, Mustafa

    2013-01-01

    A simple, environmentally friendly, and efficient dispersive liquid-liquid microextraction method combined with microsample injection flame atomic absorption spectrometry was developed for the separation and preconcentration of Cu(II). 2-(5-Bromo-2-pyridylazo)-5-(diethylamino)phenol (5-Br-PADAP) was used to form a hydrophobic complex of Cu(II) ions in the aqueous phase before extraction. To extract the Cu(II)-5-Br-PADAP complex from the aqueous phase to the organic phase, 2.0 mL of acetone as a disperser solvent and 200 microL of chloroform as an extraction solvent were used. The influences of important analytical parameters, such as the pH, types and volumes of the extraction and disperser solvents, amount of chelating agent, sample volume, and matrix effects, on the microextraction procedure were evaluated and optimized. Using the optimal conditions, the LOD, LOQ, preconcentration factor, and RSD were determined to be 1.4 microg/L, 4.7 microg/L, 120, and 6.5%, respectively. The accuracy of the proposed method was investigated using standard addition/recovery tests. The analysis of certified reference materials produced satisfactory analytical results. The developed method was applied for the determination of Cu in real samples.

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

    Directory of Open Access Journals (Sweden)

    Saeed Mohammad Sorouraddin

    2017-12-01

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

  11. Determination of Hg(II) in waters by on-line preconcentration using Cyanex 923 as a sorbent - Cold vapor atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Duan Taicheng; Song Xuejie; Xu Jingwei; Guo Pengran; Chen Hangting; Li Hongfei

    2006-01-01

    Using a solid phase extraction mini-column home-made from a neutral extractant Cyanex 923, inorganic Hg could be on-line preconcentrated and simultaneously separated from methyl mercury. The preconcentrated Hg (II) was then eluted with 10% HNO 3 and subsequently reduced by NaBH 4 to form Hg vapor before determination by cold vapor atomic absorption spectrometry (CVAAS). Optimal conditions for and interferences on the Hg preconcentration and measurement were at 1% HCl, for a 25 mL sample uptake volume and a 10 mL min -1 sample loading rate. The detection limit was 0.2 ng L -1 and much lower than that of conventional method (around 15.8 ng L -1 ). The relative standard deviation (RSD) is 1.8% for measurements of 40 ng L -1 of Hg and the linear working curve is from 20 to 2000 ng L -1 (with a correlation coefficient of 0.9996). The method was applied in determination of inorganic Hg in city lake and deep well water (from Changchun, Jilin, China), and recovery test results for both samples were satisfactory

  12. X-Ray Fluorescence Spectrometry. II Determination of Uranium in ores; Espectrometria de fluorescencia de Rayos X. II-Aplicacion a la determinacion de uranio en minerales

    Energy Technology Data Exchange (ETDEWEB)

    Bermudez Polonio, J; Crus Castillo, F. de la; Fernandez Cellini, R

    1961-07-01

    A method of analysis of uranium in ores by X-ray spectrometry was developed, using the internal standard technique. Strontium was found to be the most suitable internal standard for general use. A Norelco Philips X-ray fluorescent spectrometer was used in this work, equipped with a lithium fluoride crystal acting as a diffraction grating analyzer. The intensity of the uranium-L {alpha}{sub 1} spectral line is calculated and related to corresponding strontium-K{sub {alpha}} spectral line, both detected with a Scintillation Counter. (Author) 31 refs.

  13. Determination of telmisartan in human blood plasma: Part II: Liquid chromatography-tandem mass spectrometry method development, comparison to immunoassay and pharmacokinetic study

    NARCIS (Netherlands)

    Hempen, C.M.; Gläsle-Schwarz, Liane; Kunz, Ulrich; Karst, U.

    2006-01-01

    A new liquid chromatography/atmospheric pressure chemical ionization-tandem mass spectrometry (LC/APCI-MS/MS) method with on-line sample clean-up for the determination of telmisartan in human blood plasma is presented. This technique is compared to a previously introduced enzyme-linked immunosorbent

  14. Emulsification based dispersive liquid microextraction prior to flame atomic absorption spectrometry for the sensitive determination of Cd(II) in water samples

    International Nuclear Information System (INIS)

    Rahimi-Nasrabadi, Mehdi; Banan, Alireza; Zahedi, Mir Mahdi; Pourmortazavi, Seied Mahdi; Nazari, Zakieh; Asghari, Alireza

    2013-01-01

    We report on the application of emulsification-based dispersive liquid micro extraction (EB-DLME) to the preconcentration of Cd(II). This procedure not only possesses all the advantages of routine DLLME, but also results in a more stable cloudy state which is particularly useful when coupling it to FAAS. In EB-DLME, appropriate amounts of the extraction solvent (a solution of dithizone in chloroform) and an aqueous solution of sodium dodecyl sulfate (SDS; acting as a disperser) are injected into the samples. A stable cloudy microemulsion is formed and Cd(II) ion is extracted by chelation. After phase separation, the sedimented phase is subjected to FAAS. Under optimized conditions, the calibration curve for Cd(II) is linear in the range from 0.1 to 25 μg L −1 , the limit of detection (at S/N = 3) is 30 pg L −1 , the relative standard deviations for seven replicate analyses (at 0.56 μg L −1 of Cd(II)) is 4.6 %, and the enrichment factor is 151. EB-DLME in our opinion is a simple, efficient and rapid method for the preconcentration of Cd(II) (and most likely of many other ions) prior to FAAS determination. (author)

  15. On-line separation and preconcentration of lead(II) by solid-phase extraction using activated carbon loaded with xylenol orange and its determination by flame atomic absorption spectrometry.

    Science.gov (United States)

    Ensafi, Ali A; Shiraz, A Zendegi

    2008-02-11

    Activated carbon loaded with xylenol orange in a mini-column was used for the highly selective separation and preconcentration of Pb(II) ions. An on-line system for enrichment and the determination of Pb(II) was carried out on flame atomic absorption spectrometry. The conditions of preconcentration and quantitative recovery of Pb(II) from diluted solution, such as pH of aqueous phase, amount of the sorbent, volume of the solutions and flow variables were studied as well as effect of potential interfering ions. Under the optimum conditions, Pb(II) in an aqueous sample was concentrated about 200-fold and the detection limit was 0.4 ng mL(-1) Pb(II). The adsorption capacity of the solid phase was 0.20mg of lead per one gram of the modified activated carbon. The modified activated carbon is stable for several treatments of sample solutions without the need for using any chemical reagent. The recovery of lead(II) from river water, waste water, tap water, and in the following reference materials: SRM 2711 Montana soil and GBW-07605 tea were obtained in the range of 97-104% by the proposed method.

  16. On-line separation and preconcentration of lead(II) by solid-phase extraction using activated carbon loaded with xylenol orange and its determination by flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Ensafi, Ali A.; Shiraz, A. Zendegi

    2008-01-01

    Activated carbon loaded with xylenol orange in a mini-column was used for the highly selective separation and preconcentration of Pb(II) ions. An on-line system for enrichment and the determination of Pb(II) was carried out on flame atomic absorption spectrometry. The conditions of preconcentration and quantitative recovery of Pb(II) from diluted solution, such as pH of aqueous phase, amount of the sorbent, volume of the solutions and flow variables were studied as well as effect of potential interfering ions. Under the optimum conditions, Pb(II) in an aqueous sample was concentrated about 200-fold and the detection limit was 0.4 ng mL -1 Pb(II). The adsorption capacity of the solid phase was 0.20 mg of lead per one gram of the modified activated carbon. The modified activated carbon is stable for several treatments of sample solutions without the need for using any chemical reagent. The recovery of lead(II) from river water, waste water, tap water, and in the following reference materials: SRM 2711 Montana soil and GBW-07605 tea were obtained in the range of 97-104% by the proposed method

  17. On-line separation and preconcentration of lead(II) by solid-phase extraction using activated carbon loaded with xylenol orange and its determination by flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ensafi, Ali A. [College of Chemistry, Isfahan University of Technology, Isfahan 84156-83111 (Iran, Islamic Republic of)], E-mail: Ensafi@cc.iut.ac.ir; Shiraz, A. Zendegi [College of Chemistry, Isfahan University of Technology, Isfahan 84156-83111 (Iran, Islamic Republic of)

    2008-02-11

    Activated carbon loaded with xylenol orange in a mini-column was used for the highly selective separation and preconcentration of Pb(II) ions. An on-line system for enrichment and the determination of Pb(II) was carried out on flame atomic absorption spectrometry. The conditions of preconcentration and quantitative recovery of Pb(II) from diluted solution, such as pH of aqueous phase, amount of the sorbent, volume of the solutions and flow variables were studied as well as effect of potential interfering ions. Under the optimum conditions, Pb(II) in an aqueous sample was concentrated about 200-fold and the detection limit was 0.4 ng mL{sup -1} Pb(II). The adsorption capacity of the solid phase was 0.20 mg of lead per one gram of the modified activated carbon. The modified activated carbon is stable for several treatments of sample solutions without the need for using any chemical reagent. The recovery of lead(II) from river water, waste water, tap water, and in the following reference materials: SRM 2711 Montana soil and GBW-07605 tea were obtained in the range of 97-104% by the proposed method.

  18. Determination of selected quaternary ammonium compounds by liquid chromatography with mass spectrometry. Part II. Application to sediment and sludge samples in Austria

    International Nuclear Information System (INIS)

    Martinez-Carballo, Elena; Gonzalez-Barreiro, Carmen; Sitka, Andrea; Kreuzinger, Norbert; Scharf, Sigrid; Gans, Oliver

    2007-01-01

    Soxhlet extraction and high-performance liquid chromatography (HPLC) coupled to tandem mass spectrometry detection (MS/MS) was used for the determination of selected quaternary ammonium compounds (QACs) in solid samples. The method was applied for the determination of alkyl benzyl, dialkyl and trialkyl quaternary ammonium compounds in sediment and sludge samples in Austria. The overall method quantification limits range from 0.6 to 3 μg/kg for sediments and from 2 to 5 μg/kg for sewage sludges. Mean recoveries between 67% and 95% are achieved. In general sediments were especially contaminated by C12 chain benzalkonium chloride (BAC-C12) as well as by the long C-chain dialkyldimethylammonium chloride (DDAC-C18) with a maximum concentration of 3.6 mg/kg and 2.1 mg/kg, respectively. Maxima of 27 mg/kg for DDAC-C10, 25 mg/kg for BAC-C12 and 23 mg/kg for BAC-C14 were determined for sludge samples. The sums of the 12 selected target compounds range from 22 mg/kg to 103 mg/kg in the sludge samples. - The presence of quaternary ammonium surfactants in sediment and sludge samples is reported for the first time in Austria

  19. Development and validation of a liquid chromatography tandem mass spectrometry method for the determination of cannabinoids and phase I and II metabolites in meconium.

    Science.gov (United States)

    Prego-Meleiro, Pablo; Lendoiro, Elena; Concheiro, Marta; Cruz, Angelines; López-Rivadulla, Manuel; de Castro, Ana

    2017-05-12

    A liquid chromatography-tandem mass spectrometry (LC-MSMS) method was developed and fully validated for the determination of Δ 9 -tetrahydrocannabinol (THC), 11-hydroxyTHC (OHTHC), 11-nor-9-carboxyTHC (THCCOOH), 8-β-11-dihydroxyTHC (diOHTHC), cannabinol, cannabidiol, and THC and THCCOOH glucuronides in 0.25±0.02g meconium. Samples were homogenized in methanol and subjected to cation exchange solid-phase extraction. Chromatographic separation was performed on a Kinetex C18 column (50 mm×2.1mm, 2.6μm) at 35°C, with a gradient of 0.1% formic acid in water and acetonitrile at a flow rate of 0.3 mL/min; total run time was 10min. Two transitions per analyte were monitored in MRM mode. The method was specific and sensitive; LOD was from 1 to 2ng/g, and LOQ from 4 to 10ng/g; linearity ranged from 4 to 400 ng/g for all the analytes, except for THC glucuronide (10-400ng/g); intra-assay, inter-assay and total imprecision were <11.2%, <13.45% and <15.6%, respectively; accuracy ranged from 93.9% to 109.0% of the target concentration; matrix effect, extraction and process efficiency ranged from -26.4% to -71.4%, 49.9% to 69.5% and 14.3% to 45.0%, respectively. The inclusion of THC and THCCOOH glucuronides avoided the need for the hydrolysis process, thus facilitating sample pretreatment. Application of the method to 19 authentic meconium specimens from uncontrolled pregnancies or women suspicious of drug consumption revealed fetal cannabis exposure in 4 newborns. THCCOOH (24.1-288.8ng/g), diOHTHC (53.2-332.4ng/g), THC (4.2-7.7ng/g), CBN (30.7-93.3ng/g) and CBD (7.1-251.5ng/g) were detected in all cases; THCCOOH glucuronide (190.2-306.8ng/g) in 3 cases; and OHTHC (11.9ng/g) in the remaining one; however, THC glucuronide was not identified in any specimen. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Burnup determination of mass spectrometry for nuclear fuels

    International Nuclear Information System (INIS)

    Zhang Chunhua.

    1987-01-01

    The various methods currently being used in burnup determination of nuclear fuels are studied and reviewed. The mass spectrometry method of destructive testing is discussed emphatically. The burnup determination of mass spectrometry includes heavy isotopic abundance ratio method and isotope dilution mass spectrometry used as burnup indicator for the fission products. The former is applied to high burnup level, but the later to various burnup level. According to experiences, some problems which should be noticed in burnup determination of mass spectrometry are presented

  1. Direct extraction of lead (II) from untreated human blood serum using restricted access carbon nanotubes and its determination by atomic absorption spectrometry.

    Science.gov (United States)

    Barbosa, Valéria Maria Pereira; Barbosa, Adriano Francisco; Bettini, Jefferson; Luccas, Pedro Orival; Figueiredo, Eduardo Costa

    2016-01-15

    Oxidized carbon nanotubes were covered with layers of bovine serum albumin to result in so-called restricted-access carbon nanotubes (RACNTs). This material can extract Pb(2+) ions directly from untreated human blood serum while excluding all the serum proteins. The RACNTs have a protein exclusion capacity of almost 100% and a maximum Pb(2+) adsorption capacity of 34.5mg g(-1). High resolution transmission electron microscopy, scanning transmission electron microscopy and energy dispersive spectroscopy were used to confirm the BSA layer and Pb(2+) adsorption sites. A mini-column filled with RACNTs was used in an on-line solid phase extraction system coupled to a thermospray flame furnace atomic absorption spectrometry. At optimized experimental conditions, the method has a detection limit as low as 2.1µg L(-1), an enrichment factor of 5.5, and inter- and intra-day precisions (expressed as relative standard deviation) of <8.1%. Recoveries of the Pb(2+) spiked samples ranged from 89.4% to 107.3% for the extraction from untreated human blood serum. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. Evaluation of a novel PTFE material for use as a means for separation and preconcentration of trace levels of metal ions in sequential injection (SI) and sequential injection lab-on-valve (SI-LOV) systems. Determination of cadmium (II) with detection by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Long, Xiangbao; Chomchoei, Roongrat; Hansen, Elo Harald

    2004-01-01

    with an external packed column and in a sequential injection lab-on-valve (SI-LOV) system. Employed for the determination of cadmium(II), complexed with diethyldithiophosphate (DDPA), and detection by electrothermal atomic absorption spectrometry (ETAAS), its performance was compared to that of a previously used...

  3. Comprehensive determination of flavouring additives and nicotine in e-cigarette refill solutions. Part II: Gas-chromatography-mass spectrometry analysis.

    Science.gov (United States)

    Aszyk, Justyna; Woźniak, Mateusz Kacper; Kubica, Paweł; Kot-Wasik, Agata; Namieśnik, Jacek; Wasik, Andrzej

    2017-09-29

    Flavouring compounds are an essential part of e-liquid products for cigarettes. In general, they are regarded as safe for ingestion, but they may have unrecognized risks when they are inhaled. In some cases, manufactures do not currently abide by the Tobacco Products Directive (2014/40/EU) and do not declare the detailed contents of e-liquids on their labels. To help evaluate the health impact of flavouring substances, there is a need for comprehensive approaches to determine their concentrations in e-liquids. For this purpose, a GC-EI-MS method was developed and validated for the simultaneous determination of 46 commonly used flavour additives in e-liquids. The proposed method performed well in terms of the key validation parameters: accuracy (84-113%), inter-/intra-day precision: 0.1-10% and 1-11%, respectively, and sensitivity (limit of detection: 3-87ng/mL). The sample preparation step was based on a simple "dilute & shoot" approach. This study is a complementary method to the LC-MS/MS procedure described in Part I. Both approaches are suitable for the comprehensive determination of 88 flavouring compounds and nicotine and can be used as tools for the rapid evaluation of the quality and safety of e-cigarette products. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Determination of plutonium-238 in plutonium by alpha spectrometry

    International Nuclear Information System (INIS)

    Aggarwal, S.K.; Jain, H.C.; Mathews, C.K.; Ramaniah, M.V.

    1975-01-01

    A method is presented for the determination of 238 Pu in plutonium samples by alpha spectrometry. Various factors attributing towards the energy degradation, a problem usually encountered in alpha spectrometry, are discussed. A computer programme is given for the evaluation of peak areas when the alpha spectrum is degraded. The results are compared with those obtained by mass spectrometry. (author)

  5. 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)

  6. Architecture of the RNA polymerase II-TFIIF complex revealed by cross-linking and mass spectrometry

    DEFF Research Database (Denmark)

    Chen, Zhuo Angel; Jawhari, Anass; Fischer, Lutz

    2010-01-01

    Higher-order multi-protein complexes such as RNA polymerase II (Pol II) complexes with transcription initiation factors are often not amenable to X-ray structure determination. Here, we show that protein cross-linking coupled to mass spectrometry (MS) has now sufficiently advanced as a tool to ex...

  7. Radioimmunologic determination of plasmapepsinogen II

    International Nuclear Information System (INIS)

    Patzschke, C.; Berg, U.

    1979-01-01

    Within the frame of this study the pepsinogen II concentration could be determined for the first time with a radioimmunoassay in the plasma. In our normal study group the mean value was 13.91 ng/ml with a variation between 4.08 and 36.19 ng/ml. With increasing patient age a continuous increase of this concentration could be observed. The mean value of 14.99 ng/ml for male patients was by 4.75 ng/ml higher than the mean value of 10.24 ng/ml for female patients. The 24 hour profiles represented for the pepsinogen plasma concentration daily physiologic fluctuations and a stabilisation at night. The effects of meals could not be defined unambiguously. In stimulation tests Pentagastrin provoked in 4 of 9 test persons an increase of the concentration of up to 70% of the basic value. In short-term stress-tests the Pg II concentrations found in the test subjects presented an increase or a decrease. In investigations before or after the same patient underwent an operative procedure, an expressive Pg II decrease (up to 33.74 ng/ml) could be detected. Patients with a total resection of the stomach had only a very low Pg II concentration (less than 3.1 ng/ml). In patients with gastric pathologies a significant difference of the confidence limits was found for the Pg II concentration between superficial gastritis (m = 16.04 ng/ml) and atrophic gastritis (m = 27.38 ng/ml). Compared with various gastric diseases the normal patient group presents a significant difference with reference to the atrophic gastritis or the cancerous stomach. The mean values found in atrophic gastritis or the cancerous stomach. The mean values found in atrophic gastritis and in gastric carcinoma are close to each other and are increased, compared to those measured in the normal patient group. (orig./MG) [de

  8. Identification of phase-II metabolites of flavonoids by liquid chromatography-ion-mobility spectrometry-mass spectrometry.

    Science.gov (United States)

    Chalet, Clément; Hollebrands, Boudewijn; Janssen, Hans-Gerd; Augustijns, Patrick; Duchateau, Guus

    2018-01-01

    Flavonoids are a class of natural compounds with a broad range of potentially beneficial health properties. They are subjected to an extensive intestinal phase-II metabolism, i.e., conjugation to glucuronic acid, sulfate, and methyl groups. Flavonoids and their metabolites can interact with drug transporters and thus interfere with drug absorption, causing food-drug interactions. The site of metabolism plays a key role in the activity, but the identification of the various metabolites remains a challenge. Here, we developed an analytical method to identify the phase-II metabolites of structurally similar flavonoids. We used liquid chromatography-ion-mobility spectrometry-mass spectrometry (LC-IMS-MS) analysis to identify phase-II metabolites of flavonols, flavones, and catechins produced by HT29 cells. We showed that IMS could bring valuable structural information on the different positional isomers of the flavonols and flavones. The position of the glucuronide moiety had a strong influence on the collision cross section (CCS) of the metabolites, with only minor contribution of hydroxyl and methyl moieties. For the catechins, fragmentation data obtained from MS/MS analysis appeared more useful than IMS to determine the structure of the metabolites, mostly due to the high number of metabolites formed. Nevertheless, CCS information as a molecular fingerprint proved to be useful to identify peaks from complex mixtures. LC-IMS-MS thus appears as a valuable tool for the identification of phase-II metabolites of flavonoids. Graphical abstract Structural identification of phase-II metabolites of flavonoids using LC-IMS-MS.

  9. Simultaneous determination of seven flavonoids in Epimedium by liquid chromatography-tandem mass spectrometry method

    Institute of Scientific and Technical Information of China (English)

    Cai Sheng Wu; Bao Lin Guo; Yu Xin Sheng; Jin Lan Zhang

    2008-01-01

    In this paper, a sensitive and specific liquid chromatography-electrospray ionisation-mass spectrometry (LC-ESI-MS) method has been developed and validated for the identification and determination of seven flavonoids, namely epimedin A, epimedin B, epimedin C, icariin, sagittatoside B, 2"-0-rhamnosyl icariside II, and baohuoside I in Epimedium from different sources.

  10. Development of an in situ solvent formation microextraction and preconcentration method based on ionic liquids for the determination of trace cobalt (II in water samples by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Mohammad Reza Jamali

    2017-02-01

    Full Text Available A simple in situ solvent formation microextraction (ISFME methodology based on the application of ionic liquid (IL as an extractant solvent and sodium hexafluorophosphate (NaPF6 as an ion-pairing agent was proposed for the preconcentration of the trace levels of cobalt ions. In this method cobalt was complexed with 2-(5-bromo-2-pyridylazo-5-diethylaminophenol (5-Br-PADAP and extracted into an ionic liquid phase. After phase separation, the enriched analyte in the final solution is determined by flame atomic absorption spectrometry (FAAS. Some effective factors that influence the microextraction efficiency were investigated and optimized. Under the optimum experimental conditions, the limit of detection and the enrichment factor were 0.97 μg L−1 and 50, respectively. The relative standard deviation (R.S.D. was obtained as 2.4%. The proposed method was assessed through the analysis of certified reference water and recovery experiments.

  11. Determination of plutonium isotopes in bilberry using liquid scintillation spectrometry and alpha-particle spectrometry

    International Nuclear Information System (INIS)

    Seferinoğlu, Meryem; Aslan, Nazife; Kurt, Aylin; Erden, Pınar Esra; Mert, Hülya

    2014-01-01

    This paper presents α-particle spectrometry and liquid scintillation spectrometry methods to determine plutonium isotopes in bilberry. The analytical procedure involves sample preparation steps for ashing, digestion of bilberry samples, radiochemical separation of plutonium radioisotopes and their measurement. The validity of the method was checked for coherence using the ζ test, z-test, relative bias and relative uncertainty outlier tests. The results indicated that the recommended procedures for both measurement systems could be successfully applied for the accurate determination of plutonium activities in bilberry samples. - Highlights: • Sample preparation methods for Pu using LSS and alpha spectrometry developed. • Complete separation of plutonium from interfering radionuclides. • Commercial bilberry was spiked with NPL 2011 (AH-B11144) proficiency test sample. • Results were checked using ζ test, z-test, rel. bias and rel. uncert. outlier tests. • Recommended procedures successfully applied to bilberry samples

  12. Determination of uranium in seawater by fluorescence spectrometry

    International Nuclear Information System (INIS)

    Kawashima, Toshi; Kawakubo, Senkichi; Minegishi, Hisako.

    1984-01-01

    A Fluorescence spectrometry for the determination of uranium in seawater has been developed. Anion exchange separation of uranium from seawater followed by preparation of NaF-carbonate cake and by spectrometry for ultraviolet ray excited fluorescence of uranium on the fluoride host provide the trace determinaton of uranium at the subnano gram level. Anion exchange behavior, excitation-emission behavior of the uranium on the host and effects of foreign ions to the fluorescence have been presented. Appling the method to 1 ml of seawater 3 ppb of uranium has been determined. (author)

  13. Determination of hafnium by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Yoshida, Isao; Kobayashi, Hiroshi; Ueno, Keihei.

    1977-01-01

    Optimum conditions for atomic absorption spectrophotometric determination of hafnium were investigated by use of a Jarrel-Ash AA-1 instrument which was equipped with a premixed gas burner slotted 50 mm in length and 0.4 mm in width. Absorption of hafnium, which was atomized in an nitrous oxide-acetylene flame, was measured on a resonance line at 307.29 nm. The absorption due to hafnium was enhanced in the presence of ammonium fluoride and iron(III) ion, as shown in Figs. 2 and 3, depending on their concentration. The highest absorption was attained by the addition of (0.15 -- 0.3)M ammonium fluoride, 0.07 M of iron(III) ion and 0.05 M of hydrochloric acid. An excess of the additives decreased the absorption. The presence of zirconium, which caused a significant interference in the ordinary analytical methods, did not affect the absorption due to hafnium, if the zirconium concentration is less than 0.2 M. A standard procedure was proposed; A sample containing a few mg of hafnium was dissolved in a 25-ml volumetric flask, and ammonium fluoride, ferric nitrate and hydrochloric acid were added so that the final concentrations were 0.3, 0.07 and 0.05 M, respectively. Atomic absorption was measured on the aqueous solution in a nitrous oxide-acetylene flame and the hafnium content was calculated from the absorbance. Sensitivity was as high as 12.5 μg of Hf/ml/l% absorption. The present method is especially recommendable to the direct determination of hafnium in samples containing zirconium. (auth.)

  14. 226Ra determination in phosphogypsum by alpha-particle spectrometry

    International Nuclear Information System (INIS)

    Aguado, J.L.; Bolivar, J.P.; Garcia-Tenorio, R.

    1999-01-01

    A radiochemical method for 226 Ra determination by alpha-particle spectrometry in environmental samples has been developed in our laboratory. The method has been validated by measurements in samples with known concentrations of this radionuclide and it has been applied in studies related to 226 Ra behaviour in phosphogypsum (the main by-product of producing phosphoric acid from phosphate rocks). (author)

  15. Determination of 226Ra by alpha spectrometry of liquid scintillation

    International Nuclear Information System (INIS)

    Nobrega, A.W.; Sachett, I.A.; Hespanhol, E.C.B.

    1987-01-01

    The determination of 226 Ra in environmental samples using alpha spectrometry in liquid scintilation is studied. The Radon 1-2 emanation method and 226 Ra separation process of other radionuclides alpha emissors are analyzed. The use of 226 Ra coprecipitation with barium sulphate is evaluated. (M.J.C.) [pt

  16. Determination of uranium-235 by differential gamma spectrometry

    International Nuclear Information System (INIS)

    Suner, A.A.; La Gamma de Batistoni, A.M.G.; Botbol, J.

    1974-12-01

    A method for the determination of U-235 contained in solutions of uranium, by gamma spectrometry with Ge(Li) detector is described. Ra-226 is coprecipitated in BaSO 4 . The activity at 186 keV is measured, substracted by the corresponding of a standard. The detection limit is 1% of increment of U-235 over the standard. (author)

  17. Solid Phase Extraction of Trace Al(III), Fe(II), Co(II), Cu(II), Cd(II) and Pb(II) Ions in Beverages on Functionalized Polymer Microspheres Prior to Flame Atomic Absorption Spectrometric Determinations.

    Science.gov (United States)

    Berber, Hale; Alpdogan, Güzin

    2017-01-01

    In this study, poly(glycidyl methacrylate-methyl methacrylate-divinylbenzene) was synthesized in the form of microspheres, and then functionalized by 2-aminobenzothiazole ligand. The sorption properties of these functionalized microspheres were investigated for separation, preconcentration and determination of Al(III), Fe(II), Co(II), Cu(II), Cd(II) and Pb(II) ions using flame atomic absorption spectrometry. The optimum pH values for quantitative sorption were 2 - 4, 5 - 8, 6 - 8, 4 - 6, 2 - 6 and 2 - 3 for Al(III), Fe(II), Co(II), Cu(II), Cd(II) and Pb(II), respectively, and also the highest sorption capacity of the functionalized microspheres was found to be for Cu(II) with the value of 1.87 mmol g -1 . The detection limits (3σ; N = 6) obtained for the studied metals in the optimal conditions were observed in the range of 0.26 - 2.20 μg L -1 . The proposed method was successfully applied to different beverage samples for the determination of Al(III), Fe(II), Co(II), Cu(II), Cd(II) and Pb(II) ions, with the relative standard deviation of <3.7%.

  18. Myofiber metabolic type determination by mass spectrometry imaging

    OpenAIRE

    Théron, Laetitia; Vénien, Annie; Pujos-Guillot, Estelle; Astruc, Thierry; Chambon, Christophe

    2017-01-01

    In muscle imaging, myofiber type determination is of great importance to better understand biological mechanisms related to skeletal muscle changes associated with pathologies. However, reference methods (histo-enzymology and immunohistochemistry) require serial-cross sections, and several days from the sampling to the results of image analysis. In this work, a strategy based on MALDI-Mass Spectrometry Imaging was developed as an alternative to the classical methods for myofiber metabolic typ...

  19. Determination of cadmium in aluminium by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Batistoni, D.A.; Erlijman, L.H.

    1978-12-01

    A direct method for the determination of cadmium in elemental aluminium is described. Metal samples are dissolved in diluted hydrochloric acid and cadmium is determined by atomic absorption spectrometry in an air-acetylene flame. Interference by non-specific absorption observed at the analytical wavelength incorrected for by means of a non-absorbing line emitted by the hollow-cathode lamp. Relatively large amounts of arsenic do not interfere. The minimun determinable concentration of cadmium for this procedure is 2-3 ppm, expressed on aluminium basis. (author) [es

  20. Simultaneous determination of U and Pu isotopes by alpha spectrometry

    International Nuclear Information System (INIS)

    Equillor, H.E.; Campos, J.M.

    2011-01-01

    Determination of actinides by alpha spectrometry is usually carried out after full separation of each of the components of the sample. The procedure presented in this paper permits U and Pu isotopes to be measured together allowing faster sample processing and measurement. The method consists in the extraction with tributyl phosphate of U and Pu isotopes from the rest of the matrix, followed by a cathodic electrodeposition to obtain alpha spectrometry suitable pieces. It can be applied to various environmental samples, such as water, filters and soil (about 0.5 g of solid sample for the described conditions). High-quality electroplated discs are essential for simultaneous processing, so a technique to achieve this requirement is also explained. (authors) [es

  1. The determination and use of radionuclide background in gamma spectrometry

    International Nuclear Information System (INIS)

    Zimmer, W.H.

    1986-01-01

    Background is the major component of gross photon peak area. Therefore, net area, nuclide activity, counting uncertainty, and limits of detection calculations are no better than the calculation of background. In this study, background in gamma spectrometry is explored in several of its aspects. Means are presented to reduce background. Standard practices are presented to be used in the acquisition of valid, relevant background data. Unified standard calculations with examples are presented in the use of background data to determine net count and counting uncertainty. L. A. Currie's latest calculations of Lower Limits of Detection (1) (LLD) as they apply to gamma spectrometry are reviewed. Finally, Maximum Undetected Activity (MUA), LLD, and Critical Level (CL) concepts and calculations are compared in sample spectra

  2. Isotope determination of sulfur by mass spectrometry in soil samples

    Directory of Open Access Journals (Sweden)

    Alexssandra Luiza Rodrigues Molina Rossete

    2012-12-01

    Full Text Available Sulphur plays an essential role in plants and is one of the main nutrients in several metabolic processes. It has four stable isotopes (32S, 33S, 34S, and 36S with a natural abundance of 95.00, 0.76, 4.22, and 0.014 in atom %, respectively. A method for isotopic determination of S by isotope-ratio mass spectrometry (IRMS in soil samples is proposed. The procedure involves the oxidation of organic S to sulphate (S-SO4(2-, which was determined by dry combustion with alkaline oxidizing agents. The total S-SO4(2- concentration was determined by turbidimetry and the results showed that the conversion process was adequate. To produce gaseous SO2 gas, BaSO4 was thermally decomposed in a vacuum system at 900 ºC in the presence of NaPO3. The isotope determination of S (atom % 34S atoms was carried out by isotope ratio mass spectrometry (IRMS. In this work, the labeled material (K2(34SO4 was used to validate the method of isotopic determination of S; the results were precise and accurate, showing the viability of the proposed method.

  3. Lithium determination in whole blood by flame atomic emission spectrometry

    International Nuclear Information System (INIS)

    Rahman, S.; Khalid, N.; Nasimullah; Iqbal, M.Z.

    2003-01-01

    A simple and rapid method for the determination of lithium in whole blood using Flame atomic emission spectrometry is described. No sample preparation was required apart from dilution with 0.02 N HNO/sub 3/. The reliability of the method was determined by analyzing Standard Reference Material (SRM) under identical experimental conditions and comparing the determined lithium concentration with the reported value. These were in good agreement with each other. The determined range of lithium in the whole blood of fifty-six healthy adult volunteers (28 males and 28 females) were 13.1 - 47.8 mg L-1. The determined average concentration of lithium in whole blood was compared with the reported values of other countries. The data was statistically analyzed with respect to sex and different age groups. (author)

  4. Energy determination at BEPC-II

    International Nuclear Information System (INIS)

    Achasov, M.N.; Blinov, V.E.; Bogomyagkov, A.V.; Fu ChengDong; Harris, F.A.; Kaminsky, V.V.; Liu, Q.; Mo Xiaohu; Muchnoi, N.Yu.; Nikitin, S.A.; Nikolaev, I.B.; Qin Qing; Qu Huamin; Olsen, S.L.; Pyata, E.E.; Shamov, A.G.; Shen, C.P.; Varner, G.S.; Wang Yifang; Xu Jinqiang

    2009-01-01

    The BEPC-II collider beam energy calibration system is discussed. The system is based on the Compton backscattering method. The expected precision of the electron and positron beam energy ε determination is δε/ε∼3.10 -5 .

  5. Determination of Ra-226 by gamma-ray spectrometry

    International Nuclear Information System (INIS)

    Martinez Lobo, A.

    1988-01-01

    This work deals with the method of determination of 226 Ra by low energy photon spectrometry. For this purpose, the interference due to 235 U, that emits a photon with a close energy, has to be considered. The contribution of 235 U to the 186 KeV photopeak is studied through the 63 KeV 234 Th and the 144 KeV 235 U emissions. From the minimum detectable activity of 226 Ra it is discussed the applicability of this method to several kind of samples. (Author)

  6. Determination of metals in atmospheric particulates using atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Alduan, F.A.; Capdevila, C.

    1979-01-01

    Nineteen trace metals in atmospheric samples have been determined by atomic absorption spectrometry, using a graphite furnace for most elements. Paper filters have been used to collect air samples. The sample preparation procedure involves the removal of organic matter and the conversion of the metals to soluble salts by ashing the filters in an oxygen plasma at 125 deg C for 6 h. and by subsequent dissolution in HN0 3 HCl solution. The sensitivities achieved are in the range of 2,5.10 -5 and 6,3.10 -3 μg/m 3 , for an air volume of 2000 m 3 . (author)

  7. Determination of uranium in urine by 2-spectrometry

    International Nuclear Information System (INIS)

    Duarte, C.L.; Szeles, M.S.-M.F.

    1989-07-01

    A comparative study is presented for two technics of preparation sources for the determination of uranium isotopes by α - spectrometry: electrodeposition and chemical stripping with polymeric membrane containing trioctylphosphine oxide (TOPO). A method is described for separation of uranium from urine with an ion-exchange column Dowex 1x8 (chloride form). The mean yield obtained for electrodeposition and TOPO deposition was 74% and 8,5% respectively. The TOPO deposition presented better resolution for 238 U and 234 U than electrodeposition. The global yield of the method obtained was 50%. (author) [pt

  8. Determination of mercury in hair: Comparison between gold amalgamation-atomic absorption spectrometry and mass spectrometry.

    Science.gov (United States)

    Domanico, Francesco; Forte, Giovanni; Majorani, Costanza; Senofonte, Oreste; Petrucci, Francesco; Pezzi, Vincenzo; Alimonti, Alessandro

    2017-09-01

    Mercury is a heavy metal that causes serious health problems in exposed subjects. The most toxic form, i.e., methylmercury (MeHg), is mostly excreted through human hair. Numerous analytical methods are available for total Hg analysis in human hair, including cold vapour atomic fluorescence spectrometry (CV-AFS), inductively coupled plasma mass spectrometry (ICP-MS) and thermal decomposition amalgamation atomic absorption spectrometry (TDA-AAS). The aim of the study was to compare the TDA-AAS with the ICP-MS in the Hg quantification in human hair. After the washing procedure to minimize the external contamination, from each hair sample two aliquots were taken; the first was used for direct analysis of Hg by TDA-AAS and the second was digested for Hg determination by the ICP-MS. Results indicated that the two data sets were fully comparable (median; TDA-AAS, 475ngg -1 ; ICP-MS, 437ngg -1 ) and were not statistically different (Mann-Whitney test; p=0.44). The two techniques presented results with a good coefficient of correlation (r=0.94) despite different operative ranges and method limits. Both techniques satisfied internal performance requirements and the parameters for method validation resulting sensitive, precise and reliable. Finally, the use of the TDA-AAS can be considered instead of the ICP-MS in hair analysis in order to reduce sample manipulation with minor risk of contamination, less time consuming due to the absence of the digestion step and cheaper analyses. Copyright © 2016 Elsevier GmbH. All rights reserved.

  9. Methods of humidity determination Part II: Determination of material humidity

    OpenAIRE

    Rübner, Katrin; Balköse, Devrim; Robens, E.

    2008-01-01

    Part II covers the most common methods of measuring the humidity of solid material. State of water near solid surfaces, gravimetric measurement of material humidity, measurement of water sorption isotherms, chemical methods for determination of water content, measurement of material humidity via the gas phase, standardisation, cosmonautical observations are reviewed.

  10. Determination of iprodione in agrochemicals by infrared and Raman spectrometry.

    Science.gov (United States)

    Armenta, Sergio; Garrigues, Salvador; de la Guardia, Miguel

    2007-04-01

    Two methodologies based on vibrational spectrometry--making use of Fourier transform infrared absorption (FTIR) and Raman spectrometry--were developed for iprodione determination in solid pesticide formulations. The FTIR procedure involved the extraction of iprodione by CHCl(3), and the latter determination involved measuring the peak area between 1450 and 1440 cm(-1), corrected using a horizontal baseline defined at 1481 cm(-1). FT-Raman determination was performed directly on the powdered solid products, using standard chromatography glass vials as sample cells and measuring the Raman intensity between 1003 and 993 cm(-1), with a two-point baseline correction established between 1012 and 981 cm(-1). The sensitivities obtained were 0.319 area values g mg(-1) for FTIR determination and 5.58 area values g g(-1) for FT-Raman. The repeatabilities, taken to be the relative standard deviation of five independent measurements at 1.51 mg g(-1) and 10.98% w/w concentration levels, were equal to 0.16% and 0.9% for FTIR and FT-Raman, respectively, and the limits of detection were 0.3 and 0.2% w/w (higher than those obtained for HPLC, 0.016% w/w). FTIR determination provided a sample frequency of 60 h(-1), higher than those obtained for the Raman and reference chromatography methods (25 and 8.6 h(-1), respectively). On the other hand, the new FT-Raman method eliminates reagent consumption and waste generation, and reduces the need for sample handling and the contact of operator with the pesticide. In spite of their lack of sensitivity, vibrational procedures can therefore provide viable environmentally friendly alternatives to laborious, time- and solvent-consuming reference chromatography methods for quality control in commercially available pesticide formulations.

  11. Plutonium-236 traces determination in plutonium-238 by α spectrometry

    International Nuclear Information System (INIS)

    Acena, M.L.; Pottier, R.; Berger, R.

    1969-01-01

    Two methods are described in this report for the determination of plutonium-236 traces in plutonium-238 by a spectrometry using semi-conductor detectors. The first method involves a direct comparison of the areas under the peaks of the α spectra of plutonium-236 and plutonium-238. The electrolytic preparation of the sources is carried out after preliminary purification of the plutonium. The second method makes it possible to determine the 236 Pu/ 238 Pu ratio by comparing the areas of the α peaks of uranium-232 and uranium-234, which are the decay products of the two plutonium isotopes respectively. The uranium in the source, also deposited by electrolysis, is separated from a 1 mg amount of plutonium either by a T.L.A. extraction, or by the use of ion-exchange resins. The report ends with a discussion of the results obtained with plutonium of two different origins. (authors) [fr

  12. Determination of radium-226 by high-resolution alpha spectrometry

    International Nuclear Information System (INIS)

    Sill, C.W.

    1983-01-01

    The determination of radium-226 by alpha spectrometry has been investigated critically to determine experimental conditions under which high resolution and accurate and reliable results can be obtained. Refractory solids such as soils, ores, and tailings from uranium mills are dissolved completely by fusion with potassium fluoride in the presence of barium-133 tracer. The fluoride cake is then transposed with sulfuric acid to a pyrosulfate fusion with simultaneous volatilization of all silica and fluoride. Radium is precipitated with barium already present in the sample by addition of lead perchlorate to a dilute hydrochloric acid solution of the pyrosulfate cake. The resulting insoluble sulfates are dissolved in an alkaline solution of diethylenetriaminepentaacetic acid, and the radium and barium sulfates are reprecipitated with acetic acid. The precipitate is mounted on a membrane filter and analyzed by alpha spectrometry. Water samples are partially evaporated and treated similarly. Resolution of the subsequent alpha spectra is much better than has been achieved previously from barium sulfate, and is almost as good as is obtainable with actinides electrodeposited on polished steel plates. The resolution is about 60 keV full-width-half-maximum with 100 μg of barium on a 1-inch filter with a 450 mm 2 detector at 20% counting efficiency. Recovery is about 97% and accuracy is generally as good as the counting statistics obtained will permit. Grossly inaccurate results can be obtained under certain conditions when barium-133 tracer is used to determine the chemical yield of radium-226. Severe contamination of the surface-barrier detector by polonium-210 and by recoil products of the radium isotopes being counted is demonstrated, amd methods for virtual elimination of both problems are discussed

  13. Determination of sulphur with total reflection x-ray spectrometry

    International Nuclear Information System (INIS)

    Steinmeyer, S.; Kolbesen, B.O.

    2000-01-01

    The potential and limitations of total reflection x-ray spectrometry (TXRF) were tested for the quantitative determination of the light element sulphur in inorganic and biological samples. As representatives of inorganic samples alkali, transition metal, magnesium and aluminum sulphates were investigated. As biological samples the sulphur containing amino acid methionine and the pharmaceutical drug insulin were chosen. All measurements were performed on a TXRF-spectrometer EXTRA IIA (Atomika Instruments, Oberschleissheim/Germany) using tungsten L-radiation as the excitation tube. Various concentrations of all samples ranging from 20 mg/l to 0.5 mg/l were determined. In addition the surface topography and thickness of the dry residue of these samples were investigated with SEM and a thickness profilometer (Alpha-Step). The result show that the reliable determination of sulphur in sulphates depends on the cation involved. Alkali sulphates like Na 2 SO 4 , or K 2 SO 4 form bulky residues resulting in significant deviations of the recovery rate of sulphur. In this case the use of smoothing detergents like 1 % HF, 1 % malic acid and 2 % hydrazinhydrat was found to be necessary for accurate determination. The results for the biological samples agree well with the expected values. The investigations lead to the conclusion that TXRF combined with a proper samples preparation is well suited for the determination of sulphur in different samples with various concentrations and matrices. (author)

  14. Determination of some metal ions in various meat and baby food samples by atomic spectrometry.

    Science.gov (United States)

    Daşbaşı, Teslima; Saçmacı, Şerife; Ülgen, Ahmet; Kartal, Şenol

    2016-04-15

    In this paper, we report a simple and rapid solid phase extraction system for the separation/preconcentration and determination of Cd(II), Co(II), Cu(II), Fe(III), Cr(III), Pb(II), and Zn(II) ions by flame atomic absorption spectrometry (FAAS). This method is based upon the retention of metal ions on a column packed with poly[N-(3-methyl-1H-indole-1-yl)]-2-methacrylamide-co-2-acrylamido-2-methyl-1-propane sulphonic acid-co divinylbenzene] (MMAD) resin as a solid-phase extraction (SPE) sorbent at pH 8. At the optimized conditions, the limits of detection (3 s/b) between 0.12 and 1.6 μg L(-1), preconcentration factor of 100, and the relative standard deviation of ⩽1.8% were achieved (n=10). The accuracy of the method was verified by analyzing certified reference materials (CRMs) and performing recovery experiments. The developed method was successfully applied to the various natural water, meat products and baby food samples. The recoveries of analyte ions were found in added real samples and CRMs from 95% to 102%. Copyright © 2015 Elsevier Ltd. All rights reserved.

  15. Determination of plutonium in soils by mass spectrometry

    International Nuclear Information System (INIS)

    Storms, H.A.; Carlson, D.C.; Hunter, F.F.

    1974-01-01

    A procedure is described in which mass spectrometry is utilized for the determination of plutonium in soils. Using this procedure we have measured plutonium isotopic compositions at concentrations as low as 2 x 10 -14 grams Pu per gram soil. A thermal ionization source with canoe-shaped rhenium filament, is utilized in the mass spectrometer. The plutonium, when loaded onto the filament, is contained in a single Dowex-1 resin bead which is about 350 micrometers in diameter. Concentrating the plutonium within this single bead is a key step in the procedure and produces a relatively clean plutonium fraction. The resin bead also serves as an effective diffusion barrier such that the plutonium is prevented from being removed with the lower boiling impurities. The Pu remains in the bead until the temperature is sufficiently high for efficient production of Pu + ions. Plutonium ionization efficiencies as high as 2.5 percent have been measured

  16. Complexometric determination, Part II: Complexometric determination of Cu2+-ions

    Directory of Open Access Journals (Sweden)

    Rajković Miloš B.

    2002-01-01

    Full Text Available A copper-selective electrode of the coated wire type based on sulphidized copper wire was applied successfully for determining Cu(II ions by complexometric titration with the disodium salt of EDTA (complexon III. By the formation of internal complex compounds with the Cu(II ion, the copper concentration in the solution decreases, and all this is followed by a change of potential of the indicator system Cu-DWISE (or Cu-EDWISE/SCE. At the terminal point of titration, when all the Cu(II ions are already utilized for the formation of the complex with EDTA, there occurs a steep rise of potential, thus enabling us, through the first or second derivative to note the quantity of copper that is present in the solution. Copper-selective electrode showed a responsivity towards titration with EDTA as a complexing agent, with the absence of "fatigue" due to a great number of repeated measurings. Errors occurring during quantitative measurements were more a characteristic of the overall procedure which involve, because of the impossibility of the complete absence of subjectivity, a constant error, and the reproducibility of the results confirmed this fact. The disodium salt of EDTA appeared as a very efficient titrant in all titrations and with various concentrations ot Cu(II ions in the solution, with somewhat weaker response at lower concentrations in the solution.

  17. Determination of activities of human carbonic anhydrase II inhibitors ...

    African Journals Online (AJOL)

    Purpose: To evaluate the activities of new curcumin analogs as carbonic anhydrase II (CA-II) inhibitor. Methods: Carbonic anhydrase II (CA-II) inhibition was determined by each ligand capability to inhibit the esterase activity of CA-II using 4-NPA as a substrate in 96-well plates. Dimethyl sulfoxide was used to dissolve each ...

  18. Solid-phase extraction of copper(II) in water and food samples using silica gel modified with bis(3-aminopropyl)amine and determination by flame atomic absorption spectrometry.

    Science.gov (United States)

    Cagirdi, Duygu; Altundag, Hüseyin; Imamoglu, Mustafa; Tuzen, Mustafa

    2014-01-01

    A simple and selective separation and preconcentration method was developed for the determination of Cu(ll) ions. This method is based on adsorption of Cu(ll) ions from aqueous solution on a bis(3-aminopropyl)amine modified silica gel column and flame atomic absorption spectrometric determination after desorption. Various analytical parameters such as pH, type of eluent solution and its volume, flow rate of sample and eluent, and sample volume were optimized. Effects of some cation, anion, and transition metal ions on the recoveries of Cu(ll) ions were also investigated. Cu(ll) ions were quantitatively recovered at pH 6; 5.0 mL of 2 M HCI was used as the eluent. The preconcentration factor was found to be 150. The LOD was 0.12 microg/L for Cu(ll). The accuracy of the method was confirmed by analysis of Tea Leaves (INCT-TL-1) and Fish Protein (DORM-3) certified reference materials. The optimized method was applied to various water and food samples for the determination of Cu(ll).

  19. Determination of Ultra-Trace Amounts of Selenium(IV) by Flow Injection Hydride Generation Atomic Absorption Spectrometry with On-line Preconcentration by Co-precipitation with Lanthanium Hydroxide. Part II. On-line Addition of Coprecipating Agent

    DEFF Research Database (Denmark)

    Nielsen, Steffen; Sloth, Jens Jørgen; Hansen, Elo Harald

    1996-01-01

    -line and merged with an ammonium buffer solution of pH 9.1, which promotes precipitation and quantitative collection on the inner walls of an incorporated knotted Microline reactor. The Se(IV) preconcentrated by coprecipitation with the generated lanthanum hydroxide precipitate is subsequently eluted...... with hydrochloric acid, allowing an ensuing determination via hydride generation. At different sample flow rates, i.e., 4.8, 6.4 and 8.8 ml/min, enrichment factors of 30, 40 and 46, respectively, were obtained at a sampling frequency of 33 samples/h. The detection limit (3s) was 0.005 µg/l at a sample flow rate...

  20. Determination of radium-226 by high-resolution alpha spectrometry

    International Nuclear Information System (INIS)

    Sill, C.W.

    1983-01-01

    Condition were determined under which high resolution and accurate and reliable results can be obtained. Refractory solids are dissolved completely by fusion with KF and Ba-133 tracer. The fluoride cake is then transposed with sulfuric acid to a pyrosulfate fusion. Radium is precipitated with barium by addition of lead perchlorate to a dilute HCl solution of the pyrosulfate cake. The resulting insoluble sulfates are dissolved in an alkaline solution of DTPA and the Ra and Ba sulfates are reprecipitated with acetic acid to produce very small crystals. The precipitate is mounted on 0.1-μm membrane filter and analyzed by alpha spectrometry. Water samples are partially evaporated and treated similarly. Resolution, almost as good as with actinides electrodeposited on polished steel plates, is about 60 keV full-width-half-maximum with 100 μg of barium on a 1-inch filter with a 450 mm 2 detector at 20% counting efficiency. Recovery is about 97%. One solid sample can be prepared for counting in less than 2 hours. Methods are discussed for ensuring reliability of the results. Severe contamination of the surface-barrier detector by polonium-210 and recoil products is discussed

  1. Study on determination of 90Sr by liquid scintillation spectrometry

    International Nuclear Information System (INIS)

    Zhai Xiufang; Li Weiping; Tian Mei; Zou Ronghu

    2012-01-01

    Both of Liquid scintillation counting and Cerenkov counting can be used to determinate 90 Sr in samples by Liquid scintillation spectrometry. In this work, effects of scintillation vials wit-h different material, Liquid scintillation cocktails, sample volume, Strontium carrier, pH, quenching (chemical quenching and color quenching)are studied, and both counting methods are compared. For Liquid scintillation counting. The results show that the best appropriate volume ratio of sample and liquid scintillation cocktail is 8:12 for OPTIPHASE HISAFE-3 and OPTIPHASE HISAFE-2, stability of solution decreased when sample load exceeds the maximum load for both Liquid scintillation cocktails, and OPTIPHASE HISAFE-3 also show superior performance for high saline solution. The type of scintillation vial haven't clear influence on the MDA of 90 Sr. Chemical quenching and color quenching can decrease the counting efficiency. For Cerenkov counting, the lowest MDA is obtained when polyethylene plastic vial is used and sample volume is 20 ml. Color quenching decreases the counting efficiency, while there isn't chemical quenching for Cerenkov counting. The MDA of 90 Sr is 1.19 and 1.00 Bq/L for Liquid scintillation counting and Cerenkov counting with the optimal labeling condition. (authors)

  2. Mass spectrometry in grape and wine chemistry. Part II: The consumer protection.

    Science.gov (United States)

    Flamini, Riccardo; Panighel, Annarita

    2006-01-01

    Controls in food industry are fundamental to protect the consumer health. For products of high quality, warranty of origin and identity is required and analytical control is very important to prevent frauds. In this article, the "state of art" of mass spectrometry in enological chemistry as a consumer safety contribute is reported. Gas chromatography-mass spectrometry (GC/MS) and liquid-chromatography-mass spectrometry (LC/MS) methods have been developed to determine pesticides, ethyl carbamate, and compounds from the yeast and bacterial metabolism in wine. The presence of pesticides in wine is mainly linked to the use of dicarboxyimide fungicides on vineyard shortly before the harvest to prevent the Botrytis cinerea attack of grape. Pesticide residues are regulated at maximum residue limits in grape of low ppm levels, but significantly lower levels in wine have to be detected, and mass spectrometry offers effective and sensitive methods. Moreover, mass spectrometry represent an advantageous alternative to the radioactive-source-containing electron capture detector commonly used in GC analysis of pesticides. Analysis of ochratoxin A (OTA) in wine by LC/MS and multiple mass spectrometry (MS/MS) permits to confirm the toxin presence without the use of expensive immunoaffinity columns, or time and solvent consuming sample derivatization procedures. Inductively coupled plasma-mass spectrometry (ICP/MS) is used to control heavy metals contamination in wine, and to verify the wine origin and authenticity. Isotopic ratio-mass spectrometry (IRMS) is applied to reveal wine watering and sugar additions, and to determine the product origin and traceability.

  3. Plutonium determination in urine by techniques of mass spectrometry

    International Nuclear Information System (INIS)

    Hernandez M, H.; Yllera de Ll, A.

    2013-10-01

    The objective of this study was to develop an analytic method for quantification and plutonium reappraisal in plane tables of alpha spectrometry be means of the mass spectrometry technique of high resolution with plasma source inductively coupled and desolvator Aridus (Aridus-Hr-Icp-Ms) and mass spectrometry with accelerator (AMS). The obtained results were, the recovery percentage of Pu in the plane table was of ∼ 90% and activity minimum detectable obtained with Aridus-Hr-Icp-Ms and AMS was of ∼ 3 and ∼ 0.4 f g of 239 Pu, respectively. Conclusion, the results demonstrate the aptitude of the Aridus-Hr-Icp-Ms and AMS techniques in the Pu reappraisal in plane tables with bigger speed and precision, improving the values notably of the activity minimum detectable that can be obtained with the alpha spectrometry (∼ 50 f g of 239 Pu). (author)

  4. Methodology for determination of activity of radionuclides by gamma spectrometry

    International Nuclear Information System (INIS)

    Fragoso, Maria da Conceicao de Farias; Oliveira, Victor Rogerio S. de; Oliveira, Mercia L.; Lima, Fernando Roberto de Andrade

    2014-01-01

    Due to the growth in the number of procedures that make use of the positron emission tomography (PET), there is a need for standard solutions for the calibration of the systems used for the measurement of the PET radiopharmaceutical (activimeter) in radiopharmacies and in nuclear medicine services. Among the existing alternatives for the standardization of radioactive sources, the method known as gamma spectrometry is widely used for short-lived radionuclides. The purpose of this study was to implement the methodology for standardization of the 18 F solutions by gamma spectrometry at the Regional Center for Nuclear Sciences of the Northeast (CRCN-NE/CNEN-NE), Brazil. (author)

  5. Comparison of 4 analytical techniques based on atomic spectrometry for the determination of total tin in canned foodstuffs

    OpenAIRE

    2011-01-01

    Abstract Different techniques for the determination of total tin in beverage and canned food by atomic spectrometry were compared. The performance characteristics of Inductively Coupled Plasma Mass Spectrometry (ICP-MS), Hydride Generation Inductively Coupled Plasma Atomic Emission Spectrometry (HG-ICP-AES), Electrothermal Atomization Atomic Absorption Spectrometry (ETA-AAS) and Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) were determined in term of linearity, ...

  6. Use of X-Ray Fluorescence Spectrometry to Determine Trace ...

    African Journals Online (AJOL)

    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, as function of ...

  7. Quantitative determination of impurities in nuclear grade aluminum by Flame-Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    Jat, J.R.; Nayak, A.K.; Balaji Rao, Y.; Ravindra, H.R.

    2013-01-01

    The paper deals with quantitative determination of impurity elements in nuclear grade aluminum, used as fin tubes in research reactors, by Flame-Atomic Absorption Spectrometry (F-AAS). The results have been compared with those obtained by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) method. Experimental conditions used in both the methods are given in the paper. (author)

  8. 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…

  9. Determination of {sup 135}Cs by accelerator mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    MacDonald, C.M.; Charles, C.R.J. [Andre. E. Lalonde AMS Laboratory, University of Ottawa, 150 Louis Pasteur, Ottawa, ON K1N 6N5 (Canada); Department of Earth Sciences, University of Ottawa, 150 Louis Pasteur, Ottawa, ON K1N 6N5 (Canada); Zhao, X.-L.; Kieser, W.E. [Andre. E. Lalonde AMS Laboratory, University of Ottawa, 150 Louis Pasteur, Ottawa, ON K1N 6N5 (Canada); Department of Physics, University of Ottawa, 150 Louis Pasteur, Ottawa, ON K1N 6N5 (Canada); Cornett, R.J. [Andre. E. Lalonde AMS Laboratory, University of Ottawa, 150 Louis Pasteur, Ottawa, ON K1N 6N5 (Canada); Department of Earth Sciences, University of Ottawa, 150 Louis Pasteur, Ottawa, ON K1N 6N5 (Canada); Litherland, A.E. [IsoTrace Laboratory, University of Toronto, 60 St. George St., Toronto, ON M5S 1A7 (Canada)

    2015-10-15

    The ratio of anthropogenic {sup 135}Cs and {sup 137}Cs isotopes is characteristic of a uranium fission source. This research evaluates the technique of isotope dilution (yield tracing) for the purpose of quantifying {sup 135}Cs by accelerator mass spectrometry with on-line isobar separation. Interferences from Ba, Zn{sub 2}, and isotopes of equal mass to charge ratios were successfully suppressed. However, some sample crosstalk from source contamination remains. The transmission and di-fluoride ionization efficiencies of Cs isotopes were found to be 8 × 10{sup −3} and 1.7 × 10{sup −7} respectively. This quantification of {sup 135}Cs using yield tracing by accelerator mass spectrometry shows promise for future environmental sample analysis once the issues of sample crosstalk and low efficiency can be resolved.

  10. 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.)

  11. Determination of trimethyllead reference material using high performance liquid chromatography-inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Lu Hai; Wei Chao; Wang Jun; Chao Jingbo; Zhou Tao; Chen Dazhou

    2005-01-01

    A high-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICPMS) was combined, and the chromatography conditions were optimized. The stability and homogeneity of a trimethyllead reference material were determined using this method. (authors)

  12. Simultaneous Determination of Cobalt (II and Nickel (II By First Order Derivative Spectrophotometry in Micellar Media

    Directory of Open Access Journals (Sweden)

    Rajni Rohilla

    2012-01-01

    Full Text Available A first-derivative spectrophotometry method for the simultaneous determination of Co (II and Ni (II with Alizarin Red S in presence of Triton X-100 is described. Measurements were made at the zero-crossing wavelengths at 549.0 nm for Co (II and 546.0 nm for Ni (II. The linearity is obtained in the range of 0.291- 4.676 μg/ml of Ni (II and 0.293- 4.124 μg/ml of Co (II in the presence of each other by using first derivative spectrophotometric method. The possible interfering effects of various ions were studied. The validity of the method was examined by using synthetic mixtures of Co (II and Ni (II. The developed derivative procedure, using the zero crossing technique, has been successfully applied for the simultaneous analysis of Co (II and Ni (II in spiked water samples.

  13. CATALYTIC SPECTROPHOTOMETRIC DETERMINATION OF Mn(II ...

    African Journals Online (AJOL)

    Preferred Customer

    method is based on the catalytic effect of Mn(II) with the oxidation of Celestine blue .... water samples were filtered through a 0.45 μm pore size membrane filter to remove suspended .... slope of the calibration graph as the optimization criterion. ..... In presence of Phen as stability enhancement agent in indicator system. ( ) +.

  14. Mass Determination of Entire Amyloid Fibrils by Using Mass Spectrometry.

    Science.gov (United States)

    Doussineau, Tristan; Mathevon, Carole; Altamura, Lucie; Vendrely, Charlotte; Dugourd, Philippe; Forge, Vincent; Antoine, Rodolphe

    2016-02-12

    Amyloid fibrils are self-assembled protein structures with important roles in biology (either pathogenic or physiological), and are attracting increasing interest in nanotechnology. However, because of their high aspect ratio and the presence of some polymorphism, that is, the possibility to adopt various structures, their characterization is challenging and basic information such as their mass is unknown. Here we show that charge-detection mass spectrometry, recently developed for large self-assembled systems such as viruses, provides such information in a straightforward manner. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Determination of technetium by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Kaye, J.H.; Ballou, N.E.

    1978-01-01

    A detection limit of 6 x 10 -11 g has been achieved for measurement of technetium by graphite furnace atomic absorption spectrometry. A commercially available, demountable, hollow cathode lamp was used and both argon and neon were used as fill gases for the lamp. The range of applicability of the method, when the unresolved 2614.23 to 2615.87 A doublet is used for analysis, is from 60 pg to at least 3 ng of technetium per aliquot analyzed. 3 figures, 1 table

  16. Determination of seven pyrethroids and six pyrethrins in water by liquid chromatography/mass spectrometry

    Science.gov (United States)

    ccanccapa, alexander; Masia, Ana; Pico, Yolanda

    2016-04-01

    Pyrethroids are the synthetic analogues of pyrethrins which were developed as pesticides from the extracts of dried and powdered flower heads of Chrysanthemum cinerariaefolium. They are increasingly used in agriculture due to their broad biological activity and slow development of pest resistance. Contamination of fresh-water ecosystems appears either because of the direct discharge of industrial and agricultural effluents or as a result of effluents from sewage treatment works; residues can thus accumulate in the surrounding biosphere [1, 2]. These substances, mostly determined by gas chromatography mass spectrometry (GC-MS) can be difficult to analyse due to their volatility and degradability. The purpose of this study is, as an alternative, to develop a fast and sensitive multi-residue method for the target analysis of 7 pyrethroids and the 6 natural pyrethrins currently used in water samples by liquid chromatography tandem mass spectrometry (LC-MS/MS). The compounds included in the study were acrinathrin, etofenprox, cyfluthrin, esfenvalerate, cyhalothrin, cypermethrin and flumethrin as pyrethroids and a commercial mix of pyrethrins containing Cinerin I, Jasmolin I, pyrethrin I, cinerin II, jasmolin II, pyrethrins II in different percentages. As a preliminary step, the ionization and fragmentation of the compounds were optimized injecting individual solutions of each analyte at 10 ppm in the system, using a gradient elution profile of water-methanol both with 10 mM ammonium formate. The ESI conditions were: capillary voltage 4000 V, nebulizer15 psi, source temperature 300◦C and gas flow 10 L min-1. [M+H]+, [M+Na]+ ,[M+NH3]+ ,[M+NH4+]+ were tested as precursor ions. The most intense signal was for ammonium adduct for all compounds. The optimal fragmentor range for product ions were between 20 to 80 ev and the collision energy ranged between 5 to 86 ev. The efficiency of the method was tested in water samples from Turia River without any known exposure to

  17. Critical evaluation of analytical performance of atomic absorption spectrometry and inductively coupled plasma mass spectrometry for mercury determination

    International Nuclear Information System (INIS)

    Krata, A.; Bulska, E.

    2005-01-01

    The analytical performance of cold vapor atomic absorption spectrometry (CV AAS), graphite furnace atomic absorption spectrometry (GF AAS) and inductively coupled plasma mass spectrometry (ICP-MS) for mercury determination have been investigated with the use of two reference materials SRM 2710 Montana I Soil and BCR-144R (sewage sludge from domestic origin). The digestion conditions and their influence on determination of mercury have been studied. Samples were decomposed by microwave digestion in closed vessels with the use of HCl alone or mixture of HCl+HNO 3 +HF. The digestion solutions were analyzed by CV AAS using NaBH 4 as a reducing agent, by GF AAS with Pd or mixture of Pd/Rh as modifiers and by ICP-MS with Rh as internal standard. In the case of CV AAS, results were not dependent on digestion conditions. In the case of GF AAS and ICP-MS, results depended significantly on digestion conditions; in both cases, the use of the mixture of acids as defined above suppressed the signal of mercury. Therefore, in those cases, the microwave digestion with HCl is recommended. Detection limits of 0.003, 0.01 and 0.2 μg g -1 were achieved by ICP-MS, CV AAS and GF AAS, respectively

  18. Alpha spectrometry of thick sources. II. Application to the study of radioactive equilibria in uranium ores

    International Nuclear Information System (INIS)

    Acena Barrenechea, M.L.; Tormo Ferrero, M.J.

    1977-01-01

    A method for determining nuclide activities in 4n + 2 uranium series using alpha spectrometry of thick sources is described. This method has been applied to several uranium ores, showing different states of radioactive equilibria. The spectra from samples prepared by cold compression show some anomalies, due to the evolution and later decay of 219 Rn and daughters. This phenomenon must be taken in consideration when computing spectra line intensities. (author) [es

  19. Comparison of two methods for blood lead analysis in cattle: graphite-furnace atomic absorption spectrometry and LeadCare(R) II system.

    Science.gov (United States)

    Bischoff, Karyn; Gaskill, Cynthia; Erb, Hollis N; Ebel, Joseph G; Hillebrandt, Joseph

    2010-09-01

    The current study compared the LeadCare(R) II test kit system with graphite-furnace atomic absorption spectrometry for blood lead (Pb) analysis in 56 cattle accidentally exposed to Pb in the field. Blood Pb concentrations were determined by LeadCare II within 4 hr of collection and after 72 hr of refrigeration. Blood Pb concentrations were determined by atomic absorption spectrometry, and samples that were coagulated (n = 12) were homogenized before analysis. There was strong rank correlation (R(2) = 0.96) between atomic absorption and LeadCare II (within 4 hr of collection), and a conversion formula was determined for values within the observed range (3-91 mcg/dl, although few had values >40 mcg/dl). Median and mean blood pb concentrations for atomic absorption were 7.7 and 15.9 mcg/dl, respectively; for LeadCare II, medians were 5.2 mcg/dl at 4 hr and 4.9 mcg/dl at 72 hr, and means were 12.4 and 11.7, respectively. LeadCare II results at 4 hr strongly correlated with 72 hr results (R(2) = 0.96), but results at 72 hr were lower (P atomic absorption. Although there have been several articles that compared LeadCare with other analytical techniques, all were for the original system, not LeadCare II. The present study indicated that LeadCare II results correlated well with atomic absorption over a wide range of blood Pb concentrations and that refrigerating samples for up to 72 hr before LeadCare II analysis was acceptable for clinical purposes.

  20. Determination of trace amounts of impurities in molybdenum by spark source and glow discharge mass spectrometry

    International Nuclear Information System (INIS)

    Saito, Morimasa

    1994-01-01

    For the determination of trace and ultra-trace amounts of impurities in high-purity molybdenum, spark source mass spectrometry and glow discharge mass spectrometry were studied. In spark source mass spectrometry using the metal probe method, the liquid-helium cryogenic pump was used in order to protect the surface of the samples from oxidation. The theoretical relative sensitivity factors (Mo=1) calculated from physical properties were used. The analytical results obtained for molybdenum tablet and high-purity molybdenum were in good agreement with those obtained by other methods (atomic absorption spectrometry and others). In glow discharge mass spectrometry, the relative sensitivity factors were calculated by using the results obtained by spark source mass spectrometry and atomic absorption spectrometry, and this method was applied to the determination of ultra-trace amounts of impurities in ultra high-purity molybdenum and gave the satisfactory results. The detection limits (2σ, n=10) in the integration time of 600 s for U and Th were 0.6 ppb and 0.3 ppb, and the values for Al, Si, Cr, Mn and Cu were in the range of 10 ppb to 0.5 ppb. (author)

  1. Determination of Natural Radioactivity in Building Materials with Gamma Spectrometry

    International Nuclear Information System (INIS)

    Turki, Faten

    2010-01-01

    In the setting of this work, the natural radioactivity of building materials used in Tunisia has been measured by gamma spectrometry. These products have been ground and dried at 100 degree for 12 h. Then, they have been homogenized, weighed and finally conditioned during 23 days in order to reach the radioactive equilibrium. The measures' results proved that all building materials studied except bauxite and the ESC clay, possess doses lower than the acceptable limit (1 mSv.an-1). However, the possibility of reinforcement of the natural radioactivity in some industry of building can exist. To insure that the cement, the most used in the world, don't present any radiological risk on the workers' health, a survey has been made in the factory - les Ciments de Bizerte - about its manufacture's process. The results of this survey showed that this product can be considered like a healthy product.

  2. Spectrochemical determination of tantalum in plutonium metal using direct current plasma emission spectrometry

    International Nuclear Information System (INIS)

    Fadeff, S.K.; Morris, W.F.

    1983-01-01

    Tantalum is determined by direct current plasma spectrometry after separation of plutonium from solution as PuF 3 . After centrifugation of the PuF 3 precipitate, a low level of plutonium remains in solution in sufficient quantity to cause spectral interferences. It is necessary to determine the plutonium by dc plasma spectrometry and apply a correction to determine low tantalum concentrations with good accuracy and precision. Tantalum can be determined down to 0.4 ppM in solution with a relative standard deviation of 10 percent. Better precision can be achieved at higher concentrations. The procedure is simple and convenient for glovebox work. 5 references, 1 figure, 1 table

  3. Burn-up determination of irradiated thoria samples by isotope dilution-thermal ionisation mass spectrometry

    International Nuclear Information System (INIS)

    Aggarwal, S.K.; Jaison, P.G.; Telmore, V.M.; Shah, R.V.; Sant, V.L.; Sasibhushan, K.; Parab, A.R.; Alamelu, D.

    2010-03-01

    Burn-up was determined experimentally using thermal ionization mass spectrometry for two samples from ThO 2 bundles irradiated in KAPS-2. This involved quantitative dissolution of the irradiated fuel samples followed by separation and determination of Th, U and a stable fission product burn-up monitor in the dissolved fuel solution. Stable fission product 148 Nd was used as a burn-up monitor for determining the number of fissions. Isotope Dilution-Thermal Ionisation Mass Spectrometry (ID-TIMS) using natural U, 229 Th and enriched 142 Nd as spikes was employed for the determination of U, Th and Nd, respectively. Atom % fission values of 1.25 ± 0.03 were obtained for both the samples. 232 U content in 233 U determined by alpha spectrometry was about 500 ppm and this was higher by a factor of 5 compared to the theoretically predicted value by ORIGEN-2 code. (author)

  4. Application of Carrier Element-Free Co-precipitation Method for Ni(II), Cu(II) and Zn(II) Ions Determination in Water Samples Using Chrysin

    International Nuclear Information System (INIS)

    Layth Imad Abd Ali; Wan Aini Wan Ibrahim; Azli Sulaiman; Mohd Marsin Sanagi

    2015-01-01

    A co-precipitation method was developed to separate and pre-concentrate Ni(II), Cu(II) and Zn(II) ions using an organic co precipitant, chrysin without adding any carrier element termed as carrier element-free co-precipitation (CEFC). Analytes were determined using flame atomic absorption spectrometry (FAAS). The influence of analytical conditions, such as pH of the solution, quantity of co-precipitant, standing time, centrifugation rate and time, sample volume, and interference of concomitant ions were investigated over the recovery yields of the trace metals. The limit of detection, the limit of quantification and linearity range obtained from the FAAS measurements were found to be in the range of 0.64 to 0.86 μg L -1 , 2.13 to 2.86 μg L -1 and 0.9972 to 0.9989 for Ni(II), Cu(III) and Zn(II) ions, respectively. The precision of the method, evaluated as the relative standard deviation (RSD) obtained after analyzing a series of 10 replicates, was between 2.6 % to 3.9 % for the trace metal ions. The proposed procedure was applied and validated by analyzing river water reference material for trace metals (SLRS-5) and spiking trace metal ions in some water samples. The recoveries of the analyte metal ions were between 94.7-101.2 %. (author)

  5. Solid-phase extraction of Mn(II), Co(II), Ni(II), Cu(II), Cd(II) and Pb(II) ions from environmental samples by flame atomic absorption spectrometry (FAAS)

    Energy Technology Data Exchange (ETDEWEB)

    Duran, Celal [Department of Chemistry, Faculty of Art and Science, Karadeniz Technical University, 61080 Trabzon (Turkey); Gundogdu, Ali [Department of Chemistry, Faculty of Art and Science, Karadeniz Technical University, 61080 Trabzon (Turkey); Bulut, Volkan Numan [Department of Chemistry, Giresun Faculty of Art and Science, Karadeniz Technical University, 28049 Giresun (Turkey); Soylak, Mustafa [Department of Chemistry, Faculty of Art and Science, Erciyes University, 38039 Kayseri (Turkey)]. E-mail: soylak@erciyes.edu.tr; Elci, Latif [Department of Chemistry, Faculty of Art and Science, Pamukkale University, 20020 Denizli (Turkey); Sentuerk, Hasan Basri [Department of Chemistry, Faculty of Art and Science, Karadeniz Technical University, 61080 Trabzon (Turkey); Tuefekci, Mehmet [Department of Chemistry, Faculty of Art and Science, Karadeniz Technical University, 61080 Trabzon (Turkey)

    2007-07-19

    A new method using a column packed with Amberlite XAD-2010 resin as a solid-phase extractant has been developed for the multi-element preconcentration of Mn(II), Co(II), Ni(II), Cu(II), Cd(II), and Pb(II) ions based on their complex formation with the sodium diethyldithiocarbamate (Na-DDTC) prior to flame atomic absorption spectrometric (FAAS) determinations. Metal complexes sorbed on the resin were eluted by 1 mol L{sup -1} HNO{sub 3} in acetone. Effects of the analytical conditions over the preconcentration yields of the metal ions, such as pH, quantity of Na-DDTC, eluent type, sample volume and flow rate, foreign ions etc. have been investigated. The limits of detection (LOD) of the analytes were found in the range 0.08-0.26 {mu}g L{sup -1}. The method was validated by analyzing three certified reference materials. The method has been applied for the determination of trace elements in some environmental samples.

  6. Protein Glycation in Diabetes as Determined by Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Annunziata Lapolla

    2013-01-01

    Full Text Available Diabetes is a common endocrine disorder characterized by hyperglycemia leading to nonenzymatic glycation of proteins, responsible for chronic complications. The development of mass spectrometric techniques able to give highly specific and reliable results in proteome field is of wide interest for physicians, giving them new tools to monitor the disease progression and the possible complications related to diabetes, as well as the effectiveness of therapeutic treatments. This paper reports and discusses some of the data pertaining protein glycation in diabetic subjects obtained by matrix-assisted laser desorption ionization (MALDI mass spectrometry (MS. The preliminary studies carried out by in vitro protein glycation experiments show clear differences in molecular weight of glycated and unglycated proteins. Then, the attention was focused on plasma proteins human serum albumin (HSA and immunoglobulin G (IgG. Enzymatic degradation products of in vitro glycated HSA were studied in order to simulate the in vivo enzymatic digestion of glycated species by the immunological system leading to the highly reactive advanced glycation end-products (AGEs peptides. Further studies led to the evaluation of glycated Apo A-I and glycated haemoglobin levels. A different MALDI approach was employed for the identification of markers of disease in urine samples of healthy, diabetic, nephropathic, and diabetic-nephropathic subjects.

  7. Determination of iron in seawater by electrothermal atomic absorption spectrometry and atomic fluorescence spectrometry: A comparative study

    International Nuclear Information System (INIS)

    Cabon, J.Y.; Giamarchi, P.; Le Bihan, A.

    2010-01-01

    Two methods available for direct determination of total Fe in seawater at low concentration level have been examined: electrothermal atomization atomic absorption spectrometry (ETAAS) and electrothermal atomization laser excited atomic fluorescence spectrometry (ETA-LEAFS). In a first part, we have optimized experimental conditions of ETAAS (electrothermal program, matrix chemical modification) for the determination of Fe in seawater by minimizing the chemical interference effects and the magnitude of the simultaneous background absorption signal. By using the best experimental conditions, a detection limit of 80 ng L -1 (20 μL, 3σ) for total Fe concentration was obtained by ETAAS. Using similar experimental conditions (electrothermal program, chemical modification), we have optimized experimental conditions for the determination of Fe by LEAFS. The selected experimental conditions for ETA-LEAFS: excitation wavelength (296.69 nm), noise attenuation and adequate background correction led to a detection limit (3σ) of 3 ng L -1 (i.e. 54 pM) for total Fe concentration with the use a 20 μL seawater sample. For the two methods, concentration values obtained for the analysis of Fe in a NASS-5 (0.2 μg L -1 ) seawater sample were in good agreement with the certified values.

  8. Determination of iron in seawater by electrothermal atomic absorption spectrometry and atomic fluorescence spectrometry: a comparative study.

    Science.gov (United States)

    Cabon, J Y; Giamarchi, P; Le Bihan, A

    2010-04-07

    Two methods available for direct determination of total Fe in seawater at low concentration level have been examined: electrothermal atomization atomic absorption spectrometry (ETAAS) and electrothermal atomization laser excited atomic fluorescence spectrometry (ETA-LEAFS). In a first part, we have optimized experimental conditions of ETAAS (electrothermal program, matrix chemical modification) for the determination of Fe in seawater by minimizing the chemical interference effects and the magnitude of the simultaneous background absorption signal. By using the best experimental conditions, a detection limit of 80 ng L(-1) (20 microL, 3sigma) for total Fe concentration was obtained by ETAAS. Using similar experimental conditions (electrothermal program, chemical modification), we have optimized experimental conditions for the determination of Fe by LEAFS. The selected experimental conditions for ETA-LEAFS: excitation wavelength (296.69 nm), noise attenuation and adequate background correction led to a detection limit (3sigma) of 3 ng L(-1) (i.e. 54 pM) for total Fe concentration with the use a 20 microL seawater sample. For the two methods, concentration values obtained for the analysis of Fe in a NASS-5 (0.2 microg L(-1)) seawater sample were in good agreement with the certified values. Copyright 2010 Elsevier B.V. All rights reserved.

  9. Fluorescent sensing and determination of mercury (II) ions in water ...

    African Journals Online (AJOL)

    In this study we report on a fluorescent sensing probe based on a naphthyl azo dye modified dibenzo-18-crown-6-ether (DB18C6) for the detection and determination of mercury (II) ions in water. The probe showed high sensitivity and selectivity towards the mercury (II) ion among various alkali, alkaline earth, and transition ...

  10. Determination of ultra-low levels of uranium using resonance ionization mass spectrometry

    International Nuclear Information System (INIS)

    Kiran Kumar, P.V.; Acharyulu, G.V.S.G.

    2015-01-01

    The determination of isotopic composition of actinides like U and Pu is important, due to their distribution in the environment as a result of nuclear weapons testing, fuel reprocessing, reactor operations and to a smaller extent from accidental releases. The analytical methods like fission track analysis (FTA), thermal ionization mass spectrometry (TIMS), inductively coupled plasma mass spectrometry (ICPMS) and resonance ionization mass spectrometry (RIMS) have evolved as sensitive techniques. Resonance Ionization Mass Spectrometry yields rapid isotopic signature data for material containing actinides without requiring time-consuming sample preparation and chemical separation procedures. In this paper, authors presented the details of the methodology and results for low-level detection of uranium using RIMS

  11. Preconcentration of natural protactinium from thorium concentrate with subsequent determination using Gamma (γ) spectrometry

    International Nuclear Information System (INIS)

    Raja, Naine; Swain, Kallola; Kayasth, S.R.; Pathassarathy, R.; Mathur, P.K.; Anil Kumar, S.

    1999-01-01

    A simple and efficient method has been developed to preconcentrate natural protactinium ( 231 Pa) from large size of thorium concentrate (5.0-100.0g) on Dowex 1 X 8 in acid medium. Gamma spectrometry, a powerful determination technique, has been used for quantitative determination of protactinium

  12. Determination of heavy metals in polar snow and ice by laser-excited atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    Bolshov, M.A.; Boutron, C.F.

    1994-01-01

    The new laser-excited atomic fluorescence spectrometry technique offers unrivalled sensitivity for the determination of trace metals in a wide variety of samples. This has allowed the direct determination of Pb, Cd and Bi in Antarctic and Greenland snow and ice down to the sub pg/g level. (authors). 11 refs., 2 figs

  13. Uranium analysis. Impurities determination by spark mass spectrometry

    International Nuclear Information System (INIS)

    Anon.

    Determination of impurities in uranium, suitable for atomic content greater than 10 -8 , particularly adapted for a low content. The method is quantitative for metallic impurities and qualitative for non metallic impurities [fr

  14. 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.)

  15. Major constituent quantitative determination in uranium alloys by coupled plasma atomic emission spectrometry and X ray fluorescence wavelength dispersive spectrometry

    International Nuclear Information System (INIS)

    Oliveira, Luis Claudio de; Silva, Adriana Mascarenhas Martins da; Gomide, Ricardo Goncalves; Silva, Ieda de Souza

    2013-01-01

    A wavelength-dispersive X-ray fluorescence (WD-XRF) spectrometric method for determination of major constituents elements (Zr, Nb, Mo) in Uranium/Zirconium/Niobium and Uranium/Molybdenum alloy samples were developed. The methods use samples taken in the form of chips that were dissolved in hot nitric acid and precipitate particles melted with lithium tetraborate and dissolved in hot nitric acid and finally analyzed as a solution. Studies on the determination by inductively coupled plasma optic emission spectrometry (ICP OES) using matched matrix in calibration curve were developed. The same samples solution were analyzed in both methods. The limits of detection (LOD), linearity of the calibrations curves, recovery study, accuracy and precision of the both techniques were carried out. The results were compared. (author)

  16. Structural determination of intact proteins using mass spectrometry

    Science.gov (United States)

    Kruppa, Gary [San Francisco, CA; Schoeniger, Joseph S [Oakland, CA; Young, Malin M [Livermore, CA

    2008-05-06

    The present invention relates to novel methods of determining the sequence and structure of proteins. Specifically, the present invention allows for the analysis of intact proteins within a mass spectrometer. Therefore, preparatory separations need not be performed prior to introducing a protein sample into the mass spectrometer. Also disclosed herein are new instrumental developments for enhancing the signal from the desired modified proteins, methods for producing controlled protein fragments in the mass spectrometer, eliminating complex microseparations, and protein preparatory chemical steps necessary for cross-linking based protein structure determination.Additionally, the preferred method of the present invention involves the determination of protein structures utilizing a top-down analysis of protein structures to search for covalent modifications. In the preferred method, intact proteins are ionized and fragmented within the mass spectrometer.

  17. 134Cs emission probabilities determination by gamma spectrometry

    Science.gov (United States)

    de Almeida, M. C. M.; Poledna, R.; Delgado, J. U.; Silva, R. L.; Araujo, M. T. F.; da Silva, C. J.

    2018-03-01

    The National Laboratory for Ionizing Radiation Metrology (LNMRI/IRD/CNEN) of Rio de Janeiro performed primary and secondary standardization of different radionuclides reaching satisfactory uncertainties. A solution of 134Cs radionuclide was purchased from commercial supplier to emission probabilities determination of some of its energies. 134Cs is a beta gamma emitter with 754 days of half-life. This radionuclide is used as standard in environmental, water and food control. It is also important to germanium detector calibration. The gamma emission probabilities (Pγ) were determined mainly for some energies of the 134Cs by efficiency curve method and the Pγ absolute uncertainties obtained were below 1% (k=1).

  18. Equilibria determination in uranium ores by alpha spectrometry

    International Nuclear Information System (INIS)

    Tormo Ferrero, M.J.

    1976-01-01

    A method for the measurement of the U-234/U-238 activities is described. The separation of the uranium from the interferring elements is carried out by ionic change with anionic resine, in chlorhydric-metanol-ascorbic acid medium. The method has been applied to different spanish ores in which the equilibrium state has been determined (author)

  19. Simultaneous determination of actinides by x-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Cohen, V.H.

    1990-01-01

    The x-ray spectrometric simultaneous determination of uranium and plutonium in simulated Purex Process solutions is described. The method is accomplished by intensity measurements of the L α sub(1) lines. The thin film technique for sample preparation and thorium as an internal standard had been used. An evaporation technique had been also tested for low concentration uranium solutions. In the measurement range 0,05 - 130 U g/L, 0,5 - 20 Pu g/L linear calibration curves were effected. The standard deviation in the concentration range 10 to 130 g/L was 3,5%, 4% in the 1 to 10 g/L and 13% in 0,05 to 1 g/L for uranium determination and 4% for plutonium determination in the range of 1 to 20 g/L. The sensitivity of the method was about 3,62 μg to U and 3,95 μg to Pu. Uranium and plutonium do not reciprocally interfere with one another until U/Pu ≅ 90 m/m. The fission product as interfering elements were also verified. Finally, uranium and plutonium were determined in simulated Purex Process solutions within the requested accuracy for control method. (author)

  20. 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)

  1. Demonstration of a collimated in situ method for determining depth distributions using gamma-ray spectrometry

    CERN Document Server

    Benke, R R

    2002-01-01

    In situ gamma-ray spectrometry uses a portable detector to quantify radionuclides in materials. The main shortcoming of in situ gamma-ray spectrometry has been its inability to determine radionuclide depth distributions. Novel collimator designs were paired with a commercial in situ gamma-ray spectrometry system to overcome this limitation for large area sources. Positioned with their axes normal to the material surface, the cylindrically symmetric collimators limited the detection of un attenuated gamma-rays from a selected range of polar angles (measured off the detector axis). Although this approach does not alleviate the need for some knowledge of the gamma-ray attenuation characteristics of the materials being measured, the collimation method presented in this paper represents an absolute method that determines the depth distribution as a histogram, while other in situ methods require a priori knowledge of the depth distribution shape. Other advantages over previous in situ methods are that this method d...

  2. {sup 134}Cs emission probabilities determination by gamma spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, M.C.M. de, E-mail: candida@cnen.gov.br [Comissão Nacional de Energia Nuclear (DINOR/CNEN), Riode Janeiro, RJ (Brazil); Poledna, R.; Delgado, J.U.; Silva, R.L.; Araujo, M.T.; Silva, C.J. da [Instituto de Radioproteção e Dosimetria (LNMRI/IRD/CNEN-RJ), Rio de Janeiro, RJ (Brazil)

    2017-07-01

    The National Laboratory for Ionizing Radiation Metrology (LNMRI/IRD/CNEN) of Rio de Janeiro performed primary and secondary standardization of different radionuclides reaching satisfactory uncertainties. A solution of {sup 134}Cs radionuclide was purchased from commercial supplier to emission probabilities determination of some of its energies. {sup 134}Cs is a beta gamma emitter with 754 days of half-life. This radionuclide is used as standard in environmental, water and food control. It is also important to germanium detector calibration.The gamma emission probabilities (Pγ) were determined mainly for some energies of the {sup 134}Cs by efficiency curve method and the Pγ absolute uncertainties obtained were below 1% (k=1). (author)

  3. Determination of thoron and radon ratio by liquid scintillation spectrometry

    International Nuclear Information System (INIS)

    Yoshikawa, H.; Nakanishi, T.; Nakahara, H.

    2006-01-01

    A portable liquid scintillation counter was applied for the analysis of alpha-ray energy spectrum to determine the ratio of 220 Rn/ 222 Rn in fumarolic gas in the field. A surface-polished vial was developed, by which a Gaussian distribution could be approximated for the alpha-ray energy spectra and the peak areas of the nuclides could be estimated independently, because of the wide FWHM in the liquid scintillation pulse. A fumarolic gas sample was collected in Mt. Kamiyama (Hakoneyama geothermal field in Japan) having low 220 Rn/ 222 Rn ratio of 2.20 ± 0.13. (author)

  4. Synthesis and application of surface-imprinted activated carbon sorbent for solid-phase extraction and determination of copper (II)

    Science.gov (United States)

    Li, Zhenhua; Li, Jingwen; Wang, Yanbin; Wei, Yajun

    2014-01-01

    A new Cu(II)-imprinted amino-functionalized activated carbon sorbent was prepared by a surface imprinting technique for selective solid-phase extraction (SPE) of Cu(II) prior to its determination by inductively coupled plasma atomic emission spectrometry (ICP-AES). Experimental conditions for effective adsorption of Cu(II) were optimized with respect to different experimental parameters using static and dynamic procedures in detail. Compared with non-imprinted sorbent, the ion-imprinted sorbent had higher selectivity and adsorption capacity for Cu(II). The maximum static adsorption capacity of the ion-imprinted and non-imprinted sorbent for Cu(II) was 26.71 and 6.86 mg g-1, respectively. The relatively selectivity factor values (αr) of Cu(II)/Zn(II), Cu(II)/Ni(II), Cu(II)/Co(II) and Cu(II)/Pb(II) were 166.16, 50.77, 72.26 and 175.77, respectively, which were greater than 1. Complete elution of the adsorbed Cu(II) from Cu(II)-imprinted sorbent was carried out using 2 mL of 0.1 mol L-1 EDTA solution. The relative standard deviation of the method was 2.4% for eleven replicate determinations. The method was validated for the analysis by two certified reference materials (GBW 08301, GBW 08303), the results obtained is in good agreement with standard values. The developed method was also successfully applied to the determination of trace copper in natural water samples with satisfactory results.

  5. Determination of radium isotopes in environmental samples by gamma spectrometry, liquid scintillation counting and alpha spectrometry: a review of analytical methodology

    International Nuclear Information System (INIS)

    Jia, Guogang; Jia, Jing

    2012-01-01

    Radium (Ra) isotopes are important from the viewpoints of radiation protection and environmental protection. Their high toxicity has stimulated the continuing interest in methodology research for determination of Ra isotopes in various media. In this paper, the three most routinely used analytical techniques for Ra isotope determination in biological and environmental samples, i.e. low-background γ-spectrometry, liquid scintillation counting and α-spectrometry, were reviewed, with emphasis on new methodological developments in sample preparation, preconcentration, separation, purification, source preparation and measurement techniques. The accuracy, selectivity, traceability, applicability and minimum detectable activity (MDA) of the three techniques were discussed. It was concluded that the MDA (0.1 mBq L −1 ) of the α-spectrometry technique coupled with chemical separation is about two orders of magnitude lower than that of low-background HPGe γ-spectrometry and LSC techniques. Therefore, when maximum sensitivity is required, the α-spectrometry technique remains the first choice. - Highlights: ► A review is made for determination of Ra isotopes in environmental samples. ► Gamma spectrometry, LSC and a-spectrometry are the main concerned radiometric approach. ► Sample preparation, preconcentration, separation and source preparation are discussed. ► The methods can analyse air, water, seawater, soil, sediment and foodstuffs samples. ► Some new data obtained recently from our laboratory for Ra method study are included.

  6. Determination of cobalt(II) and nickel(II) with isoamylxanthate as a complexing reagent in micellar media

    International Nuclear Information System (INIS)

    Shar, G.A.; Soomro, G.A.

    2008-01-01

    Cobalt(II) and nickel(II) were determined spectrophotometrically using sodium isoamyl xanthate as a complexing reagent in aqueous phase in the presence of anionic surfactant sodium dodecylsulphate (SDS). Beer's law was obeyed for Co(ll) and Ni(ll) over the concentration range 3.0-35 and 2.0-37 micro gmL/sup -1/ respectively. The lambda/sub max/ molar absorptivity and Sandell's sensitivity of Co(ll) and Ni(ll) were 360 nm and 416 nm; is 0.19 and 0.2 (x 10/sup 4/ mol/sup -1/ cm/sup -1/) 31.1 and 29.3 ng cm/sup -2/ respectively. Maximum absorbance at 1:2 (M: L) molar ratio suggested the formation of M(C/sub 6/H/sub 11/ OS/sub 2/)/sub 2/ where M = Co(II) and Ni(II). The complex remained stable for more than 2 h. The optimized reagent concentration 0.5% was used throughout the study. Surfactant concentration of 1.0% SDS caused significant enhancement in absorbance. Maximum absorption was observed at 360 nm and 416 nm for Co and Ni complexes, respectively. The absorption maxima were obtained at optimized pH of 7.0. Validation of method has been made by comparing the results with Atomic Absorption Spectrometry, no significant difference was obtained between the two methods at 95% confidence interval. The method is simple, accurate, economical and has been applied to the determination of cobalt(ll) and nickel(ll) in industrial wastewater, pharmaceutical and edible oil samples. (author)

  7. Determination of tin (II) in radiopharmaceutical kits by polarographic method

    International Nuclear Information System (INIS)

    Aungurarat, A.; Thuntawewadthananon, T.

    1996-01-01

    Radiopharmaceutical kit is a diagnostic compound which contains Stannous (II) as a reducing agent. The quantity of Stannous (II) is depended on the type of kits. So the quantity of Stannous (II) is determined by polarographic method with Differential Pulse Voltammetry (D P Mode) in which a saturated calomel electrode is used as anode and a dropping mercury electrode is used as cathode. Both of electrodes are immerged in the premixed solution of supporting electrolyte and analytical Stannous (II). The Stannous (II) is determined by direct method Stannous (II) is analyzed in the form of Stannous; Sn 2 + itself, and indirect method Stannous (II) is analyzed in the form of S tannic; Sn 4+ (Sn 2+ , + N H 4 + ----> Sn 4+ ). Both methods are done at polarographic half wave potential -470 and -520 mV respectively. The Limit of Detection (LOD) of the direct method is 1.9445 micro g and indirect method is 1.3018 micro g. The result received from indirect method is much more accurate than the direct method (Sn 2+ ). The accuracy of the direct method is about 97.5-102.5% recovery

  8. Determination of ribavirin in human serum using liquid chromatography tandem mass spectrometry

    NARCIS (Netherlands)

    van der Lijke, H.; Alffenaar, J.-W. C.; Kok, W.Th.; Greijdanus, B.; Uges, D.R.A.

    2012-01-01

    A method has been developed for the determination of ribavirin in human serum for therapeutic drug monitoring purposes, using liquid chromatography electrospray ionization mass spectrometry. Separation was obtained with a mobile phase gradient starting and ending in 100% aqueous conditions using a

  9. Correction for sample self-absorption in activity determination by gamma spectrometry

    International Nuclear Information System (INIS)

    Galloway, R.B.

    1991-01-01

    Gamma ray spectrometry is a convenient method of determining the activity of the radioactive components in environmental samples. Commonly samples vary in gamma absorption or differ in absorption from the calibration standards available, so that accurate correction for self-absorption in the sample is essential. A versatile correction procedure is described. (orig.)

  10. Determination of ''226Ra by Alpha Spectrometry by Using ''225Ra as Yield Tracer

    International Nuclear Information System (INIS)

    Crespo, M. T.; Oller, O.

    1999-01-01

    A method for the determination of low-level ''226 Ra in environmental and geological samples by alpha spectrometry is described. The method is based on the use of ''225 Ra from ''229 Th as yield tracer and has been developed to analyze U, Th and Ra in the same sample. (Author) 12 refs

  11. Determination of /sup 226/Ra by alpha spectrometry of liquid scintillation

    Energy Technology Data Exchange (ETDEWEB)

    Nobrega, A W; Sachett, I A; Hespanhol, E C.B.

    1987-07-01

    The determination of /sup 226/Ra in environmental samples using alpha spectrometry in liquid scintilation is studied. The Radon/sup 1-2/ emanation method and /sup 226/Ra separation process of other radionuclides alpha emissors are analyzed. The use of /sup 226/Ra coprecipitation with barium sulphate is evaluated. (M.J.C.).

  12. Preparation of /sup 237/Np samples by electrodeposition and its determination by alpha spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mertzig, W; Matsuda, H T; Araujo, B.F. de; Araujo, J.A. de [Instituto de Pesquisas Energeticas e Nucleares, Sao Paulo (Brazil). Centro de Engenharia Quimica

    1980-01-01

    An analytical method followed by alpha spectrometry was developed for the determination of trace amounts of actinides. A technique for quantitative electrodeposition of /sup 237/Np, under optimal conditions, using a carrier, is presented. This method will be applied for the control of trace amounts of /sup 237/Np in the solutions from the reprocessing (Purex process) of irradiated uranium.

  13. Determination of organophosphorus acids by thermo-spray liquid chromatography-mass spectrometry

    NARCIS (Netherlands)

    Wils, E.R.J.; Hulst, A.G.

    1988-01-01

    The determination of thirteen organophosphorus acids, hydrolysis products of nerve agents and pesticides, by a combination of ion-pair liquid chromatography on a reversed-phase C18 column and thermospray mass spectrometry was investigated. Ammonium acetate and three tetraalkylammonium salts with

  14. Determination of platinum in human subcellular microsamples by inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Björn, Erik; Nygren, Yvonne; Nguyen, Tam T. T. N.

    2007-01-01

    A fast and robust method for the determination of platinum in human subcellular microsamples by inductively coupled plasma mass spectrometry was developed, characterized, and validated. Samples of isolated DNA and exosome fractions from human ovarian (2008) and melanoma (T289) cancer cell lines w...

  15. Determination of chlormequat in pears by liquid chromatography/mass spectrometry

    NARCIS (Netherlands)

    Mol, H.G.J.; Dam, R.C.J. van; Vreeken, R.J.; Steijger, O.M.

    2000-01-01

    A straightforward and reliable method was developed for the determination of chlormequat in pears by liquid chromatography/mass spectrometry (LC/MS). Water and methanol were compared as extraction solvents. Because no significant differences in extraction efficiency or repeatability were found,

  16. Determination of trace elements by resonant ionization mass spectrometry (RIMS)

    International Nuclear Information System (INIS)

    Ruster, W.; Ames, F.; Rehklau, D.; Mang, M.; Muehleck, C.; Rimke, H.; Sattelberger, P.; Herrmann, G.; Trautmann, N.; Kluge, H.J.; Otten, E.W.

    1988-01-01

    A resonant ionization mass spectrometer has been developed as an analytical tool for the detection of trace elements, especially of plutonium and other radionuclides. The sample, deposited on a rhenium filament, is evaporated by electrical heating and the atoms of the element under investigation are selectively ionized by laser light delivered from three dye lasers pumped by a copper vapour laser. The resulting photoions are detected in a time-of-flight spectrometer with a channelplate detector. For plutonium a mass resolution of M/ΔM=1500 was obtained and an overall detection efficiency of 4x10 -6 was determined for stepwise excitation and ionization via autoionizing states. With a laser light bandwidth of 3-5 GHz neighbouring isotopes could be suppressed by a factor of 20 due to isotope shifts in the excitation transitions. The isotope composition of synthetic samples was measured and good agreement was found with mass spectroscopic results. The influence of the hyperfine structure on the isotope ratios is discussed. (orig.)

  17. Determination of antimony by using tungsten trap atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Titretir, Serap [Department of Chemistry, Inoenue University, 44065 Malatya (Turkey); Kenduezler, Erdal [Department of Primary Education, Faculty of Education, Ahi Evran University, 40100 Kirsehir (Turkey); Arslan, Yasin [Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey); Department of Chemistry, Atatuerk University, 25240 Erzurum (Turkey); Kula, Ibrahim [Department of Chemistry, Mugla University, 48000 Mugla (Turkey); Bakirdere, Sezgin [Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey); Department of Chemistry, Zonguldak Karaelmas University, 67100 Zonguldak (Turkey); Ataman, O. Yavuz. [Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey)], E-mail: ataman@metu.edu.tr

    2008-08-15

    An electrically heated tungsten coil was used as a trap in the determination of antimony. The technique consists of three steps. Initially, SbH{sub 3} is formed by hydride generation procedure; then the analyte species in vapor form are transported to W-coil trap heated at 370 deg. C. Following the preconcentration step, the trap is heated to 895 deg. C; analyte species are revolatilized and transported to the flame-heated quartz atom cell where atomization and the formation of signal take place. The experimental parameters were optimized both for trap and no-trap studies. The most important experimental parameters are concentrations of HCl and NaBH{sub 4} solutions, H{sub 2} and Ar gas flow rates, and collection and revolatilization temperatures of W-coil. Accuracy was tested using a certified reference material, waste water EU-L-1. Limit of detection for the system is 16 ng l{sup -1} using a sample of 36 ml collected in 4.0 min. Enhancement factor in sensitivity was 17.

  18. Determination of uranium and thorium using gamma spectrometry: A pilot study

    Energy Technology Data Exchange (ETDEWEB)

    Olivares, D.M.M.; Koch, E.S.; Manso Guevara, M.V.; Garcia Velasco, F., E-mail: diango.mo87@gmail.com [Universidade Estadual de Santa Cruz (UNESC), Ilhéus, BA (Brazil)

    2017-07-01

    This paper presents the results of a pilot experiment aimed at standardizing procedures for the CPqCTR/UESC Gamma Spectrometry Laboratory (LEG) for the quantification of natural radioactive elements in solid environmental samples. The concentrations of {sup 238}U, {sup 232}Th and {sup 40}K in two sediment matrix belonging to the Caetité region were determined, by using the absolute method with uncertainties about 5%. The results were obtained using gamma spectrometry with a high-resolution p-type HPGe detector. As a closure, the absorbed dose, radium equivalent activity and the annual effective dose were calculated. (author)

  19. Determination of uranium and thorium using gamma spectrometry: a pilot study

    Science.gov (United States)

    Olivares, D. M. M.; Koch, E. S.; Guevara, M. V. M.; Velasco, F. G.

    2018-03-01

    This paper presents the results of a pilot experiment aimed at standardizing procedures for the CPqCTR/UESC Gamma Spectrometry Laboratory (LEG) for the quantification of natural radioactive elements in solid environmental samples. The concentrations of 238U, 232Th and 40K in two sediment matrix belonging to the Caetité region were determined, by using the absolute method with uncertainties about 5%. The results were obtained using gamma spectrometry with a high-resolution p-type HPGe detector. As a closure, the absorbed dose, radium equivalent activity and the annual effective dose were calculated.

  20. Standard addition strip for quantitative electrostatic spray ionization mass spectrometry analysis: determination of caffeine in drinks.

    Science.gov (United States)

    Tobolkina, Elena; Qiao, Liang; Roussel, Christophe; Girault, Hubert H

    2014-12-01

    Standard addition strips were prepared for the quantitative determination of caffeine in different beverages by electrostatic spray ionization mass spectrometry (ESTASI-MS). The gist of this approach is to dry spots of caffeine solutions with different concentrations on a polymer strip, then to deposit a drop of sample mixed with an internal standard, here theobromine on each spot and to measure the mass spectrometry signals of caffeine and theobromine by ESTASI-MS. This strip approach is very convenient and provides quantitative analyses as accurate as the classical standard addition method by MS or liquid chromatography. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Total cholesterol in serum determined by isotope dilution/mass spectrometry, with liquid-chromatographic separation

    International Nuclear Information System (INIS)

    Takatsu, Akiko; Nishi, Sueo

    1988-01-01

    We describe an accurate, precise method for determination of total serum cholesterol by isotope dilution/mass spectrometry (IDMS) with liquid chromatographic separation. After adding [3,4- 13 C] cholesterol to serum and hydrolyzing the cholesterol esters, we extract the total cholesterol. High-performance liquid chromatography (HPLC) is used to separate the extracted cholesterol for measurement by electron-impact mass spectrometry with use of a direct-insertion device. To evaluate the specificity and the accuracy of this method, we also studied the conventional IDMS method, which involves converting cholesterol to the trimethylsilyl ether and assay by gas chromatography-mass spectrometry with use of a capillary column. The coefficient of variation for the HPLC method was a little larger than for the conventional method, but mean values by each method agreed within 1% for all sera tested. (author)

  2. Age determination of trace plutonium using liquid scintillation counting and α-spectrometry

    International Nuclear Information System (INIS)

    Chen Yan; Chang Zhiyuan; Zhao Yonggang; Li Jinghuai; Shu Fujun

    2010-01-01

    Liquid scintillation counting combined with α-spectrometry through measuring 241 Pu/ 241 Am ratio to determine the age of trace Pu was studied. The technique was explored for the age determination of nanogram grade Pu sample on the basis of Pu/Am separation. The ages of two Pu samples-one with known and the other with unknown age were determined by the method. The determined age by the method is in agreement with the reference value. The established method for determining the age of trace Pu can be adopted in the verification activities of nuclear safeguards and nuclear arms control. (authors)

  3. Cloud point extraction and flame atomic absorption spectrometric determination of cadmium(II), lead(II), palladium(II) and silver(I) in environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Ghaedi, Mehrorang, E-mail: m_ghaedi@mail.yu.ac.ir [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of); Shokrollahi, Ardeshir [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of); Niknam, Khodabakhsh [Chemistry Department, Persian Gulf University, Bushehr (Iran, Islamic Republic of); Niknam, Ebrahim; Najibi, Asma [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of); Soylak, Mustafa [Chemistry Department, University of Erciyes, 38039 Kayseri (Turkey)

    2009-09-15

    The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of cadmium(II), lead(II), palladium(II) and silver(I). The analytical procedure involved the formation of understudy metals complex with bis((1H-benzo [d] imidazol-2yl)ethyl) sulfane (BIES), and quantitatively extracted to the phase rich in octylphenoxypolyethoxyethanol (Triton X-114) after centrifugation. Methanol acidified with 1 mol L{sup -1} HNO{sub 3} was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The concentration of BIES, pH and amount of surfactant (Triton X-114) was optimized. At optimum conditions, the detection limits of (3 sdb/m) of 1.4, 2.8, 1.6 and 1.4 ng mL{sup -1} for Cd{sup 2+}, Pb{sup 2+}, Pd{sup 2+} and Ag{sup +} along with preconcentration factors of 30 and enrichment factors of 48, 39, 32 and 42 for Cd{sup 2+}, Pb{sup 2+}, Pd{sup 2+} and Ag{sup +}, respectively, were obtained. The proposed cloud point extraction has been successfully applied for the determination of metal ions in real samples with complicated matrix such as radiology waste, vegetable, blood and urine samples.

  4. Cloud point extraction and flame atomic absorption spectrometric determination of cadmium(II), lead(II), palladium(II) and silver(I) in environmental samples

    International Nuclear Information System (INIS)

    Ghaedi, Mehrorang; Shokrollahi, Ardeshir; Niknam, Khodabakhsh; Niknam, Ebrahim; Najibi, Asma; Soylak, Mustafa

    2009-01-01

    The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of cadmium(II), lead(II), palladium(II) and silver(I). The analytical procedure involved the formation of understudy metals complex with bis((1H-benzo [d] imidazol-2yl)ethyl) sulfane (BIES), and quantitatively extracted to the phase rich in octylphenoxypolyethoxyethanol (Triton X-114) after centrifugation. Methanol acidified with 1 mol L -1 HNO 3 was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The concentration of BIES, pH and amount of surfactant (Triton X-114) was optimized. At optimum conditions, the detection limits of (3 sdb/m) of 1.4, 2.8, 1.6 and 1.4 ng mL -1 for Cd 2+ , Pb 2+ , Pd 2+ and Ag + along with preconcentration factors of 30 and enrichment factors of 48, 39, 32 and 42 for Cd 2+ , Pb 2+ , Pd 2+ and Ag + , respectively, were obtained. The proposed cloud point extraction has been successfully applied for the determination of metal ions in real samples with complicated matrix such as radiology waste, vegetable, blood and urine samples.

  5. Determination of boron in natural waters using atomic-absorption spectrometry with electrothermal atomization

    International Nuclear Information System (INIS)

    Usenko, S.I.; Prorok, M.M.

    1992-01-01

    A method of direct determination of boron in natural waters using atomic-absorption spectrometry with electrothermal atomization was developed. Concomitant elements Si, K, Mg, Na, present in natural waters in the concentration of 0.05-100 mg/cv 3 , do not produce effect on the value of boron atomic absorption. Boron determination limit constituted 0.02 mg/cm 3 for 25 ml of solution introduced

  6. Evaluation of a method for the determination of chromium in urine by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Garcia, M.; Sardinas, O.; Castaneda, I.; Sanchez, R.

    1990-01-01

    A method for the determination of chromium in urine by atomic absorption spectrometry, using electrothermic atomization with pyrolytic graphite tubes, is proposed. The determinations are performed by standard addition. The method is applicable to biologic monitoring of populations with different degrees of exposition. It is also used in the analysis of chromium in sediments. Results of chromium in urine of a population group non-exposed to the metal are presented. 11 refs

  7. Determination of static and dynamic reactivity effects in KNK II

    International Nuclear Information System (INIS)

    Essig, C.

    1987-11-01

    In the frame of a pre-study of the KNK II test program two series of experiments related to inherent safety characteristics of sodium cooled breeder reactors have been elaborated, which are one basis for the performance of experiments of the Loss Of Flow (LOF) type and the Loss Of Heat Sink (LOHS) type. Tests of this type at KNK II would -different from the earlier tests at RAPSODIE and EBR-II- provide a demonstration of the inherently safe performance in case of a significantly non-zero Doppler effect. With a suitable execution, the foreseen series of experiments allow, as explained in this report, a substantial separation of the reactivity contributions and the determination of reactivity effects, i.e. the time constants of the recouplings. The performance and evaluation of these experiments with respect to the inherent safety potential will once more underline the distinguished role of KNK II for the development of fast breeders [de

  8. Speciation of Mn(II), Mn(VII) and total manganese in water and food samples by coprecipitation-atomic absorption spectrometry combination

    International Nuclear Information System (INIS)

    Citak, Demirhan; Tuzen, Mustafa; Soylak, Mustafa

    2010-01-01

    A speciation procedure based on the coprecipitation of manganese(II) with zirconium(IV) hydroxide has been developed for the investigation of levels of manganese species. The determination of manganese levels was performed by flame atomic absorption spectrometry (FAAS). Total manganese was determined after the reduction of Mn(VII) to Mn(II) by ascorbic acid. The analytical parameters including pH, amount of zirconium(IV), sample volume, etc., were investigated for the quantitative recoveries of manganese(II). The effects of matrix ions were also examined. The recoveries for manganese(II) were in the range of 95-98%. Preconcentration factor was calculated as 50. The detection limit for the analyte ions based on 3 sigma (n = 21) was 0.75 μg L -1 for Mn(II). The relative standard deviation was found to be lower than 7%. The validation of the presented procedure was performed by analysis of certified reference material having different matrices, NIST SRM 1515 (Apple Leaves) and NIST SRM 1568a (Rice Flour). The procedure was successfully applied to natural waters and food samples.

  9. Chiral recognition and determination of enantiomeric excess by mass spectrometry: A review

    International Nuclear Information System (INIS)

    Yu, Xiangying; Yao, Zhong-Ping

    2017-01-01

    Chiral analysis is of great importance to fundamental and applied research in chemical, biological and pharmaceutical sciences. Due to the superiority of mass spectrometry (MS) over other analytical methods in terms of speed, specificity and sensitivity, chiral analysis by MS has attracted much interest in recent years. Chiral analysis by MS typically involves introduction of a chiral selector to form diastereomers with analyte enantiomers, and comparison of the behaviors of diastereomers in MS. Chiral differentiation can be achieved by comparing the relative abundances of diastereomers, the thermodynamic or kinetic constants of ion-molecule reactions of diastereomers in the gas phase, the dissociation of diastereomers in MS/MS, or the mobility of diastereomers in ion mobility mass spectrometry. In this review, chiral recognition and determination of enantiomeric excess by these chiral MS methods were summarized, and the prospects of chiral analysis by MS were discussed. - Highlights: • Both chiral recognition and determination of enantiomeric excess by mass spectrometry are systematically reviewed. • Classification is based on the behavioral differences of diastereomers formed between chiral analytes and chiral selectors. • Development of ion mobility mass spectrometry for chiral differentiation is covered. • Various methods are highlighted and compared.

  10. Chiral recognition and determination of enantiomeric excess by mass spectrometry: A review

    Energy Technology Data Exchange (ETDEWEB)

    Yu, Xiangying [College of Pharmacy, Jinan University, Guangzhou 510632, Guangdong (China); State Key Laboratory of Chinese Medicine and Molecular Pharmacology (Incubation) and Shenzhen Key Laboratory of Food Biological Safety Control, Shenzhen Research Institute of Hong Kong Polytechnic University, Shenzhen 518057 (China); Yao, Zhong-Ping, E-mail: zhongping.yao@polyu.edu.hk [State Key Laboratory of Chinese Medicine and Molecular Pharmacology (Incubation) and Shenzhen Key Laboratory of Food Biological Safety Control, Shenzhen Research Institute of Hong Kong Polytechnic University, Shenzhen 518057 (China); Key Laboratory of Natural Resources of Changbai Mountain and Functional Molecules (Yanbian University), Ministry of Education, Yanji 133002, Jilin (China); State Key Laboratory of Chirosciences, Food Safety and Technology Research Centre and Department of Applied Biology and Chemical Technology, The Hong Kong Polytechnic University, Hung Hom, Kowloon, Hong Kong Special Administrative Region (China)

    2017-05-22

    Chiral analysis is of great importance to fundamental and applied research in chemical, biological and pharmaceutical sciences. Due to the superiority of mass spectrometry (MS) over other analytical methods in terms of speed, specificity and sensitivity, chiral analysis by MS has attracted much interest in recent years. Chiral analysis by MS typically involves introduction of a chiral selector to form diastereomers with analyte enantiomers, and comparison of the behaviors of diastereomers in MS. Chiral differentiation can be achieved by comparing the relative abundances of diastereomers, the thermodynamic or kinetic constants of ion-molecule reactions of diastereomers in the gas phase, the dissociation of diastereomers in MS/MS, or the mobility of diastereomers in ion mobility mass spectrometry. In this review, chiral recognition and determination of enantiomeric excess by these chiral MS methods were summarized, and the prospects of chiral analysis by MS were discussed. - Highlights: • Both chiral recognition and determination of enantiomeric excess by mass spectrometry are systematically reviewed. • Classification is based on the behavioral differences of diastereomers formed between chiral analytes and chiral selectors. • Development of ion mobility mass spectrometry for chiral differentiation is covered. • Various methods are highlighted and compared.

  11. Selection of an analytical line for determining lithium in aluminum alloys by laser induced breakdown spectrometry

    International Nuclear Information System (INIS)

    Lednev, V.N.; Yakovlev, A.V.; Labutin, T.A.; Popov, A.M.; Zorov, N.B.

    2007-01-01

    Possibilities for determining lithium in aluminum alloys by laser spark spectrometry are studied. The optimum conditions for registering the emission signal of lithium at which the effect of the continuous background radiation of the laser plasma attains a minimum are found. The possibility of determining lithium by laser spark spectrometry using the spectral line at 610 nm is studied for the first time. A comparison of the detection limits and sensitivities of determining lithium by emission its lines at 610 and 671 nm has indicated the advisability of using the line 610 nm for the studied alloys. The detection limit calculated using the 3σ test was found to be 230 ppm (610 nm) and 870 ppm (671 nm) [ru

  12. Determining activity of 40K with disturbing from 228Ra by γ spectrometry

    International Nuclear Information System (INIS)

    Su Qiong

    1997-09-01

    The measurement methods and some viewpoints for processing data about determining activities in a reference material are reported (The Laboratory of Industrial Hygiene Ministry have a hand in the determining). The measurement and correct problems of determining activity of 40 K with disturbing from 228 Ra by γ spectrometry, which were neglected in the past a lot of measurement, are especially described. It is pointed out that if the correct is neglected then the value of 40 K in the current reference material, in that activities of both 22 '8Ra and 40 K are matched, will be determined with system error of about 20%. (14 refs., 3 tabs.)

  13. Dispersive liquid-liquid microextraction for simultaneous determination of cadmium, cobalt, lead and nickel in water samples by inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Dos Santos Silva, E.; Correia, L.O.; Dos Santos, L.O.; Dos Santos Vieira, E.V.; Lemos, V.A.

    2012-01-01

    We report on a new method for the dispersive liquid-liquid microextraction of Cd(II), Co(II), Pb(II) and Ni (II) from water samples prior to their simultaneous determination by inductively coupled plasma optical emission spectrometry (ICP-OES). The procedure is based on the injection of a ternary solvent system composed of appropriate quantities of extraction solvent (trichloroethylene), dispersive solvent (ethanol), and the chelating reagent 2-(2'-benzothiazolylazo)-p-cresol into the sample solution. The solution turns turbid immediately after injection, and the analytes are extracted into the droplets of the organic phase which was dried and dissolved in a mixture of Triton X-114, nitric acid, and ethanol. The metal ions in this mixture were quantified by ICP-OES. The detection limits under optimized conditions are 0.2, 0.3, 0.2 and 0.7 μg L -1 for Cd(II), Co(II), Pb(II) and Ni(II), respectively. The enrichment factors were also calculated for Cd (13), Co (11), Pb (11) and Ni (8). The procedure was applied to the determination of cadmium, cobalt, lead and nickel in certified reference material (waterway sediment) and water samples. (author)

  14. Determination of methylmercury by electrothermal atomic absorption spectrometry using headspace single-drop microextraction with in situ hydride generation

    Energy Technology Data Exchange (ETDEWEB)

    Gil, Sandra [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Universidad de Vigo, Facultad de Ciencias (Quimica), As Lagoas-Marcosende s/n, 36200 Vigo (Spain); Fragueiro, Sandra [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Universidad de Vigo, Facultad de Ciencias (Quimica), As Lagoas-Marcosende s/n, 36200 Vigo (Spain); Lavilla, Isela [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Universidad de Vigo, Facultad de Ciencias (Quimica), As Lagoas-Marcosende s/n, 36200 Vigo (Spain); Bendicho, Carlos [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Universidad de Vigo, Facultad de Ciencias (Quimica), As Lagoas-Marcosende s/n, 36200 Vigo (Spain)]. E-mail: bendicho@uvigo.es

    2005-01-10

    A new method is proposed for preconcentration and matrix separation of methylmercury prior to its determination by electrothermal atomic absorption spectrometry (ETAAS). Generation of methylmercury hydride (MeHgH) from a 5-ml solution is carried out in a closed vial and trapped onto an aqueous single drop (3-{mu}l volume) containing Pd(II) or Pt(IV) (50 and 10 mg/l, respectively). The hydrogen evolved in the headspace (HS) after decomposition of sodium tetrahydroborate (III) injected for hydride generation caused the formation of finely dispersed Pd(0) or Pt(0) in the drop, which in turn, were responsible for the sequestration of MeHgH. A preconcentration factor of ca. 40 is achieved with both noble metals used as trapping agents. The limit of detection of methylmercury was 5 and 4 ng/ml (as Hg) with Pd(II) or Pt(IV) as trapping agents, and the precision expressed as relative standard deviation was about 7%. The preconcentration system was fully characterised through optimisation of the following variables: Pd(II) or Pt(IV) concentration in the drop, extraction time, pH of the medium, temperatures of both sample solution and drop, concentration of salt in the sample solution, sodium tetrahydroborate (III) concentration in the drop and stirring rate. The method has been successfully validated against two fish certified reference materials (CRM 464 tuna fish and CRM DORM-2 dogfish muscle) following selective extraction of methylmercury in 2 mol/l HCl medium.

  15. Determination of methylmercury by electrothermal atomic absorption spectrometry using headspace single-drop microextraction with in situ hydride generation

    International Nuclear Information System (INIS)

    Gil, Sandra; Fragueiro, Sandra; Lavilla, Isela; Bendicho, Carlos

    2005-01-01

    A new method is proposed for preconcentration and matrix separation of methylmercury prior to its determination by electrothermal atomic absorption spectrometry (ETAAS). Generation of methylmercury hydride (MeHgH) from a 5-ml solution is carried out in a closed vial and trapped onto an aqueous single drop (3-μl volume) containing Pd(II) or Pt(IV) (50 and 10 mg/l, respectively). The hydrogen evolved in the headspace (HS) after decomposition of sodium tetrahydroborate (III) injected for hydride generation caused the formation of finely dispersed Pd(0) or Pt(0) in the drop, which in turn, were responsible for the sequestration of MeHgH. A preconcentration factor of ca. 40 is achieved with both noble metals used as trapping agents. The limit of detection of methylmercury was 5 and 4 ng/ml (as Hg) with Pd(II) or Pt(IV) as trapping agents, and the precision expressed as relative standard deviation was about 7%. The preconcentration system was fully characterised through optimisation of the following variables: Pd(II) or Pt(IV) concentration in the drop, extraction time, pH of the medium, temperatures of both sample solution and drop, concentration of salt in the sample solution, sodium tetrahydroborate (III) concentration in the drop and stirring rate. The method has been successfully validated against two fish certified reference materials (CRM 464 tuna fish and CRM DORM-2 dogfish muscle) following selective extraction of methylmercury in 2 mol/l HCl medium

  16. A new atomization cell for trace metal determinations by tungsten coil atomic spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Donati, G.L., E-mail: georgedonati@yahoo.com.br [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Wildman, R.B.; Jones, B.T. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States)

    2011-02-28

    A new metallic atomization cell is used for trace metal determinations by tungsten coil atomic absorption spectrometry and tungsten coil atomic emission spectrometry. Different protecting gas mixtures are evaluated to improve atomic emission signals. Ar, N{sub 2}, CO{sub 2} and He are used as solvents, and H{sub 2} and C{sub 2}H{sub 2} as solutes. A H{sub 2}/Ar mixture provided the best results. Parameters such as protecting gas flow rate and atomization current are also optimized. The optimal conditions are used to determine the figures of merit for both methods and the results are compared with values found in the literature. The new cell provides a better control of the radiation reaching the detector and a small, more isothermal environment around the atomizer. A more concentrated atomic cloud and a smaller background signal result in lower limits of detection using both methods. Cu (324.7 nm), Cd (228.8 nm) and Sn (286.3 nm) determined by tungsten coil atomic absorption spectrometry presented limits of detection as low as 0.6, 0.1, and 2.2 {mu}g L{sup -1}, respectively. For Cr (425.4 nm), Eu (459.4 nm) and Sr (460.7 nm) determined by tungsten coil atomic emission spectrometry, limits of detection of 4.5, 2.5, and 0.1 {mu}g L{sup -1} were calculated. The method is used to determine Cu, Cd, Cr and Sr in a water standard reference material. Results for Cu, Cd and Cr presented no significant difference from reported values in a 95% confidence level. For Sr, a 113% recovery was obtained.

  17. Determination of Cd in urine by cloud point extraction-tungsten coil atomic absorption spectrometry.

    Science.gov (United States)

    Donati, George L; Pharr, Kathryn E; Calloway, Clifton P; Nóbrega, Joaquim A; Jones, Bradley T

    2008-09-15

    Cadmium concentrations in human urine are typically at or below the 1 microgL(-1) level, so only a handful of techniques may be appropriate for this application. These include sophisticated methods such as graphite furnace atomic absorption spectrometry and inductively coupled plasma mass spectrometry. While tungsten coil atomic absorption spectrometry is a simpler and less expensive technique, its practical detection limits often prohibit the detection of Cd in normal urine samples. In addition, the nature of the urine matrix often necessitates accurate background correction techniques, which would add expense and complexity to the tungsten coil instrument. This manuscript describes a cloud point extraction method that reduces matrix interference while preconcentrating Cd by a factor of 15. Ammonium pyrrolidinedithiocarbamate and Triton X-114 are used as complexing agent and surfactant, respectively, in the extraction procedure. Triton X-114 forms an extractant coacervate surfactant-rich phase that is denser than water, so the aqueous supernatant is easily removed leaving the metal-containing surfactant layer intact. A 25 microL aliquot of this preconcentrated sample is placed directly onto the tungsten coil for analysis. The cloud point extraction procedure allows for simple background correction based either on the measurement of absorption at a nearby wavelength, or measurement of absorption at a time in the atomization step immediately prior to the onset of the Cd signal. Seven human urine samples are analyzed by this technique and the results are compared to those found by the inductively coupled plasma mass spectrometry analysis of the same samples performed at a different institution. The limit of detection for Cd in urine is 5 ngL(-1) for cloud point extraction tungsten coil atomic absorption spectrometry. The accuracy of the method is determined with a standard reference material (toxic metals in freeze-dried urine) and the determined values agree with

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-10-17

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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  20. Determination of Uranium plus Plutonium by Alpha spectrometry in different matrix

    International Nuclear Information System (INIS)

    Equillor, Hugo E.; Campos, Juan M.

    2011-01-01

    Usually, the determination of alpha emitters by alpha spectrometry is performed with a prior purification of each of the elements to be quantified. In this work, a methodology for the determination of uranium and plutonium isotopes as jointly described, in order to improve analytical processing times and measurement. The method includes purifying uranium and plutonium, and the subsequent electrodeposition for alpha spectrometry measurement. The technique is based on the use of TBP (tributyl phosphate) as extractant and easy to obtain reactants. It is applicable to various matrices, including water, filters and soils. In the conditions described, is applied to small aliquots of approximately 0.5 g of solid. The technique produces high quality electrodeposits. (authors) [es

  1. Speciation of iron (II) and (III) by using solvent extraction and flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Yaman, Mehmet; Kaya, Gokce

    2005-01-01

    A method for speciation, preconcentration and separation of Fe 2+ and Fe 3+ in different matrices was developed using solvent extraction and flame atomic absorption spectrometry. PAN as complexing reagent for Fe 2+ and chloroform as organic solvent were used. The complex of Fe 2+ -PAN was extracted into chloroform phase in the pH range of 0.75-4.0 and Fe 3+ remains in water phase in the pH range 0.75-1.25. The optimum conditions for maximum recovery of Fe 2+ and minimum recovery of Fe 3+ were determined as pH = 1, the stirring time of 20 min, the PAN amount of 0.5 mg and chloroform volume of 8 mL. The developed method was applied to the determination of Fe 2+ and Fe 3+ in tea infusion, fruit juice, cola and pekmez. It is seen that there is high bioavailable iron (Fe 2+ ) in pekmez. The developed method is sensitive, simple and need the shorter time in comparison with other similar studies

  2. Mass determination of U-233 and Pu-239 by gamma spectrometry technique

    International Nuclear Information System (INIS)

    Moraes, M.A.P.V. de; Pugliesi, R.

    1988-09-01

    The gamma spectrometry technique has been used for masses determinations of uranium-233 and plutonium-239, granted by AERE-HARWELL. A high purity Ge semicondutor detector was used and the total efficiency curve was obtained for the counting system in the energy range 13 KeV to 135 KeV. The calculated values for the masses compared with that obtained by means of gravimetry technique. (author) [pt

  3. Determination of ketone bodies in blood by headspace gas chromatography-mass spectrometry

    DEFF Research Database (Denmark)

    Holm, Karen Marie Dollerup; Linnet, Kristian; Rasmussen, Brian Schou

    2010-01-01

    A gas chromatography-mass spectrometry (GC-MS) method for determination of ketone bodies (ß-hydroxybutyrate, acetone, and acetoacetate) in blood is presented. The method is based on enzymatic oxidation of D-ß-hydroxybutyrate to acetoacetate, followed by decarboxylation to acetone, which...... was quantified by the use of headspace GC-MS using acetone-(13)C(3) as an internal standard. The developed method was found to have intra- and total interday relative standard deviations

  4. Determination of five trace elements in leaves in Nanfang sweet orange by flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Li Fangqing

    2006-01-01

    The five trace elements of copper, zinc, manganese, iron and cobalt in leaves of Nanfang sweet orange are determined by flame atomic absorption spectrometry. The technique is simple, precise and sensitive. The effect of the type of digesting solution (mixed acid), the ratio of mixed acid, the volume of digesting solution and the time of digesting are investigated in details. The results show that leaves of Nanfang sweet orange contain higher amount of iron and zinc. (authors)

  5. Determination of lead and cadmium in urine by electrothermal atomization atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Vasil'eva, L.A.; Grinshtejn, I.L.; Gucher, Sh.; Izgi, B.

    2008-01-01

    The applicability of a DETATA sorbent to the preconcentration of lead and cadmium followed by the determination of these elements in urine using atomic absorption spectrometry with electrothermal atomization was demonstrated. After preconcentration by a factor of 10, the limits of detection were 0.01 and 0.2 μg/l for cadmium and lead, respectively. The accuracy of the results was supported by the analysis of Seronorm TM Trace Elements Urine Batch no.101021 [ru

  6. 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...

  7. Classification of wine by determination of bioactive phenolic compounds using high resolution mass spectrometry

    OpenAIRE

    Ivanova, Violeta; Dimovska, Violeta; Mitrev, Sasa; Gulaboski, Rubin; Bogeva, Elena; Petruseva, Dragana; Causon, Tim; Hann, Stephan

    2016-01-01

    In this project proposal, metabolomic fingerprinting of wine samples will be examined using high performance liquid chromatography combined with ion mobility quadruple time-of-flight mass spectrometry (HPLC–IMS-QTOF-MS) for the first time. Bioactive compounds in wines from various red and white varieties produced in Macedonia and Austria from different wine regions and different vintages will be determined for the first time using a non-targeted fingerprinting approach on this analytical plat...

  8. Determination of trace amounts of selenium in minerals and rocks by flemeless atomic-absorption spectrometry

    International Nuclear Information System (INIS)

    Capdevila, C.; Alduan, F.A.

    1980-01-01

    The determination of trace amounts of selenium in silicate rocks and feldspart by solvent extraction and graphite furnace atomic-absorption spectrometry has been studied. Sodium diethyl-ditiocarbamate and ammonium pyrrolidinedithiocarbamate have been tried as chelating agents. The best results are achieved when selenium is extracted into carbon tetrachloride as the sodium diethylditiocarbamate complex. The method allows to detect 0,75 ppm of selenium in the sample. Recoveries are about 100%. (author)

  9. Determination of the-230 on urine by means of alpha spectrometry

    International Nuclear Information System (INIS)

    1992-01-01

    The measurements of activity on urine samples are data very important to evaluation the internal doses. We have developed a radiochemistry method with the measure of Th-230 in urine. The method is based in the coprecipitation of the like phosphate the activity of sample is determined by alpha spectrometry. We use like tracer Th-234. The results show a recuperation between 65%-85%

  10. Regional differences in brain glucose metabolism determined by imaging mass spectrometry

    OpenAIRE

    André Kleinridders; Heather A. Ferris; Michelle L. Reyzer; Michaela Rath; Marion Soto; M. Lisa Manier; Jeffrey Spraggins; Zhihong Yang; Robert C. Stanton; Richard M. Caprioli; C. Ronald Kahn

    2018-01-01

    Objective: Glucose is the major energy substrate of the brain and crucial for normal brain function. In diabetes, the brain is subject to episodes of hypo- and hyperglycemia resulting in acute outcomes ranging from confusion to seizures, while chronic metabolic dysregulation puts patients at increased risk for depression and Alzheimer's disease. In the present study, we aimed to determine how glucose is metabolized in different regions of the brain using imaging mass spectrometry (IMS). Metho...

  11. Radioimmunoassay and chemical ionization/mass spectrometry compared for plasma cortisol determination

    International Nuclear Information System (INIS)

    Lindberg, C.; Johnson, S.; Hedner, P.; Gustafsson, A.

    1982-01-01

    A method is described for determination of cortisol in plasma and urine, based on chemical ionization/mass spectrometry with deuterium-labeled cortisol as the internal standard. The within-run precision (CV) was 2.5-5.7%, the between-run precision 4.6%. Results by this method were compared with those by a radioimmunological method (RIANEN Cortisol, New England Nuclear) for 395 plasma samples. The latter method gave significantly higher (approx. 25%) cortisol values

  12. Direct microcomputer controlled determination of zinc in human serum by flow injection atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Simonsen, Kirsten Wiese; Nielsen, Bent; Jensen, Arne

    1986-01-01

    A procedure is described for the direct determination of zinc in human serum by fully automated, microcomputer controlled flow injection atomic absorption spectrometry (Fl-AAS). The Fl system is pumpless, using the negative pressure created by the nebuliser. It only consists of a three-way valve......, programmable from the microcomputer, to control the sample volume. No pre-treatment of the samples is necessary. The limit of detection is 0.14 mg l–1, and only small amounts of serum (

  13. [Determination of mercury in Boletus impolitus by flow injection-atomic absorption spectrometry].

    Science.gov (United States)

    Li, Tao; Wang, Yuan-Zhong

    2008-04-01

    Various test conditions and effect factors for the determination of mercury by flow injection-atomic absorption spectrometry were discussed, and a method for the determination of mercury in Boletus impolitus has been developed. The linear range for mercury is 0-60 microg x L(-1). The relative standard deviation is less than 3.0%, and the recovery is 96%-107%. This method is simple, rapid and has been applied to the determination of mercury in Boletus impolitus samples with satisfactory results.

  14. Determination of B and Li in nuclear materials by secondary-ion mass spectrometry

    International Nuclear Information System (INIS)

    Eby, R.E.; Christie, W.H.

    1981-01-01

    Secondary ion mass spectrometry (SIMS) was used to perform mass and isotopic analysis for B and Li in samples that are not readily amenable to more conventional mass spectrometric techniques (e.g., surface ionization, electron impact, etc.). In this paper three specific applications of SIMS analysis to nuclear materials are discussed: first, the quantitative determination of B and its isotopic composition in borosilicate glasses; second, the determination of the isotopic composition of B and Li in irradiated nuclear-grade aluminum oxide/boron carbide composite pellets, and, lastly, the quantitative and isotopic determination of B and Li in highly radioactive solutions of unknown composition

  15. Determination of trace amounts of cerium in paint by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Wong, K.L.

    1981-01-01

    The determination of Ce in paint by inductively coupled plasma atomic emission spectrometry (ICP-OES) is described, and the detection limit of ICP-OES of 0.0004 ppM is compared with that of other methods. The effects of the major elemental components of paint, Si, Pb, Cr, and Na on the ICP-OES determination of Ce were studied. The interference of 400 ppM of the other ions on the determination of 10 ppM Ce was small (0 to 3% error). The method is applicable to the range of 0.2 to 700 ppM Ce

  16. Ultratrace determination of Pb, Se and As in wine samples by electrothermal vaporization inductively coupled plasma mass spectrometry

    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); de Loos-Vollebregt, M.T.C. [Delft University of Technology, Fac. Applied Sciences, Julianalaan 67, 2628 BC - Delft (Netherlands)

    2009-10-12

    The determination of Pb, Se and As in wine has a great interest due to health risks and legal requirements. To perform the analysis of wine, two considerations must be taken into account: (i) the low concentration level of the analytes; and (ii) the risk of interferences due to wine matrix components. The goal of this work is to evaluate electrothermal vaporization (ETV) sample introduction for ultratrace determination of Pb, Se and As in wine samples by inductively coupled plasma mass spectrometry (ICP-MS). The results obtained with ETV-ICP-MS were compared to those obtained with conventional liquid sample introduction in ICP-MS and electrothermal atomic absorption spectrometry (ETAAS). Analytical figures of merit of ETV sample introduction strongly depend on the amount of wine sample, on the modifier nature (i.e. Pd, ascorbic acid or citric acid) and concentration and on the temperature program. Wine matrix components exert a great influence on analyte transport efficiency. Due to this fact, the analysis of wine cannot be performed by means of external calibration but the standard addition methodology should be used. The determination of Pb and Se in wine by ETV-ICP-MS provides similar results as conventional liquid sample introduction ICP-MS. For As, the concentration values obtained with ETV sample introduction were between two and four times lower than with the conventional system. These differences are related to the lower intensity of polyatomic interferences (i.e. {sup 40}Ar{sup 35}Cl{sup +} vs. {sup 75}As{sup +}) obtained for ETV sample introduction when compared to the conventional system. Finally, no differences for Pb determination were observed between ETV sample introduction and ETAAS. Unfortunately, the limits of detection for As and Se in ETAAS were not low enough to quantify these elements in the wine samples tested.

  17. Ultratrace determination of Pb, Se and As in wine samples by electrothermal vaporization inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

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

    2009-01-01

    The determination of Pb, Se and As in wine has a great interest due to health risks and legal requirements. To perform the analysis of wine, two considerations must be taken into account: (i) the low concentration level of the analytes; and (ii) the risk of interferences due to wine matrix components. The goal of this work is to evaluate electrothermal vaporization (ETV) sample introduction for ultratrace determination of Pb, Se and As in wine samples by inductively coupled plasma mass spectrometry (ICP-MS). The results obtained with ETV-ICP-MS were compared to those obtained with conventional liquid sample introduction in ICP-MS and electrothermal atomic absorption spectrometry (ETAAS). Analytical figures of merit of ETV sample introduction strongly depend on the amount of wine sample, on the modifier nature (i.e. Pd, ascorbic acid or citric acid) and concentration and on the temperature program. Wine matrix components exert a great influence on analyte transport efficiency. Due to this fact, the analysis of wine cannot be performed by means of external calibration but the standard addition methodology should be used. The determination of Pb and Se in wine by ETV-ICP-MS provides similar results as conventional liquid sample introduction ICP-MS. For As, the concentration values obtained with ETV sample introduction were between two and four times lower than with the conventional system. These differences are related to the lower intensity of polyatomic interferences (i.e. 40 Ar 35 Cl + vs. 75 As + ) obtained for ETV sample introduction when compared to the conventional system. Finally, no differences for Pb determination were observed between ETV sample introduction and ETAAS. Unfortunately, the limits of detection for As and Se in ETAAS were not low enough to quantify these elements in the wine samples tested.

  18. Adsorption studies of Cd(II) onto Al{sub 2}O{sub 3}/Nb{sub 2}O{sub 5} mixed oxide dispersed on silica matrix and its on-line preconcentration and determination by flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mendonca Costa, Lucimara [Programa de Pos-Graduacao em Quimica da Universidade Federal de Alfenas, Rua Gabriel Monteiro da Silva, 700, Alfenas-MG, CEP 37130-000 (Brazil); Ribeiro, Emerson Schwingel [Instituto de Quimica, Universidade Federal do Rio de Janeiro, Rio de Janeiro-RJ, CEP 21941-909 (Brazil); Segatelli, Mariana Gava [Departamento de Quimica, Universidade Estadual de Londrina, Rod. Celso Garcia Cid, PR 445 Km 380, Campus Universitario, Londrina-PR, CEP 86051-990 (Brazil); Nascimento, Danielle Raphael do [Instituto de Quimica, Universidade Federal do Rio de Janeiro, Rio de Janeiro-RJ, CEP 21941-909 (Brazil); Midori de Oliveira, Fernanda [Departamento de Quimica, Universidade Estadual de Londrina, Rod. Celso Garcia Cid, PR 445 Km 380, Campus Universitario, Londrina-PR, CEP 86051-990 (Brazil); Tarley, Cesar Ricardo Teixeira, E-mail: tarley@uel.br [Programa de Pos-Graduacao em Quimica da Universidade Federal de Alfenas, Rua Gabriel Monteiro da Silva, 700, Alfenas-MG, CEP 37130-000 (Brazil); Departamento de Quimica, Universidade Estadual de Londrina, Rod. Celso Garcia Cid, PR 445 Km 380, Campus Universitario, Londrina-PR, CEP 86051-990 (Brazil)

    2011-05-15

    The present study describes the adsorption characteristic of Cd(II) onto Nb{sub 2}O{sub 5}/Al{sub 2}O{sub 3} mixed oxide dispersed on silica matrix. The characterization of the adsorbent has been carried out by infrared spectroscopy (IR), scanning electronic microscopy (SEM), energy dispersive spectroscopy (EDS), energy dispersive X-ray fluorescence analysis (EDXRF) and specific surface area (S{sub BET}). From batch experiments, adsorption kinetic of Cd(II) was described by a pseudo-second-order kinetic model. The Langmuir linear isotherm fitted to the experimental adsorption isotherm very well, and the maximum adsorption capacity was found to be 17.88 mg g{sup -1}. Using the effective material, a method for Cd(II) preconcentration at trace level was developed. The method was based on on-line adsorption of Cd(II) onto SiO{sub 2}/Al{sub 2}O{sub 3}/Nb{sub 2}O{sub 5} at pH 8.64, in which the quantitative desorption occurs with 1.0 mol L{sup -1} hydrochloric acid towards FAAS detector. The experimental parameters related to the system were studied by means of multivariate analysis, using 2{sup 4} full factorial design and Doehlert matrix. The effect of SO{sub 4}{sup 2-}, Cu{sup 2+}, Zn{sup 2+} and Ni{sup 2+} foreign ions showed no interference at 1:100 analyte:interferent proportion. Under the most favorable experimental conditions, the preconcentration system provided a preconcentration factor of 18.4 times, consumption index of 1.08 mL, sample throughput of 14 h{sup -1}, concentration efficiency of 4.35 min{sup -1}, linear range from 5.0 up to 35.0 {mu}g L{sup -1} and limits of detection and quantification of 0.19 and 0.65 {mu}g L{sup -1} respectively. The feasibility of the proposed method for Cd(II) determination was assessed by analysis of water samples, cigarette sample and certified reference materials TORT-2 (Lobster hepatopancreas) and DOLT-4 (Dogfish liver).

  19. Synchronous determination of mercury (II) and copper (II) based on quantum dots-multilayer film

    International Nuclear Information System (INIS)

    Ma Qiang; Ha Enna; Yang Fengping; Su Xingguang

    2011-01-01

    Graphical abstract: We developed a sensitive sensor for synchronous detection of Hg (II) and Cu (II) based on the quenchedand recovered PL intensity of QDs-multilayer films. Solutions containing Hg (II) or Cu (II) were used to quench the fluorescence of the QDs-multilayer films firstly. Then, glutathione (GSH) was used to remove Hg (II) or Cu (II) from the QDs-multilayer films due to stronger affinity of GSH-metal ions than that of QDs metal ions. Thus, the fluorescence of QDs-multilayer films was recovered. Highlights: → QDs-multilayer films were developed for synchronous detection of Hg (II) and Cu (II). → Hg (II) and Cu (II) could quench the photoluminescence of the QDs-multilayer films. → Glutathione was used to remove metal ions and recovery photoluminescence of QDs-multilayer films. - Abstract: A sensitive sensor for mercury (II) and copper (II) synchronous detection was established via the changed photoluminescence of CdTe quantum dots (QDs) multilayer films in this work. QDs were deposited on the quartz slides to form QDs-multilayer films by electrostatic interactions with poly(dimethyldiallyl ammonium chloride) (PDDA). Hg 2+ or Cu 2+ could quench the photoluminescence of the QDs-multilayer films, and glutathione (GSH) was used to remove Hg 2+ or Cu 2+ from QDs-multilayer films due to strong affinity of GSH-metal ions, which resulted in the recovered photoluminescence of QDs-multilayer films. There are good linear relationships between the metal ions concentration and the photoluminescence intensity of QDs in the quenched and recovered process. It was found that the Stern-Volmer constants for Hg 2+ are higher than that for Cu 2+ . Based on different quenching and recovery constant between Hg 2+ and Cu 2+ , the synchronous detection of Hg 2+ and Cu 2+ can be achieved. The linear ranges of this assay were obtained from 0.005 to 0.5 μM for Hg 2+ and from 0.01 to 1 μM for Cu 2+ , respectively. And the artificial water samples were determined by this

  20. Indigenous instrumentation for mass spectrometry: Part II - development of plasma source mass spectrometers. PD-5-3

    International Nuclear Information System (INIS)

    Nataraju, V.

    2007-01-01

    The growing demands from analytical community, for a precise isotope ratio and ultra trace concentration measurements, has lead to significant improvement in mass spectrometer instrumentation development with respect to sensitivity, detection limits, precision and accuracy. Among the many analytical techniques available, plasma source mass spectrometers like Inductively Coupled Plasma Mass Spectrometry (ICPMS), multi collector (MC) ICPMS and Glow Discharge Mass Spectrometry (GDMS), have matured into reliable tools for the above applications. Where as ICPMS is by far the most successful method for aqueous solutions, GDMS is being applied for bulk and impurity analysis of conducting as well non-conducting solids. VPID, BARC has been developing mass spectrometers for different inorganic applications of DAE users. Over the years expertise has been developed in all the aspects of mass spectrometry instrumentation. Part 1 of this indigenous instrumentation on mass spectrometry gives details of magnetic sector instruments with either EI or TI source for isotopic ratio analysis. The present paper is a continuation of that on plasma source and quadrupole mass spectrometers. This paper covers i) ICP-QMS, ii) MC-ICPMS, iii) GDMS and iv) QMS

  1. Determination of concentration of heavy metals (Pb, Cd, Fe) in animal tissues using atomic absorption spectrometry

    International Nuclear Information System (INIS)

    RAZAFINTSALAMA, V.T.

    2009-01-01

    Heavy metals are classified among the inorganic compounds. The latter type of metal is found in rocks, fertilizers, urban mud but may also originate from the atmospheric pollution. A particular characteristic of heavy metals is their bioaccumulation in the food chain. Therefore, lead and cadmium, which are classified as heavy metals may be easily found in animal products and can lead to food poisoning if their concentrations are higher than the maximum permissible values as requested by international agencies such as the c odex alimentarius . The values are set down and differ according to types of food for human consuption and the trading companies take action accordingly. Therefore, it is necessary to set up a quality control system through analytical laboratory measurements and testings. This study underlies the method of determination of lead, cadmium and iron in animal tissues by atomic absorption spectrometry. The results showed that the method is sensitive and reliable. For each analyte, the Z-score lies between -2 and 2, indicating that the method is working properly. The analytical results showed that: (i) only beef and chicken meats and beef liver contain lead [0,09μg.g - 1; 0,29μg.g - 1]. The limit value of 0,1μg.g - 1 is almost reached in beef and chicken meats, (ii) as far as cadmium is concerned, the five studied samples contain this analyte [0,02μg.g - 1; 0,9μg.g - 1]. Except the chicken liver of which the concentration (0,15μg.g - 1) exceeds the maximum permissible value (0,1μg.g - 1), the others are in conformity with the standards and appropriate to be consumed,(iii) iron is higher in the liver and kidney samples: beef liver 282mg.g - 1, chicken liver 250 mg.g - 1, pork kidney 247mg.g - 1. The study also showed that the calcium concentration in animal tissues is low and they can be classified as poor-calcium food. [fr

  2. Cadmium (II) imprinted 3-mercaptopropyltrimethoxysilane coated stir bar for selective extraction of trace cadmium from environmental water samples followed by inductively coupled plasma mass spectrometry detection

    International Nuclear Information System (INIS)

    Zhang Nan; Hu Bin

    2012-01-01

    Graphical abstract: Ion imprinted 3-mercaptopropyltrimethoxysilane (MPTS) coated stir bar for selective extraction of trace Cd(II). Highlights: ► Ion imprinted polymers were proposed as the coating for SBSE for the first time. ► Cd(II) imprinted MPTS-silica coating was prepared by a double-imprinting concept. ► A novel method of SBSE–ICP-MS was developed for the determination of Cd in waters. ► This method is rapid, selective, sensitive and applicable for determining trace Cd(II) in waters. - Abstract: Cd(II) imprinted 3-mercaptopropyltrimethoxysilane (MPTS)-silica coated stir bar was prepared by sol–gel technique combining with a double-imprinting concept for the first time and was employed for stir bar sorptive extraction (SBSE) of trace Cd(II) from water samples followed by inductively coupled plasma mass spectrometry (ICP-MS) detection. A tetramethoxysilane (TMOS) coating was first in situ created on the glass bar surface. Afterward, a sol solution containing MPTS as the functional precursor, ethanol as the solvent and both Cd(II) and surfactant micelles (cetyltrimethylammonium bromide, CTAB) as the template was again coated on the TMOS bar. The structures of the stir bar coating were characterized by FT-IR spectroscopy. Round-bottom vial was used for the extraction of Cd(II) by SBSE to avoid abrasion of stir bar coatings. The factors affecting the extraction of Cd(II) by SBSE such as pH, stirring rate and time, sample/elution volume and interfering ions have been investigated in detail, and the optimized experimental parameters were obtained. Under the optimized conditions, the adsorption capacities of non-imprinted and imprinted coating stir bars were found to be 0.5 μg and 0.8 μg bar −1 . The detection limit (3σ) based on three times standard deviations of the method blanks by 7 replicates was 4.40 ng L −1 and the relative standard deviation (RSD) was 3.38% (c = 1 μg L −1 , n = 7). The proposed method was successfully applied for the

  3. Cadmium (II) imprinted 3-mercaptopropyltrimethoxysilane coated stir bar for selective extraction of trace cadmium from environmental water samples followed by inductively coupled plasma mass spectrometry detection

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Nan [Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin, E-mail: binhu@whu.edu.cn [Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072 (China)

    2012-04-20

    Graphical abstract: Ion imprinted 3-mercaptopropyltrimethoxysilane (MPTS) coated stir bar for selective extraction of trace Cd(II). Highlights: Black-Right-Pointing-Pointer Ion imprinted polymers were proposed as the coating for SBSE for the first time. Black-Right-Pointing-Pointer Cd(II) imprinted MPTS-silica coating was prepared by a double-imprinting concept. Black-Right-Pointing-Pointer A novel method of SBSE-ICP-MS was developed for the determination of Cd in waters. Black-Right-Pointing-Pointer This method is rapid, selective, sensitive and applicable for determining trace Cd(II) in waters. - Abstract: Cd(II) imprinted 3-mercaptopropyltrimethoxysilane (MPTS)-silica coated stir bar was prepared by sol-gel technique combining with a double-imprinting concept for the first time and was employed for stir bar sorptive extraction (SBSE) of trace Cd(II) from water samples followed by inductively coupled plasma mass spectrometry (ICP-MS) detection. A tetramethoxysilane (TMOS) coating was first in situ created on the glass bar surface. Afterward, a sol solution containing MPTS as the functional precursor, ethanol as the solvent and both Cd(II) and surfactant micelles (cetyltrimethylammonium bromide, CTAB) as the template was again coated on the TMOS bar. The structures of the stir bar coating were characterized by FT-IR spectroscopy. Round-bottom vial was used for the extraction of Cd(II) by SBSE to avoid abrasion of stir bar coatings. The factors affecting the extraction of Cd(II) by SBSE such as pH, stirring rate and time, sample/elution volume and interfering ions have been investigated in detail, and the optimized experimental parameters were obtained. Under the optimized conditions, the adsorption capacities of non-imprinted and imprinted coating stir bars were found to be 0.5 {mu}g and 0.8 {mu}g bar{sup -1}. The detection limit (3{sigma}) based on three times standard deviations of the method blanks by 7 replicates was 4.40 ng L{sup -1} and the relative standard

  4. Determination of 239Pu and 240Pu isotope ratio for a nuclear bomb particle using X-ray spectrometry in conjunction with γ-ray spectrometry and non-destructive α-particle spectrometry

    International Nuclear Information System (INIS)

    Poellaenen, R.; Ruotsalainen, K.; Toivonen, H.

    2009-01-01

    A nuclear bomb particle from Thule containing Pu and U was analyzed using X-ray spectrometry in combination with γ-ray spectrometry and non-destructive α-spectrometry. The main objective was to investigate the possibility to determine the 239 Pu and 240 Pu isotope ratios. Previously, X-ray spectrometry together with the above-mentioned methods has been successfully applied for radiochemically processed samples, but not for individual particles. In the present paper we demonstrate the power of non-destructive analysis. The 239 Pu/( 239 Pu+ 240 Pu) atom ratio for the Thule particle was determined, using two different approaches, to be 0.93±0.07 and 0.91±0.05. These results are consistent with weapons-grade material and the results obtained by other investigators.

  5. KRAS G12C Drug Development: Discrimination between Switch II Pocket Configurations Using Hydrogen/Deuterium-Exchange Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lu, Jia; Harrison, Rane A.; Li, Lianbo; Zeng, Mei; Gondi, Sudershan; Scott, David; Gray, Nathanael S.; Engen, John R.; Westover, Kenneth D. (NEU); (DFCI); (UTSMC); (Harvard-Med)

    2017-09-01

    KRAS G12C, the most common RAS mutation found in non-small-cell lung cancer, has been the subject of multiple recent covalent small-molecule inhibitor campaigns including efforts directed at the guanine nucleotide pocket and separate work focused on an inducible pocket adjacent to the switch motifs. Multiple conformations of switch II have been observed, suggesting that switch II pocket (SIIP) binders may be capable of engaging a range of KRAS conformations. Here we report the use of hydrogen/deuterium-exchange mass spectrometry (HDX MS) to discriminate between conformations of switch II induced by two chemical classes of SIIP binders. We investigated the structural basis for differences in HDX MS using X-ray crystallography and discovered a new SIIP configuration in response to binding of a quinazoline chemotype. These results have implications for structure-guided drug design targeting the RAS SIIP.

  6. Determination of {sup 126}Sn half-life from ICP-MS and gamma spectrometry measurements

    Energy Technology Data Exchange (ETDEWEB)

    Bienvenu, P.; Arnal, N.; Comte, J. [CEA Cadarache DEN/DEC/SA3C/LARC, Paul Lez Durance (France); Ferreux, L.; Lepy, M.C.; Be, M.M. [CEA Saclay LIST LNE/LNHB, Gif sur Yvette (France); Andreoletti, G. [AREVA Cogema SL/UP2-800, Beaumont Hague (France)

    2009-07-01

    A new value of {sup 126}Sn half-life was determined by combination of inductively coupled plasma-mass spectrometry (ICP-MS) and gamma spectrometry measurements on purified sample solutions collected from nuclear fuel reprocessing. {sup 126}Sn was isolated through dissolution of fission product precipitates and liquid-liquid extraction with N-benzoyl-N-phenyl-hydroxylamine (BPHA). The abundance of {sup 126}Sn atoms together with the absence of interfering species in the analysed solutions made it possible to measure both mass concentration and nuclide activity with high precision and accuracy. This led to a {sup 126}Sn half-life value of 1.980 (57) x 10{sup 5} a. (orig.)

  7. Determination of clarithromycin in human plasma by liquid chromatography-electrospray ionization tandem mass spectrometry.

    Science.gov (United States)

    Jiang, Yao; Wang, Jiang; Li, Hao; Wang, Yingwu; Gu, Jingkai

    2007-03-12

    A rapid and sensitive method has been developed for the determination of clarithromycin in human plasma with liquid chromatography-tandem mass spectrometry. Clarithromycin and the internal standard, telmisartan were precipitated from the matrix (50 microl) with 200 microl acetonitrile and separated by HPLC using formic acid:10 mM ammonium acetate:methanol (1:99:400, v/v/v) as the mobile phase. The assay based on detection by electrospray positive ionization mass spectrometry in the multiple-reaction monitoring mode was finished within 2.4 min. Linearity was over the concentration range 10-5000 ng/ml with a limit of detection of 0.50 ng/ml. Intra- and inter-day precision measured as relative standard deviation were bioequivalence study of two tablet formulations of clarithromycin.

  8. Determination of the self-attenuation correction factor for environmental samples analysis in gamma spectrometry

    International Nuclear Information System (INIS)

    Santos, Talita O.; Rocha, Zildete; Knupp, Eliana A.N.; Kastner, Geraldo F.; Oliveira, Arno H. de; Oliveira, Arno H. de

    2015-01-01

    Gamma spectrometry technique has been used in order to obtain the activity concentrations of natural and artificial radionuclides in environmental samples of different origins, compositions and densities. These samples characteristics may influence the calibration condition by the self-attenuation effect. The sample density has been considered the most important factor. For reliable results, it is necessary to determine self-attenuation correction factor which has been subject of great interest due to its effect on activity concentration. In this context, the aim of this work is to show the calibration process considering the correction by self-attenuation in the evaluation of the concentration of each radionuclide to a gamma HPGEe detector spectrometry system. (author)

  9. Time sequence determination of parent–daughter radionuclides using gamma-spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Burnett, J. L.; Britton, R. E.; Abrecht, D. G.; Davies, A. V.

    2017-05-06

    The acquisition of time-stamped list (TLIST) data provides additional information useful to gamma-spectrometry analysis. A novel technique is described that uses non-linear least-squares fitting and the Levenberg-Marquardt algorithm to simultaneously determine parent-daughter atoms from time sequence measurements of only the daughter radionuclide. This has been demonstrated for the radioactive decay of short-lived radon progeny (214Pb/214Bi, 212Pb/212Bi) described using the Bateman first-order differential equation. The calculated atoms are in excellent agreement with measured atoms, with a difference of 1.3 – 4.8% for parent atoms and 2.4% - 10.4% for daughter atoms. Measurements are also reported with reduced uncertainty. The technique has potential to redefine gamma-spectrometry analysis.

  10. Determination of albendazole sulfoxide in human plasma by using liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Saraner, Nihal; Özkan, Güler Yağmur; Güney, Berrak; Alkan, Erkin; Burul-Bozkurt, Nihan; Sağlam, Onursal; Fikirdeşici, Ezgi; Yıldırım, Mevlüt

    2016-06-01

    A rapid, simple and sensitive method was developed and validated using liquid chromatography-tandem mass spectrometry (LC-MS/MS) for determination of albendazole sulfoxide (ABZOX) in human plasma. The plasma samples were extracted by protein precipitation using albendazole sulfoxide-d3 as internal standard (IS). The chromatographic separation was performed on Waters Xbridge C18Column (100×4.6mm, 3.5μm) with a mobile phase consisting of ammonia solution, water and methanol at a flow rate of 0.70mL/min. ABZOX was detected and identified by mass spectrometry with electrospray ionization (ESI) in positive ion and multiple-reaction monitoring (MRM) mode. The method was linear in the range of 3-1500ng/mL for ABZOX. This method was successfully applied to the bioequivalence study in human plasma samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Determination of molybdenum in natural waters by laser thermal-lens spectrometry

    International Nuclear Information System (INIS)

    Proskurnin, M.A.; Abroskin, A.G.; Artemova, S.I.; Belyaeva, T.V.; Ivanova, E.K.

    1992-01-01

    As before, the determination of nanogram quantities of heavy metals from small sample volumes of natural water represents an acute problem. This task has been solved more or less successfully by the use of different and sufficiently developed physicochemical methods. In most cases the determination requires a 100-fold preconcentration of the component determined (for instance, when using atomic absorption spectrometry). This significant disadvantage can be avoided by the use of thermal-lens laser spectrometry (TLS); some alternatives of the method have already found applications in analytical practice. The objective of the present study has been to investigate the optimum conditions for the determination of molybdenum in natural waters from small sample volumes by TLS. The resulting method based on the reaction with thiocyanate ions in the presence of ascorbic acid, has a detection limit of 19 pg/ml. Masking of iron(III) with a 1000-fold excess of tartrate ions has been proposed and it has been shown that a 10-fold excess of iron does not interfere in the determination of molybdenum. The procedure has been applied to the determination of molybdenum in drinking and natural waters

  12. Determination of Uranium, Thorium and Radium 226 in Zircon containig sands by alpha spectrometry

    International Nuclear Information System (INIS)

    Spezzano, P.

    1985-01-01

    The industrial utilization of Zircon sands for the production of refractories presents radiological problems owing to the risk of inhalation of Uranium, Thorium and their decay products, present in high concentrations in such materials. A method of analysis was realized for the determination of Uranium, Thorium and Radium-226 in Zircon sands, including the total dissolution of the sample, radiochemical separation and final measurement by alpha spectrometry with surface barrier detector. The concentrations of the main alpha-emitting radionuclides presents in two samples of Zircon sands have been determined and the possibility of disequilibrium along the decay series has been pointed out

  13. Determination of the neutron activation profile of core drill samples by gamma-ray spectrometry.

    Science.gov (United States)

    Gurau, D; Boden, S; Sima, O; Stanga, D

    2018-04-01

    This paper provides guidance for determining the neutron activation profile of core drill samples taken from the biological shield of nuclear reactors using gamma spectrometry measurements. Thus, it provides guidance for selecting a model of the right form to fit data and using least squares methods for model fitting. The activity profiles of two core samples taken from the biological shield of a nuclear reactor were determined. The effective activation depth and the total activity of core samples along with their uncertainties were computed by Monte Carlo simulation. Copyright © 2017 Elsevier Ltd. All rights reserved.

  14. The determination, by x-ray-fluorescence spectrometry, of gold in activated charcoal

    International Nuclear Information System (INIS)

    Austen, C.E.

    1977-01-01

    A rapid method is described for the determination of gold in activated charcoal by X-ray-fluorescence spectrometry. Compensation for matrix effects is achieved by means of platinum that is added for use as an internal standard. Calibration is achieved by use of a series of synthetic standards that are made by the spiking of barren charcoal with gold and platinum. The limit of determination is about 8 p.p.m. of gold, and the relative standard deviation is 1,2 per cent at a concentration level of 2300 p.p.m

  15. Determination of sulfonamides in meat by liquid chromatography coupled with atmospheric pressure chemical ionization mass spectrometry

    International Nuclear Information System (INIS)

    Kim, Dal Ho; Choi, Jong Oh; Kim, Jin Seog; Lee, Dai Woon

    2002-01-01

    Liquid chromatography/atmospheric pressure chemical ionization-mass spectrometry (LC-APCI-MS) has been used for the determination of sulfonamides in meat. Five typical sulfonamides were selected as target compounds, and beef meat was selected as a matrix sample. As internal standards, sulfapyridine and isotope labeled sulfamethazine ( 13 C 6 -SMZ) were used. Compared to the results of recent reports, our results have shown improved precision to a RSD of 1.8% for the determination of sulfamethazine spiked with 75 ng/g level in meat

  16. 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.

  17. An indirect method for determining phosphorus in aluminium alloys by atomic-absorption spectrometry.

    Science.gov (United States)

    Bernal, J L; Del Nozal, M A; Deban, L; Aller, A J

    1981-07-01

    An indirect method is described for the determination of phosphorus in aluminium alloys. Ammonium molybdate is added to a solution of the aluminium alloy and the molybdophosphoric acid formed is selectively extracted into n-butyl acetate. The twelve molybdenum atoms associated with each phosphate ion are determined by direct atomic-absorption spectrometry with the n-butyl acetate phase in a nitrous oxide-acetylene flame, with measurement at 313.2 nm. The most suitable conditions have been established and the effect of other ions has been studied.

  18. Direct determination of selenoproteins in polyvinylidene difluoride membranes by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Sidenius, U; Gammelgaard, Bente

    2000-01-01

    A method for the direct determination of selenoproteins in plastic membranes after protein separation by gel electrophoresis was developed. Quantification was based on the determination of the selenium content of the proteins by electrothermal atomic absorption spectrometry (ET-AAS) after manual...... were excised and chemical modifier was added on top of the excised membrane prior to atomic absorption measurement. Acceptable linearity was achieved in the range 2-10 ng Se, corresponding to selenium concentrations close to 1 mg/L, when aqueous solutions of selenomethionine standard as well...

  19. Studies in the determination of lead isotope ratios by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Date, A.R.; Yuk Ying Cheung

    1987-01-01

    The application of ICP-MS to the determination of lead isotope ratios in geological materials is described. Data presented for a series of lead mineral concentrates are compared with reference values obtained by conventional solid source thermal ionisation mass spectrometry. The simultaneous determination of lead isotope ratios and trace elements is carried out in a rapid analysis mode. The application of an electrothermal vaporisation technique for small solution aliquots is described. Lead isotope ratio data for the United States Geological Survey standard reference silicate rock BCR-1, obtained without separation of lead from the matrix, are compared with previously published values obtained after separation. (author)

  20. Determination of cobalt in human liver by atomic absorption spectrometry with electrothermal atomization

    International Nuclear Information System (INIS)

    Caldas, E.D.; Gine-Rosias, M.F.; Dorea, J.G.

    1991-01-01

    A detailed study of the use of electrothermal atomic absorption spectrometry for the determination of cobalt in human liver is described. Comparisons of sample digestion using nitric acid or nitric acid plus perchloric acid, atomization procedures and the application of palladium and magnesium nitrate chemical modifiers were studied using NBS SRM 1577a Bovine Liver. The best results were achieved with sample decomposition in nitric acid, atomization from the tube wall and no chemical modifier. Cobalt was determined in 90 samples of livers from foetuses and deceased newborns using the standard addition method with an average recovery of 99.8%. (author). 30 refs.; 4 figs.; 2 tabs

  1. Optimization of simultaneous electrochemical determination of Cd(II), Pb(II), Cu(II) and Hg(II) at carbon nanotube-modified graphite electrodes.

    Science.gov (United States)

    Pikna, L'ubomír; Heželová, Mária; Kováčová, Zuzana

    2015-01-01

    The health of the environment is worsening every day. Monitoring of potentially toxic elements and remediation of environmental pollution are necessary. Therefore, the research and development of simple, inexpensive, portable and effective sensors is important. Electrochemistry is a useful component of the field of environment monitoring. The present study focuses on evaluating and comparing three types of electrodes (PIGE, PIGE/MWCNT/HNO3 and PIGE/MWCNT/EDTA/HNO3) employed for the simultaneous electrochemical determination of four potentially toxic elements: Cd(II), Pb(II), Cu(II) and Hg(II). Cyclic voltammograms were measured in an acetate buffer. The LOD, LOQ, the standard and relative precisions of the method and a prediction intervals were calculated (according to the technical procedure DIN 32 645) for the three electrodes and for each measured element. The LOD for PIGE/CNT/HNO3 (the electrode with narrowest calculated prediction intervals) was 2.98 × 10(-7) mol L(-1) for Cd(II), 4.83 × 10(-7) mol L(-1) for Pb(II), 3.81 × 10(-7) mol L(-1) for Cu(II), 6.79 × 10(-7) mol L(-1) for Hg(II). One of the benefits of this study was the determination of the amount of Hg(II) in the mixture of other elements.

  2. Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: a tutorial review. Part II. Practical considerations.

    Science.gov (United States)

    Leclercq, Amélie; Nonell, Anthony; Todolí Torró, José Luis; Bresson, Carole; Vio, Laurent; Vercouter, Thomas; Chartier, Frédéric

    2015-07-23

    Inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are increasingly used to carry out analyses in organic/hydro-organic matrices. The introduction of such matrices into ICP sources is particularly challenging and can be the cause of numerous drawbacks. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP sources. Part I provided theoretical considerations associated with the physico-chemical properties of such matrices, in an attempt to understand the induced phenomena. Part II of this tutorial review is dedicated to more practical considerations on instrumentation, instrumental and operating parameters, as well as analytical strategies for elemental quantification in such matrices. Two important issues are addressed in this part: the first concerns the instrumentation and optimization of instrumental and operating parameters, pointing out (i) the description, benefits and drawbacks of different kinds of nebulization and desolvation devices and the impact of more specific instrumental parameters such as the injector characteristics and the material used for the cone; and, (ii) the optimization of operating parameters, for both ICP-OES and ICP-MS. Even if it is at the margin of this tutorial review, Electrothermal Vaporization and Laser Ablation will also be shortly described. The second issue is devoted to the analytical strategies for elemental quantification in such matrices, with particular insight into the isotope dilution technique, particularly used in speciation analysis by ICP-coupled separation techniques. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Emodin (1,3,8-trihydroxy-6-methylanthraquinone): a spectrophotometric reagent for the determination of beryllium(II), magnesium(II) and calcium(II)

    International Nuclear Information System (INIS)

    Pal, T.; Jana, N.R.

    1993-01-01

    The individual determination of Be II , Mg II or Ca II by conventional spectrophotometry and simultaneous determination of Mg II and Ca II in mixtures by first-derivative spectrophotometry are possible at trace levels, using emodin (1,3,8-trihydroxy-6-methylanthraquinone) as spectrophotometric reagent. Interference from other metal species, application of these methods to rock samples and statistical analysis of the results are discussed. (author)

  4. Determination of long-lived actinides in soil leachates by inductively coupled plasma: Mass spectrometry

    International Nuclear Information System (INIS)

    Crain, J.S.; Smith, L.L.; Yaeger, J.S.; Alvarado, J.A.

    1994-01-01

    Inductively coupled plasma -- mass spectrometry (ICP-MS) was used to concurrently determine multiple long-lived (t 1/2 > 10 4 y) actinide isotopes in soil samples. Ultrasonic nebulization was found to maximize instrument sensitivity. Instrument detection limits for actinides in solution ranged from 50 mBq L -1 ( 239 Pu) to 2 μBq L -1 ( 235 U) Hydride adducts of 232 Th and 238 U interfered with the determinations of 233 U and 239 Pu; thus, extraction chromatography was, used to eliminate the sample matrix, concentrate the analytes, and separate uranium from the other actinides. Alpha spectrometric determinations of 230 Th, 239 Pu, and the 234 U/ 238 U activity ratio in soil leachates compared well with ICP-MS determinations; however, there were some small systematic differences (ca. 10%) between ICP-MS and a-spectrometric determinations of 234 U and 238 U activities

  5. Preconcentration and determination of zinc and lead ions by a combination of cloud point extraction and flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tavallali, H. [Chemistry Department, Payamenore University, Shiraz (Iran); Shokrollahi, A.; Zahedi, M. [Chemistry Department, Yasouj University, Yasouj (Iran); Niknam, K. [Chemistry Department, Persian Gulf University, Bushehr (Iran); Soylak, M. [Chemistry Department, University of Erciyes, Kayseri (Turkey); Ghaedi, M.

    2009-04-15

    The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of lead(II) and zinc(II). After complexation with 3-[(4-bromophenyl) (1-H-inden-3-yl)methyl]-1 H-indene (BPIMI), the analytes were quantitatively extracted to a phase rich in Triton X-114 after centrifugation. Methanol acidified with 1 mol/L HNO{sub 3} was added to the surfactant rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The concentration of bis((1H-benzo [d] imidazol-2yl)ethyl)sulfane, Triton X-114, pH and amount of surfactant were all optimized. Detection limits (3 SDb/m) of 2.5 and 1.6 ng/mL for Pb{sup 2+} and Zn{sup 2+} along with preconcentration factors of 30 and an enrichment factor of 32 and 48 for Pb{sup 2+}and Zn {sup 2+} ions were obtained, respectively. The proposed cloud point extraction was been successfully applied for the determination of these ions in real samples with complicated matrices such as food and soil samples, with high efficiency. (Abstract Copyright [2009], Wiley Periodicals, Inc.)

  6. Determination of the binding sites for oxaliplatin on insulin using mass spectrometry-based approaches

    DEFF Research Database (Denmark)

    Møller, Charlotte; Sprenger, Richard R.; Stürup, Stefan

    2011-01-01

    Using insulin as a model protein for binding of oxaliplatin to proteins, various mass spectrometric approaches and techniques were compared. Several different platinum adducts were observed, e.g. addition of one or two diaminocyclohexane platinum(II) (Pt(dach)) molecules. By top-down analysis...... and fragmentation of the intact insulin-oxaliplatin adduct using nano-electrospray ionisation quadrupole time-of-flight mass spectrometry (nESI-Q-ToF-MS), the major binding site was assigned to histidine5 on the insulin B chain. In order to simplify the interpretation of the mass spectrum, the disulphide bridges...... were reduced. This led to the additional identification of cysteine6 on the A chain as a binding site along with histidine5 on the B chain. Digestion of insulin-oxaliplatin with endoproteinase Glu-C (GluC) followed by reduction led to the formation of five peptides with Pt(dach) attached...

  7. 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)

  8. Simultaneous determination of ramipril, ramiprilat and telmisartan in human plasma using liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Gupta, V K; Jain, Rajeev; Lukram, Ojitkumar; Agarwal, Shilpi; Dwivedi, Ashish

    2011-01-15

    A rapid and sensitive liquid chromatography tandem mass spectrometry method has been developed and validated for the simultaneous determination of ramipril, ramiprilat and telmisartan in human plasma. The solid-phase extraction technique was used for the extraction of ramipril, ramiprilat and telmisartan from human plasma. Trandolaprilat and hydrochlorothiazide were used as the internal standards (ISs). Chromatography was performed on a Hypurity C18, 5 μm, 50 mm × 4.6mm column, with the mobile phase consisting of ammonium acetate and acetonitrile (in a 20:80 ratio), followed by detection using mass spectrometry. The method involves a simple reversed isocratic chromatography condition and mass spectrometry detection, which enables detection at sub-nanogram levels. The method was validated and the lower limit of quantification for ramipril, ramiprilat and telmisartan was found to be 0.1 ng mL(-1), 0.1 ng mL(-1) and 2 ng mL(-1), respectively. The mean recovery for ramipril, ramiprilat and telmisartan ranged from 90.1 to 104.1%. This method increased the sensitivity and selectivity; resulting in high-throughput analysis of ramipril, ramiprilat and telmisartan using two different ISs in a single experiment for bioequivalence studies, with a chromatographic run time of 1.5 min only. Copyright © 2010 Elsevier B.V. All rights reserved.

  9. Recent advances in applying mass spectrometry and systems biology to determine brain dynamics.

    Science.gov (United States)

    Scifo, Enzo; Calza, Giulio; Fuhrmann, Martin; Soliymani, Rabah; Baumann, Marc; Lalowski, Maciej

    2017-06-01

    Neurological disorders encompass various pathologies which disrupt normal brain physiology and function. Poor understanding of their underlying molecular mechanisms and their societal burden argues for the necessity of novel prevention strategies, early diagnostic techniques and alternative treatment options to reduce the scale of their expected increase. Areas covered: This review scrutinizes mass spectrometry based approaches used to investigate brain dynamics in various conditions, including neurodegenerative and neuropsychiatric disorders. Different proteomics workflows for isolation/enrichment of specific cell populations or brain regions, sample processing; mass spectrometry technologies, for differential proteome quantitation, analysis of post-translational modifications and imaging approaches in the brain are critically deliberated. Future directions, including analysis of cellular sub-compartments, targeted MS platforms (selected/parallel reaction monitoring) and use of mass cytometry are also discussed. Expert commentary: Here, we summarize and evaluate current mass spectrometry based approaches for determining brain dynamics in health and diseases states, with a focus on neurological disorders. Furthermore, we provide insight on current trends and new MS technologies with potential to improve this analysis.

  10. Determination of Nerve Agent Metabolites by Ultraviolet Femtosecond Laser Ionization Mass Spectrometry.

    Science.gov (United States)

    Hamachi, Akifumi; Imasaka, Tomoko; Nakamura, Hiroshi; Li, Adan; Imasaka, Totaro

    2017-05-02

    Nerve agent metabolites, i.e., isopropyl methylphosphonic acid (IMPA) and pinacolyl methylphosphonic acid (PMPA), were derivatized by reacting them with 2,3,4,5,6-pentafluorobenzyl bromide (PFBBr) and were determined by mass spectrometry using an ultraviolet femtosecond laser emitting at 267 and 200 nm as the ionization source. The analytes of the derivatized compounds, i.e., IMPA-PFB and PMPA-PFB, contain a large side-chain, and molecular ions are very weak or absent in electron ionization mass spectrometry. The use of ultraviolet femtosecond laser ionization mass spectrometry, however, resulted in the formation of a molecular ion, even for compounds such as these that contain a highly bulky functional group. The signal intensity was larger at 200 nm due to resonance-enhanced two-photon ionization. In contrast, fragmentation was suppressed at 267 nm (nonresonant two-photon ionization) especially for PMPA-PFB, thus resulting in a lower background signal. This favorable result can be explained by the small excess energy in ionization at 267 nm and by the low-frequency vibrational mode of a bulky trimethylpropyl group in PMPA.

  11. 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)

  12. Polarographic determination of Sn (II) and total Sn in PYRO and MDP radiopharmaceutical kits

    International Nuclear Information System (INIS)

    Sebastian, Maria V.A.; Lugon, Marcelo Di M.V.; Silva, Jose L. da; Fukumori, Neuza T.O.; Pereira, Nilda P.S. de; Silva, Constancia P.G. da; Matsuda, Margareth M.N.

    2007-01-01

    A sensitive, alternative method to atom absorption spectrometry, fluorimetry or potentiometry for the evaluation of tin(II) ions (0.1- 10 mg) and total tin in radiopharmaceutical kits was investigated. Differential pulse polarography was chosen. The supporting electrolyte was H 2 SO 4 3 mol L -1 and HCl 3 mol L -1 solution. The potential was swept from -250 to -800 mV vs Ag/AgCl/saturated KCl, using a dropping mercury electrode with 1 s drop time, 50 mV s -1 scan rate, -50 mV pulse amplitude, 40 ms pulse time and 10 mV step amplitude. Pure nitrogen was used to deaerate the polarographic cell solution for 5 min, before and after each sample introduction. Oxidation of Sn(II) was made in the same sample vial by adding H 2 O 2 (hydrogen peroxide) 10 mol L -1 , at 37 deg C, in order to quantify the total Sn. The calibration curve for Sn(II) and Sn(IV) was obtained in the concentration range of 0-10 ppm from a 1000 ppm standard solution. The detection limit of Sn(II) is 0.5 ppm and for Sn(IV) is 0.6 ppm. Differential pulse polarography was performed in the pyrophosphate (PYRO) and methylenediphosphonic acid (MDP) radiopharmaceutical kits, containing 2 mg and 1 mg of SnCl 2 .2H 2 O per vial, respectively. The described method for determination of stannous ion (Sn(II)), is selective, reproducible and adequate to be used in the quality control of lyophilized reagents and it shall be performed for other cold kits produced at IPEN. (author)

  13. Silica gel modified with N-(3-propyl)-O-phenylenediamine: functionalization, metal sorption equilibrium studies and application to metal enrichment prior to determination by flame atomic absorption spectrometry.

    Science.gov (United States)

    Akl, Magda Ali Abd-elAziz; Kenawy, Ibraheim Mohamed; Lasheen, Rabab Ramadan

    2005-08-01

    The use of the chemically modified silica gel N-(3-propyl)-O-phenylenediamine (SiG-NPPDA) adsorbent, for the preconcentration and separation of trace heavy metals, was described. SiG-NPPDA sorbs quantitatively (90-100% recovery) trace amounts of nine heavy metals, viz., Cd(II), Zn(II), Fe(III), Cu(II), Pb(II), Mn(II), Cr(III), Co(II) and Ni(II) at pH 7-8. The sorption capacity varies from 350 to 450 micromol g(-1). Desorption was found to be quantitative with 1-2 M HNO3 or 0.05 M Na2EDTA. The distribution coefficient, Kd and the percentage concentration of the investigated metal ions on the adsorbent at equilibrium, C(M,eqm)% (Recovery, R%), were studied as a function of experimental parameters. The logarithmic values of the distribution coefficient, log Kd, ranges between 4.0 and 6.4. Some foreign ions caused little interference in the preconcentration and determination of the investigated nine metals by flame atomic absorption spectrometry (AAS). The adsorbent and its formed metal chelates were characterized by IR (absorbance and/or reflectance), potentiometric titrations and thermogravimetric analysis (TGA and DTG). The mode of chelation between the SiG-NPPDA adsorbent and the investigated metal ions is proposed to be due to the reaction of the investigated metal ions with the two nitrogen atoms of the SiG-NPPDA adsorbent. The present adsorbent coupled with flame AAS has been used to enrich and determine the nine metal ions in natural aqueous systems and in certified reference materials (RSD < or = 5%). The copper, iron, manganese and zinc present in some pharmaceutical vitamin samples were also preconcentrated on SiG-NPPDA adsorbent and determined by flame AAS (RSD < or = 4.2%). Nanogram concentrations (0.07-0.14 ng ml(-1)) of Cd(II), Zn(II), Fe(III), Pb(II), Cr(III), Mn(II), Cu(II), Co(II) and Ni(II) can be determined reliably with a preconcentration factor of 100.

  14. Determination of ultratrace elements in natural waters by solid-phase extraction and atomic spectrometry methods.

    Science.gov (United States)

    Grotti, Marco; Abelmoschi, Maria Luisa; Soggia, Francesco; Frache, Roberto

    2003-01-01

    A study was carried out on the preconcentration of ultratrace amounts of cadmium, lead, manganese, copper and iron from high-salinity aqueous samples and determination by atomic spectrometry methods. Sample volume, amount of resin, loading flow rate, and elution volume were optimized in order to obtain the simultaneous preconcentration of all the analytes. Quantitative recoveries were obtained by using 200 mg of iminodiacetic resin with a loading flow rate of 2 mL min(-1), elution volume of 3 mL and sample volume of 50-450 mL. Only copper in seawater samples was not completely retained by the resin (60-70% recovery), due to unfavorable competition of iminodiacetic-active groups with organically bound metal.To quantify the metals in the eluates, two atomic spectrometry techniques were compared: electrothermal atomization atomic absorption spectrometry (ETAAS) and inductively coupled plasma-optical emission spectrometry (ICP-OES) with simultaneous CCD detection system. Both techniques are suitable for sample analysis with detection limits of 1.0, 4.7, 3.3, 6.8, and 53 ng L(-1) using ETAAS and 12, 122, 3.4, 17, and 21 ng L(-1) using ICP-OES for Cd, Pb, Mn, Cu, and Fe, respectively. Relative standard deviations of the procedures ranged from 1.7 to 14% at the sub-microg L(-1) concentration level. The accuracy of both methods was verified by analyzing various certified reference materials (river water, estuarine water, coastal and off-shore seawater).

  15. Determination of ultratrace elements in natural waters by solid-phase extraction and atomic spectrometry methods

    Energy Technology Data Exchange (ETDEWEB)

    Grotti, Marco; Abelmoschi, Maria Luisa; Soggia, Francesco; Frache, Roberto [Department of Chemistry and Industrial Chemistry, University of Genoa, Via Dodecaneso, 31-16146, Genoa (Italy)

    2003-01-01

    A study was carried out on the preconcentration of ultratrace amounts of cadmium, lead, manganese, copper and iron from high-salinity aqueous samples and determination by atomic spectrometry methods. Sample volume, amount of resin, loading flow rate, and elution volume were optimized in order to obtain the simultaneous preconcentration of all the analytes. Quantitative recoveries were obtained by using 200 mg of iminodiacetic resin with a loading flow rate of 2 mL min{sup -1}, elution volume of 3 mL and sample volume of 50-450 mL. Only copper in seawater samples was not completely retained by the resin (60-70% recovery), due to unfavorable competition of iminodiacetic-active groups with organically bound metal.To quantify the metals in the eluates, two atomic spectrometry techniques were compared: electrothermal atomization atomic absorption spectrometry (ETAAS) and inductively coupled plasma-optical emission spectrometry (ICP-OES) with simultaneous CCD detection system. Both techniques are suitable for sample analysis with detection limits of 1.0, 4.7, 3.3, 6.8, and 53 ng L{sup -1} using ETAAS and 12, 122, 3.4, 17, and 21 ng L{sup -1} using ICP-OES for Cd, Pb, Mn, Cu, and Fe, respectively. Relative standard deviations of the procedures ranged from 1.7 to 14% at the sub-{mu}g L{sup -1} concentration level. The accuracy of both methods was verified by analyzing various certified reference materials (river water, estuarine water, coastal and off-shore seawater). (orig.)

  16. Determination of rubidium and strontium in geological materials by X-Ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Roca, M.

    1979-01-01

    In order to determine whole-rock ages by the Rb/Sr procedure, an X-ray fluorescence spectrometry method for the determination of both elements has been developed. The samples are pressed into boric acid backed and ringed pellets with this material as a binding agent. Matrix corrections are made following the determination od the mass absorption coefficients, based on the intensity of the Compton-scattered peak of MoKα. or MoKβ 1 .3. The U. S. Geological Survey granodiorite GSP-1 is used as a reference standard. Spectral-line interferences have been carefully studied and the empirical correction factors determined. A BASIC language program for calculating the Rb and Sr concentrations and the Rb/Sr ratios has been written. (Author) 7 refs

  17. 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

  18. The determination of radium-226 in uranium ores and mill products by alpha energy spectrometry

    International Nuclear Information System (INIS)

    Zimmerman, J.B.; Armstrong, V.C.

    1975-12-01

    A reliable routine procedure for determining 226 Ra by alpha energy spectrometry is described. Radium is isolated as sulphate from the sample matrix by co-precipitation with a small mass of barium and analysed using a ruggedized silicon surface barrier detector. The method is capable of providing high accuracy over a large 226 Ra concentration range and is applicable to materials such as uranium ores, uranium mill products and effluent streams. Samples resulting from nitric acid leach experiments with Elliot Lake ores were examined using the procedure. The distribution of 223 Ra, 224 Ra and 226 Ra between the leach products, (residue and leach liquor), is discussed. (author)

  19. Thallium determination in reference materials by isotope dilution mass spectrometry (IDMS) using thermal ionization

    International Nuclear Information System (INIS)

    Waidmann, E.; Hilpert, K.; Stoeppler, M.

    1990-01-01

    Using Isotope Dilution Mass Spectrometry (IDMS) with thermal ionization, thallium concentrations were determined in reference materials from NIST and BCR, from other sources, and reference materials from the German Environmental Specimen Bank 203 Tl spike solution is applied for the isotope dilution technique. Thallium concentrations in the investigated materials range from 2.67 μg Tl.kg -1 to 963 μg Tl.kg -1 with a relative standard deviation from 0.14 to 10%. The detection limit was 0.1 ng thallium for this work. (orig.)

  20. Determination of molybdenum in plant reference material by thermal-ionization isotope-dilution mass spectrometry

    International Nuclear Information System (INIS)

    Saumer, M.; Gantner, E.; Reinhardt, J.; Ache, H.J.

    1992-01-01

    An analytical method is described for the determination of the concentration and the isotopic composition of molybdenum in plant samples using thermal ionization mass spectrometry. After microwave acid digestion and liquid-liquid extractive separation with Amberlite LA-2, the molybdenum isotopes are measured as MoO 3 - -ions in a quadrupole mass spectrometer. In all cases, the relative standard deviation of the measurements of both natural and spike molybdenum was better than 3% for all ratios measured. The concentration of molybdenum found in three different plant reference materials agreed well with the certified values. (orig.)

  1. Comparison of Titration ICP and XRF Spectrometry Methods in Determination of Cerium in Lens Polishing Powder

    International Nuclear Information System (INIS)

    Ninlaphruk, Sumalee; Pichestapong, Pipat; Mungpayabal, Harinate; Jiyavaranant, Thitima; Srisukho, Supapan; Chaisai, Prapassurn

    2004-10-01

    Three analytical methods in determination of cerium in cerium oxide separated from monazite ore for producing lens polishing powder were compared. These methods are titration ICP and XRF spectrometry techniques. The cerium oxide sample with estimated 45% cerium content needed to be digested and converted into solution before the analysis. The analytical results shown significantly no difference between each method. However, the titration method was found to be more convenient and suitable for quality control in the production of cerium oxide as it does not require standard cerium and the complicated analytical instruments

  2. Application of ion mobility spectrometry for the determination of tramadol in biological samples

    OpenAIRE

    Ali Sheibani; Najmeh Haghpazir

    2014-01-01

    In this study, a simple and rapid ion mobility spectrometry (IMS) method has been described for the determination of tramadol. The operating instrumental parameters that could influence IMS were investigated and optimized (temperature; injection: 220 and IMS cell: 190°C, flow rate; carrier: 300 and drift: 600 mL/minute, voltage; corona: 2300 and drift: 7000 V, pulse width: 100 μs). Under optimum conditions, the calibration curves were linear within two orders of magnitude with R2 ≥ 0.998 for ...

  3. Determination of plutonium isotopic ratios and total concentration by gamma ray spectrometry

    International Nuclear Information System (INIS)

    Despres, Michele.

    1980-11-01

    A non-destructive method of analysis is being investigated for the control in situ of plutonium isotopic composition and total concentration in different matrix without preliminary calibration. The plutonium isotopic composition is determined by gamma-ray spectrometry using germanium detector systems. The same apparatus is used for direct measuring of the total plutonium concentration in solutions or solids by a differential attenuation technique based on two transmitted gamma rays with energies on both sides of the k shell absorption edge of plutonium [fr

  4. Exploiting flow Injection and sequential injection schemes for trace metal determinations by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    Determination of low or trace-level amounts of metals by electrothermal atomic absorption spectrometry (ETAAS) often requires the use of suitable preconcentration and/or separation procedures in order to attain the necessary sensitivity and selectivity. Such schemes are advantageously executed...... by superior performance and versatility. In fact, two approaches are conceivable: The analyte-loaded ion-exchange beads might either be transported directly into the graphite tube where they are pyrolized and the measurand is atomized and quantified; or the loaded beads can be eluted and the eluate forwarded...

  5. Results from an interlaboratory exercise on the determination of plutonium isotopic ratios by gamma spectrometry

    International Nuclear Information System (INIS)

    Ottmar, H.

    1981-07-01

    Results form interlaboratory comparison measurements on the determination of plutonium isotopic ratios by gamma spectrometry, organized by the ESARDA Working Group on Techniques and Standards for Nondestructive Analysis, are presented and discussed. Nine laboratories from nine countries or international organizations participated in the intercomparison exercise, which included both laboratories' own measurements on the plutonium isotopic reference materials NBS-SRM 946, 947, 948 and comparison analyses of gamma spectra from these materials distributed to the participating laboratories. Results from the intercomparison analyses have been used to reevaluate some gamma branching intensity ratios required for plutonium isotopic ratio measurements. (orig.) [de

  6. Determination of tin(II) in reagents for radiopharmaceuticals

    International Nuclear Information System (INIS)

    Morosanova, E.I.; Loginova, K. A.; Epstein, N.B.

    2003-01-01

    The goal of this work is to elaborate a procedure for rapid and simple determination of tin(II) in reagents for preparation of radiopharmaceuticals based on a system albumin-Tc-99m. Original test tools for the determination of various analytes have been suggested in our lab based on the use of small glass tubes (1-2 mm i.d. - 50-70 mm) filled with indicator powders containing suitable immobilized chromogenic reagents. An analytical signal (a length of colored zone which is proportional to the concentration of an analyte) is detected after a sample passing through the indicator tube. Heteropoly compounds are well-known analytical reagents for a photometric determination of various reductants. For elaboration of indicator tubes abilities of Mo,P-heteropoly compounds to give deeply colored blue compounds after reduction were used. (authors)

  7. Determination of iodine in oyster tissue by isotope dilution laser resonance ionization mass spectrometry

    International Nuclear Information System (INIS)

    Fassett, J.D.; Murphy, T.J.

    1990-01-01

    The technique of laser resonance ionization mass spectrometry has been combined with isotope dilution analysis to determine iodine in oyster tissue. The long-lived radioisotope, 129I, was used to spike the samples. Samples were equilibrated with the 129I, wet ashed under controlled conditions, and iodine separated by coprecipitation with silver chloride. The analyte was dried as silver ammonium iodide upon a tantalum filament from which iodine was thermally desorbed in the resonance ionization mass spectrometry instrument. A single-color, two-photon resonant plus one-photon ionization scheme was used to form positive iodine ions. Long-lived iodine signals were achieved from 100 ng of iodine. The precision of 127I/129I measurement has been evaluated by replicate determinations of the spike, the spike calibration samples, and the oyster tissue samples and was 1.0%. Measurement precision among samples was 1.9% for the spike calibration and 1.4% for the oyster tissue. The concentration of iodine determined in SRM 1566a, Oyster Tissue, was 4.44 micrograms/g with an estimate of the overall uncertainty for the analysis of +/- 0.12 microgram/g

  8. Determination of chlorine in coal by X-ray fluorescence spectrometry method

    Energy Technology Data Exchange (ETDEWEB)

    Marek, S.; Bojarska, K. [Central Mining Institute, Katowice (Poland). Dept. of Environmental Monitoring

    1997-12-31

    Determination of chlorine contents in coal is essential for both environmental protection and its technological use. The existing method of chlorine determination in coal are titration methods which have considerable errors particularly in the low concentration range. The elaborated method with the use of X-ray fluorescence spectrometry in a comparison to the other methods is much faster and has better precision and accuracy. The principle of the method lies in the measurement of X-ray fluorescence radiation intensity which is emitted by chlorine in a sample and its comparison with standards. The calibration of the elaborated XRF method is based on natural coals having various concentrations of chlorine within the whole range of its occurrence in Polish coals. Concentrations for the calibration purpose were obtained by the determination of chlorine contents in selected coals by atomic absorption spectrometry method. The procedure of sample preparation for direct X-ray measurements, instrumental measuring conditions and the way of calibration curve preparation are described in the paper. All X-ray measurements were done with a Phillips sequential X-ray fluorescence spectrometer. A double anode Cr-Au X-ray tube with maximum power 3000 MW was used as the excitation source. 5 figs., 4 tabs.

  9. STRUCTURAL STUDY OF BIS(2,6-BIS(PYRAZOL-3-YLPYRIDINENICKEL(II BY CALORIMETRY AND EXAFS SPECTROMETRY

    Directory of Open Access Journals (Sweden)

    Kristian H Sugiyarto

    2010-06-01

    Full Text Available The main aim of this work is to reveal the complex formation of 2,6-bis(pyrazol-3-ylpyridine, bpp, with nickel(II perchlorate in DMF by calorimetric stepwise complex formation and then followed by EXAFS spectrometry. It was found that the complex formation follows two stepwise pathways namely the formation of mono pyrazolyl-pyridine, [Ni(DMF3 bpp]2+, and bis pyrazolyl-pyridine, [Ni(bpp2]2+;  the formation constants being  log β1 = 6.57, and log β2 = 5.02, and the total value of log β  = 11.58. The final formation of six-coordinated compound was confirmed by EXAFS analysis with the mean Ni-Nbpp bond length of 2.0646(0.0014 Å.   Keywords: nickel(II, bpp, EXAFS

  10. 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)

  11. Some metals determination in beers by atomic emission spectrometry of induced argon plasma

    International Nuclear Information System (INIS)

    Matsushige, I.

    1990-01-01

    It was made the identification and determination of metals in brazilian bottled and canned beer, using atomic emission spectrometry with d.c. are and argon coupled plasma excitation sources. The elements Co, Cr, Cu, Fe, Pb and Zn were determined in beer samples, after treatment with HNO sub(3) conc. /H sub(2) O sub(2) (30%). In the determination of Co, Cr, Cu, Pb and Zn and alternative method using HNO sub(3) conc. /O sub(3) was proved be useful. The results obtained for Co, Cr, Cu, Fe, Pb and Zn were below the limits established by brazilian legislation, showing the good quality of the beer concerning the metals. The results of this work were requested by the previous Ministerio do Meio Ambiente e Urbanismo in order to contribute to review the brazilian legislation in foods and beverages about metals contents. (author)

  12. Standard test method for quantitative determination of americium 241 in plutonium by Gamma-Ray spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    1994-01-01

    1.1 This test method covers the quantitative determination of americium 241 by gamma-ray spectrometry in plutonium nitrate solution samples that do not contain significant amounts of radioactive fission products or other high specific activity gamma-ray emitters. 1.2 This test method can be used to determine the americium 241 in samples of plutonium metal, oxide and other solid forms, when the solid is appropriately sampled and dissolved. 1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

  13. [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.

  14. Standard test method for the radiochemical determination of americium-241 in soil by alpha spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2007-01-01

    1.1 This method covers the determination of americium–241 in soil by means of chemical separations and alpha spectrometry. It is designed to analyze up to ten grams of soil or other sample matrices that contain up to 30 mg of combined rare earths. This method allows the determination of americium–241 concentrations from ambient levels to applicable standards. The values stated in SI units are to be regarded as standard. 1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific precaution statements, see Section 10.

  15. Remarks on the gamma-ray spectrometry for the determination of natural radioisotopes

    International Nuclear Information System (INIS)

    Kalita, S.; Niewodniczanski, J.

    1987-01-01

    Semiconductor low-energy gamma ray spectrometry is compared with the routinely used scintillation method (within higher energy range). Measurements of low-energy natural gamma radiation using a semiconductor detector permit the determination of radioactive equilibrium of the uranium series. In this method 238 U ( 234 Th) content is determined by 63 keV, 226 Ra by 186 keV and 214 Pb by 295 keV gamma rays. Using the same results one can calculate a radioactive equilibrium coefficient R, defined as concentration ratio 226 Ra/ 238 U and a 222 Rn emanation ratio E, defined as 1 - 214 Pb/ 226 Ra (concentrations in uranium equivalent units). The relative standard errors for the method are: 10 - 15% in case of radioisotope content and about 18% for R and E determination. 7 refs., 2 figs., 2 tabs. (author)

  16. Determination of cobalt in human biological liquids from electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Dragan, Felicia [University of Oradea, Faculty of Medicine and Pharmacy, 29 N Jiga, 410028 Oradea (Romania); HIncu, Lucian [University of Medicine and Pharmacy ' Carol Davila' , Faculty of Pharmacy, 6 Traian Vuia, 020956 Bucuresti (Romania); Bratu, Ioan, E-mail: fdragan@uoradea.r [National Institute for Research and Development of Isotopic and Molecular Technologies, 65-103 Donath, 400293 Cluj-Napoca (Romania)

    2009-08-01

    Problems and possibilities of the determination of Co in serum and urine samples by electrothermal atomic absorption spectrometry (ETAAS) are described. Optimal instrumental parameters as well as a suitable atomizer, calibration procedure and hydrogen peroxide as modifier are proposed for direct ETAAS measurement of Co in serum and urine. The detection limit achieved was 0.1 {mu}g L{sup -1} for both matrices and relative standard deviations varied in the range 5-20% depending on the Co concentration in the sample. The validity of the method was verified by the analyses of standard reference materials. For serum samples with Co content lower than the detection limit, a separation and preconcentration procedure based on liquid/liquid extraction is suggested prior to determination of Co in the organic phase by ETAAS. This procedure permits determination of 0.02 {mu}g L{sup -1} Co in serum samples with a relative standard deviation of 10-18%.

  17. Determination of microquantities of cesium in leaching tests by atomic absorption spectrometry with electrothermal atomization

    International Nuclear Information System (INIS)

    Crubellati, R.O.; Di Santo, N.R.

    1988-01-01

    An original method for cesium determinations by atomic absorption spectrometry with electrothermal atomization is described. The effect of foreign ions (alkali and earth alkaline metals) present in leaching test of glasses with incorporated radioactive wastes was studied. The effect of different mineral acids was also investigated. A comparison between the flame excitation method and the electrothermal atomization one was made. Under optimum conditions, cesium in quantities down to 700 ng in 1000 ml of sample could be determined. The calibration curve was linear in the range of 0.7 - 15 ng/mL. The fact that the proposed determinations can be performed in a short time and that a small sample volume is required are fundamental advantages of this method, compared with the flame excitation procedure. Besides, it is adaptable to be applied in hot cells and glove boxes. (Author) [es

  18. Uranium isotopes determination in urine samples using alpha spectrometry and ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Rosa, Mychelle M.L.; Maihara, Vera A. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Tine, Fernanda D.; Santos, Sandra M.C.; Bonifacio, Rodrigo L.; Taddei, Maria HelenaT. [Comissao Nacional de Energia Nuclear (LAPOC/CNEN-MG), Pocos de Caldas, MG (Brazil). Laboratorio de Pocos de Caldas

    2015-07-01

    The action of determining the concentration of uranium isotopes in biological samples, 'in vitro' bioassay, is an indirect method for evaluating the incorporation and quantification of these radionuclides internally deposited. When incorporated, these radionuclides tend to be disposed through excretion, with urine being the main source of data because it can be easily collected and analyzed. The most widely used methods for determination of uranium isotopes ({sup 234}U, {sup 235}U and {sup 238}U) are Alpha Spectrometry and ICP-MS. This work presents a comparative study for the determination of uranium isotopes using these two methodologies in real samples from occupationally exposed workers. In order to validate the methodology, a sample of the intercomparison exercise organized by PROCORAD (Association pour la Promotion du Controle de Qualite des Analyses de Biologie Medicale em Radiotoxicologie) was used, and the results were statistically compared applying the Student's t-test. (author)

  19. Determination of aluminium and beryllium by diffuse reflectance spectrometry with the use of chromaticity functions

    International Nuclear Information System (INIS)

    Ivanov, V.M.; Ershova, N.I.

    2001-01-01

    Immobilized Eriochrome Cyanine R was used for the direct trace determination of aluminium and beryllium by diffuse reflectance spectrometry. Anion exchanger AV-17, silica gel Silochrom C-120, Chromaton N-Super, silica gel C 18 , and cellulose were examined as supports. Optimal sorption conditions were found. The dependence of chromaticity functions (chromaticity coordinates, lightness, color saturation, yellowness, and whiteness) on different factors was studied. Advantages of the use of chromaticity functions rather than the diffuse reflectance coefficient were demonstrated. A method is developed for the separate determination of aluminium and beryllium using cellulose as the support; the method was used for the analysis of real samples and tested with standard samples. When solution samples of 50 and 100 ml were used, the determination limit was 0.004 μg/ml for aluminium and 0.0002 μg/ml for beryllium, respectively [ru

  20. Determination of cadmium in seawater by chelate vapor generation atomic fluorescence spectrometry

    Science.gov (United States)

    Sun, Rui; Ma, Guopeng; Duan, Xuchuan; Sun, Jinsheng

    2018-03-01

    A method for the determination of cadmium in seawater by chelate vapor generation (Che-VG) atomic fluorescence spectrometry is described. Several commercially available chelating agents, including ammonium pyrrolidine dithiocarbamate (APDC), sodium dimethyl dithiocarbamate (DMDTC), ammonium dibutyl dithiophosphate (DBDTP) and sodium O,O-diethyl dithiophosphate (DEDTP), are compared with sodium diethyldithiocarbamate (DDTC) for the Che-VG of cadmium, and results showed that DDTC and DEDTP had very good cadmium signal intensity. The effect of the conditions of Che-VG with DDTC on the intensity of cadmium signal was investigated. Under the optimal conditions, 85 ± 3% Che-VG efficiency is obtained for cadmium. The detection limit (3σ) obtained in the optimal conditions was 0.19 ng ml- 1. The relative standard deviation (RSD, %) for ten replicate determinations at 2 ng ml- 1 Cd was 3.42%. The proposed method was successfully applied to the ultratrace determination of cadmium in seawater samples by the standard addition method.

  1. [Graphite furnace atomic absorption spectrometry for determination of thallium in blood].

    Science.gov (United States)

    Zhang, Q L; Gao, G

    2016-04-20

    Colloidal palladium was used as chemical modifier in the determination of blood thallium by graphite furnace atomic absorption spectrometry. Blood samples were precipitated with 5% (V/V)nitric acid, and then determined by GFAAS with colloidal palladium used as a chemical modifier. 0.2% (W/V)sodium chloride was added in the standard series to improve the matrix matching between standard solution and sample. The detection limit was 0.2 μg/L. The correlation coefficient was 0.9991. The recoveries were between 93.9% to 101.5%.The relative standard deviations were between 1.8% to 2.7%.The certified reference material of whole blood thallium was determined and the result was within the reference range Conclusion: The method is accurate, simple and sensitive, and it can meet the needs of detection thallium in blood entirely.

  2. Uranium isotopes determination in urine samples using alpha spectrometry and ICP-MS

    International Nuclear Information System (INIS)

    Rosa, Mychelle M.L.; Maihara, Vera A.; Tine, Fernanda D.; Santos, Sandra M.C.; Bonifacio, Rodrigo L.; Taddei, Maria HelenaT.

    2015-01-01

    The action of determining the concentration of uranium isotopes in biological samples, 'in vitro' bioassay, is an indirect method for evaluating the incorporation and quantification of these radionuclides internally deposited. When incorporated, these radionuclides tend to be disposed through excretion, with urine being the main source of data because it can be easily collected and analyzed. The most widely used methods for determination of uranium isotopes ( 234 U, 235 U and 238 U) are Alpha Spectrometry and ICP-MS. This work presents a comparative study for the determination of uranium isotopes using these two methodologies in real samples from occupationally exposed workers. In order to validate the methodology, a sample of the intercomparison exercise organized by PROCORAD (Association pour la Promotion du Controle de Qualite des Analyses de Biologie Medicale em Radiotoxicologie) was used, and the results were statistically compared applying the Student's t-test. (author)

  3. Extractive alkylation of 6-mercaptopurine and determination in plasma by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Floberg, S; Hartvig, P; Lindström, B; Lönner-Holm, G; Odlind, B

    1981-09-11

    An analytical procedure was developed for the determination of 6-mercaptopurine in plasma. Owing to the polar character and low plasma concentration of the compound, extraction and derivatization was carried out directly from the plasma sample by extractive alkylation. Determination was made using gas chromatography-mass spectrometry with multiple-ion detection. Conditions with respect to the rate of formation and the stability of the derivative formed in the extractive alkylation step were evaluated. The selectively of the method to azathioprine and to metabolites was thoroughly investigated. No 6-mercaptopurine was formed from azathioprine added to water or plasma and run through the method. The method enables the detection of 2 ng of 6 mercaptopurine in a 1.0-ml plasma sample. Quantitative determinations were done down to 10 ng/ml 6 mercaptopurine in plasma.

  4. Radionuclide determination in environmental samples by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Lariviere, Dominic; Taylor, Vivien F.; Evans, R. Douglas; Cornett, R. Jack

    2006-01-01

    The determination of naturally occurring and anthropogenic radionuclides in the environment by inductively coupled plasma mass spectrometry has gained recognition over the last fifteen years, relative to radiometric techniques, as the result of improvement in instrumental performance, sample introduction equipment, and sample preparation. With the increase in instrumental sensitivity, it is now possible to measure ultratrace levels (fg range) of many radioisotopes, including those with half-lives between 1 and 1000 years, without requiring very complex sample pre-concentration schemes. However, the identification and quantification of radioisotopes in environmental matrices is still hampered by a variety of analytical issues such as spectral (both atomic and molecular ions) and non-spectral (matrix effect) interferences and instrumental limitations (e.g., abundance sensitivity). The scope of this review is to highlight recent analytical progress and issues associated with the determination of radionuclides by inductively coupled plasma mass spectrometry. The impact of interferences, instrumental limitations (e.g., degree of ionization, abundance sensitivity, detection limits) and low sample-to-plasma transfer efficiency on the measurement of radionuclides by inductively coupled plasma mass spectrometry will be described. Solutions that overcome these issues will be discussed, highlighting their pros and cons and assessing their impact on the measurement of environmental radioactivity. Among the solutions proposed, mass and chemical resolution through the use of sector-field instruments and chemical reactions/collisions in a pressurized cell, respectively, will be described. Other methods, such as unique sample introduction equipment (e.g., laser ablation, electrothermal vaporisation, high efficiency nebulization) and instrumental modifications/optimizations (e.g., instrumental vacuum, radiofrequency power, guard electrode) that improve sensitivity and performance

  5. Complexation of malic acid with cadmium(II) probed by electrospray ionization mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Jaklová Dytrtová, Jana; Jakl, M.; Schröder, Detlef

    2012-01-01

    Roč. 90, 15 Feb (2012), s. 63-68 ISSN 0039-9140 Institutional research plan: CEZ:AV0Z40550506 Keywords : electrospray ionization * hazardous metal s * mass spectrometry * root exudates * soil solution Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 3.498, year: 2012

  6. Iodometric determination of peroxydiphosphate in the presence of copper(II) or iron(II) as catalyst.

    Science.gov (United States)

    Kapoor, S; Sharma, P D; Gupta, Y K

    1975-09-01

    Peroxydiphosphate can be determined iodometrically in the presence of a large excess of potassium iodide with copper(II) or iron(II) as catalyst through the operation of the Cu(II)/Cu(I) or Fe(II)/Fe(III) cycle. The method is applicable in HClO(4), H(2)SO(4), HCl and CH(3)COOH acid media in the range 0.1-1.0M studied. Nickel, manganese(II), cobalt(II), silver, chloride and phosphate are without effect.

  7. ETAAS determination of thallium and silver from water matrix after colloidal precipitate flotation using lead(II hexamethylenedithiocarbamate

    Directory of Open Access Journals (Sweden)

    TRAJCE STAFILOV

    2001-10-01

    Full Text Available Afast method for the preconcentration of thallium and silver in nanogram quantities in fresh drinking waters (source, well, tap and waters for irrigation using colloidal precipitate flotation is described. Lead(II hexamethylenedithiocarbamate, Pb(HMDTC2 played the role of flotation collector. The experimental conditions for the successful separation of thallium and silver (mass of Pb, amount ofHMDTC-, pHof the system, induction time, type of surfactant etc. were optimized. After flotation separation from the mother liquor, the solid sublate containing traces of thallium and silver was dissolved and the analytes were determined by electrothermal atomic absorption spectrometry (ETAAS. The results of the ETAAS analysis are compared with those obtained by inductively coupled plasma-atomic emission spectrometry. The detection limit for thallium by this method is 0.027 mg/l, and for silver 0.005 microg/l.

  8. Determination of 226Ra by gamma spectrometry: study of packaging vial of sample for analysis

    International Nuclear Information System (INIS)

    Carneiro, Andre Cavalcanti

    2015-01-01

    Determination of radioactivity levels of 226 Ra by gamma spectrometry in a sample is based on measurements of 214 Pb and 214 Bi, daughters of 222 Rn. Because radon is a gas, it can leak from the sample vial or accumulate on the upper empty it. If the vial has any crack, there will be loss of gas, which will cause error in determining the 226 Ra concentration. One possible cause of cracks in the vials, that houses standards and samples, is the radiolysis action in the vial material, usually a polymer. As the demand 226 Ra analysis in different matrices (geological samples, food, plants, etc.) is increasing, it was decided to study some polymer vials available on the market, to verify the feasibility to be used when is applied the analysis method using gamma spectrometry. Four types of polymer vials have been studied. The radiation doses in walls of the vials caused by natural radionuclides present in the sample were simulated using gamma irradiation. Tests, such as compressive strength test and tightness, were applied to the irradiated and non-irradiated vials. First, to verify the effect of radiolysis on the vial material and also if there was 222 Rn diffusion in their walls. These preliminary results pointed out that the acrylic vials are the best option of packaging samples for analysis. This study should be repeated in a larger number of samples for a better evaluation. (author)

  9. Determination of 7BE in soil sample by gamma spectrometry for erosion researchs

    International Nuclear Information System (INIS)

    Esquivel, Alexander D.; Kastner, Geraldo F.; Amaral, Angela M.; Monteiro, Roberto Pellacani G.; Moreira, Rubens M.

    2015-01-01

    Cosmogenic 7 Be is a natural radiotracer produced in the stratosphere and troposphere and reached to the Earth surface via wet and dry fallout and hence its measurement for research of erosion in soils is very significant. The 7 Be radio analyse based on gamma spectrometry technique has been a routine methodology for decades and although is the reference procedure is not free of analytical interference. 7 Be is a β-γ emitting radionuclide (Eγ = 477.59 keV, T½ = 53.12d) and depending on the chemical profile of the soil its determination is susceptible to 228 Ac (E γ = 478.40 keV, T½ = 6.15h) interference. The aim of this work was to establish an analytical protocol for the 7 Be determination in soil samples from Juatuba-Mg region in different sampling periods of dry and rainy seasons for erosion studies and to establish some methodologies for evaluating and correcting the interference level of 228 Ac in the 7 Be activity measurements by gamma spectrometry. (author)

  10. Determination of Dibutyltin in Sediments Using Isotope Dilution Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    Yim, Yong Hyeon; Park, Ji Youn; Han, Myung Sub; Park, Mi Kyung; Kim, Byung Joo; Lim, Young Ran; Hwang, Eui Jin; So, Hun Young

    2005-01-01

    A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties

  11. Determination of Dibutyltin in Sediments Using Isotope Dilution Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Yim, Yong Hyeon; Park, Ji Youn; Han, Myung Sub; Park, Mi Kyung; Kim, Byung Joo; Lim, Young Ran; Hwang, Eui Jin; So, Hun Young [Korea Research Institute of Standards and Science, Daejeon (Korea, Republic of)

    2005-03-15

    A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties.

  12. Status of determining transuranic nuclides speciation in aqueous solution with laser spectrometry

    International Nuclear Information System (INIS)

    Wang Bo; Liu Dejun; Yao Jun; Chen Xi; Long Haoqi; Zeng Jishu; Su Xiguang; Fan Xianhua

    2007-01-01

    The knowledge about speciation of transuranic nuclides in aqueous solution is a basis for understanding the chemical and migration behavior of transuranic nuclides in aqueous solution. The speciation of transuranic nuclides with trace concentration is complicated in near neutral aqueous solutions, including change of oxidation state, complexation and colloid generation, etc. The concentrations of transuranium in near neutral aqueous solution usually below the sensitivity range of method such as conventional absorption spectroscopy. The radioactive analysis method has a very low detection limits for radionuclides, however, it wouldn' t allow the direct measurement of the transuranic species. In contrast with these methods, laser spectroscopy is an ideal method with high sensitivity, and non-contact and non-destructive for determining the speciation of transuranic nuclides. This paper summarizes the status and application of LIPAS (Laser-induced Photoacoustic Spectrometry), LIBD (Laser-induced Breakdown Detection) and TRLFS (Time-resolved Laser Fluorescence Spectrometry) to determine the speciation of transuranic nuclides with trace concentration in aqueous solutions. (authors)

  13. Determination of radionuclide levels in rainwater using ion exchange resin and γ-spectrometry

    International Nuclear Information System (INIS)

    Jungck, Matthias H.A.; Andrey, Jean-Louis; Froidevaux, Pascal

    2009-01-01

    The evaluation of radioactivity accidentally released into the atmosphere involves determining the radioactivity levels of rainwater samples. Rainwater scavenges atmospheric airborne radioactivity in such a way that surface contamination can be deduced from rainfall rate and rainwater radioactivity content. For this purpose, rainwater is usually collected in large surface collectors and then measured by γ-spectrometry after such treatments as evaporation or iron hydroxide precipitation. We found that collectors can be adapted to accept large surface (diameter 47 mm) cartridges containing a strongly acidic resin (Dowex AG 88) which is able to quantitatively extract radioactivity from rainwater, even during heavy rainfall. The resin can then be measured by γ-spectrometry. The detection limit is 0.1 Bq per sample of resin (80 g) for 137 Cs. Natural 7 Be and 210 Pb can also be measured and the activity ratio of both radionuclides is comparable with those obtained through iron hydroxide precipitation and air filter measurements. Occasionally 22 Na has also been measured above the detection limit. A comparison between the evaporation method and the resin method demonstrated that 2/3 of 7 Be can be lost during the evaporation process. The resin method is simple and highly efficient at extracting radioactivity. Because of these great advantages, we anticipate it could replace former rainwater determination methods. Moreover, it does not necessitate the transportation of large rainwater volumes to the laboratory

  14. [Determination of Heavy Metal Elements in Diatomite Filter Aid by Inductively Coupled Plasma Mass Spectrometry].

    Science.gov (United States)

    Nie, Xi-du; Fu, Liang

    2015-11-01

    This study established a method for determining Be, Cr, Ni, As, Cd, Sb, Sn, Tl, Hg and Pb, total 10 heavy metals in diatomite filter aid. The diatomite filter aid was digested by using the mixture acid of HNO₃ + HF+ H₃PO₄ in microwave system, 10 heavy metals elements were determined by inductively coupled plasma mass spectrometry (ICP-MS). The interferences of mass spectrometry caused by the high silicon substrate were optimized, first the equipment parameters and isotopes of test metals were selected to eliminate these interferences, the methane was selected as reactant gas, and the mass spectral interferences were eliminated by dynamic reaction cell (DRC). Li, Sc, Y, In and Bi were selected as the internal standard elements to correct the interferences caused by matrix and the drift of sensitivity. The results show that the detection limits for analyte is in the range of 3.29-15.68 ng · L⁻¹, relative standard deviations (RSD) is less than 4.62%, and the recovery is in the range of 90.71%-107.22%. The current method has some advantages such as, high sensitivity, accurate, and precision, which can be used in diatomite filter aid quality control and safety estimations.

  15. Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: A tutorial review. Part II. Practical considerations

    International Nuclear Information System (INIS)

    Leclercq, Amélie; Nonell, Anthony; Todolí Torró, José Luis; Bresson, Carole; Vio, Laurent; Vercouter, Thomas; Chartier, Frédéric

    2015-01-01

    Graphical abstract: This tutorial review is dedicated to the analysis of organic/hydro-organic matrices by ICP techniques. A state-of-the-art focusing on sample introduction, relevant operating parameters optimization and analytical strategies for elemental quantification is provided. - Highlights: • Practical considerations to perform analyses in organic/hydro-organic matrices. • Description, benefits and drawbacks of recent introduction devices. • Optimization to improve plasma tolerance towards organic/hydro-organic matrices. • Analytical strategies for elemental quantification in organic/hydro-organic matrices. - Abstract: Inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are increasingly used to carry out analyses in organic/hydro-organic matrices. The introduction of such matrices into ICP sources is particularly challenging and can be the cause of numerous drawbacks. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP sources. Part I provided theoretical considerations associated with the physico-chemical properties of such matrices, in an attempt to understand the induced phenomena. Part II of this tutorial review is dedicated to more practical considerations on instrumentation, instrumental and operating parameters, as well as analytical strategies for elemental quantification in such matrices. Two important issues are addressed in this part: the first concerns the instrumentation and optimization of instrumental and operating parameters, pointing out (i) the description, benefits and drawbacks of different kinds of nebulization and desolvation devices and the impact of more specific instrumental parameters such as the injector characteristics and the material used for the cone; and, (ii) the optimization of operating parameters, for both ICP-OES and ICP-MS. Even if it is at the margin of this tutorial review

  16. Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: A tutorial review. Part II. Practical considerations

    Energy Technology Data Exchange (ETDEWEB)

    Leclercq, Amélie, E-mail: amelie.leclercq@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Nonell, Anthony, E-mail: anthony.nonell@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Todolí Torró, José Luis, E-mail: jose.todoli@ua.es [Universidad de Alicante, Departamento de Quimica Analitica, Nutricion y Bromatología, Ap. de Correos, 99, 03080 Alicante (Spain); Bresson, Carole, E-mail: carole.bresson@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Vio, Laurent, E-mail: laurent.vio@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Vercouter, Thomas, E-mail: thomas.vercouter@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Chartier, Frédéric, E-mail: frederic.chartier@cea.fr [CEA Saclay, DEN, DANS, DPC, 91191 Gif-sur-Yvette (France)

    2015-07-23

    Graphical abstract: This tutorial review is dedicated to the analysis of organic/hydro-organic matrices by ICP techniques. A state-of-the-art focusing on sample introduction, relevant operating parameters optimization and analytical strategies for elemental quantification is provided. - Highlights: • Practical considerations to perform analyses in organic/hydro-organic matrices. • Description, benefits and drawbacks of recent introduction devices. • Optimization to improve plasma tolerance towards organic/hydro-organic matrices. • Analytical strategies for elemental quantification in organic/hydro-organic matrices. - Abstract: Inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are increasingly used to carry out analyses in organic/hydro-organic matrices. The introduction of such matrices into ICP sources is particularly challenging and can be the cause of numerous drawbacks. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP sources. Part I provided theoretical considerations associated with the physico-chemical properties of such matrices, in an attempt to understand the induced phenomena. Part II of this tutorial review is dedicated to more practical considerations on instrumentation, instrumental and operating parameters, as well as analytical strategies for elemental quantification in such matrices. Two important issues are addressed in this part: the first concerns the instrumentation and optimization of instrumental and operating parameters, pointing out (i) the description, benefits and drawbacks of different kinds of nebulization and desolvation devices and the impact of more specific instrumental parameters such as the injector characteristics and the material used for the cone; and, (ii) the optimization of operating parameters, for both ICP-OES and ICP-MS. Even if it is at the margin of this tutorial review

  17. 3-Mercaptopropyltrimethoxysilane Modified Diatomite: Preparation and Application for Voltammetric Determination of Lead (II and Cadmium (II

    Directory of Open Access Journals (Sweden)

    Dinh Quang Khieu

    2017-01-01

    Full Text Available In this study, functionalized diatomite was prepared by grafting of 3-mercaptopropyltrimethoxysilane (MPTMS to diatomite (MPTMS-diatomite. The diatomite with thermal treatment from 100 to 700°C was functionalized by MPTMS under dry and humid conditions. The obtained MPTMS-diatomite was characterized by X-ray diffraction (XRD, thermal gravity-differential scanning calorimeter (TG-DSC, and Fourier transformation infrared (FT-IR. The results showed that an increase in treatment temperature seems to reduce the loading of MPTMS onto diatomite. The humidity of diatomite was favorable for the grafting of functional groups on the surface. The possible mechanisms of MPTMS loading to diatomite (MPTMS-diatomite were also proposed. The performance of a carbon paste electrode (CPE modified with MPTMS-diatomite in the simultaneous determination of Cd(II and Pb(II ions was addressed.

  18. Determination of rare earth elements in tomato plants by inductively coupled plasma mass spectrometry techniques.

    Science.gov (United States)

    Spalla, S; Baffi, C; Barbante, C; Turetta, C; Turretta, C; Cozzi, G; Beone, G M; Bettinelli, M

    2009-10-30

    In recent years identification of the geographical origin of food has grown more important as consumers have become interested in knowing the provenance of the food that they purchase and eat. Certification schemes and labels have thus been developed to protect consumers and genuine producers from the improper use of popular brand names or renowned geographical origins. As the tomato is one of the major components of what is considered to be the healthy Mediterranean diet, it is important to be able to determine the geographical origin of tomatoes and tomato-based products such as tomato sauce. The aim of this work is to develop an analytical method to determine rare earth elements (RRE) for the control of the geographic origin of tomatoes. The content of REE in tomato plant samples collected from an agricultural area in Piacenza, Italy, was determined, using four different digestion procedures with and without HF. Microwave dissolution with HNO3 + H2O2 proved to be the most suitable digestion procedure. Inductively coupled plasma quadrupole mass spectrometry (ICPQMS) and inductively coupled plasma sector field plasma mass spectrometry (ICPSFMS) instruments, both coupled with a desolvation system, were used to determine the REE in tomato plants in two different laboratories. A matched calibration curve method was used for the quantification of the analytes. The detection limits (MDLs) of the method ranged from 0.03 ng g(-1) for Ho, Tm, and Lu to 2 ng g(-1) for La and Ce. The precision, in terms of relative standard deviation on six replicates, was good, with values ranging, on average, from 6.0% for LREE (light rare earth elements) to 16.5% for HREE (heavy rare earth elements). These detection limits allowed the determination of the very low concentrations of REE present in tomato berries. For the concentrations of REE in tomato plants, the following trend was observed: roots > leaves > stems > berries. Copyright 2009 John Wiley & Sons, Ltd.

  19. A review on the determination of isotope ratios of boron with mass spectrometry.

    Science.gov (United States)

    Aggarwal, Suresh Kumar; You, Chen-Feng

    2017-07-01

    The present review discusses different mass spectrometric techniques-viz, thermal ionization mass spectrometry (TIMS), inductively coupled plasma mass spectrometry (ICPMS), and secondary ion mass spectrometry (SIMS)-used to determine 11 B/ 10 B isotope ratio, and concentration of boron required for various applications in earth sciences, marine geochemistry, nuclear technology, environmental, and agriculture sciences, etc. The details of the techniques-P-TIMS, which uses Cs 2 BO 2 + , N-TIMS, which uses BO 2 - , and MC-ICPMS, which uses B + ions for bulk analysis or B - and B + ions for in situ micro-analysis with SIMS-are highlighted. The capabilities, advantages, limitations, and problems in each mass spectrometric technique are summarized. The results of international interlaboratory comparison experiments conducted at different times are summarized. The certified isotopic reference materials available for boron are also listed. Recent developments in laser ablation (LA) ICPMS and QQQ-ICPMS for solids analysis and MS/MS analysis, respectively, are included. The different aspects of sample preparation and analytical chemistry of boron are summarized. Finally, the future requirements of boron isotope ratios for future applications are also given. Presently, MC-ICPMS provides the best precision and accuracy (0.2-0.4‰) on isotope ratio measurements, whereas N-TIMS holds the potential to analyze smallest amount of boron, but has the issue of bias (+2‰ to 4‰) which needs further investigations. © 2016 Wiley Periodicals, Inc. Mass Spec Rev 36:499-519, 2017. © 2016 Wiley Periodicals, Inc.

  20. Determination of phospholipid regiochemistry by Ag(I) adduction and tandem mass spectrometry.

    Science.gov (United States)

    Yoo, Hyun Ju; Håkansson, Kristina

    2011-02-15

    Collision-activated dissociation (CAD) and infrared multiphoton dissociation (IRMPD) of Ag-adducted phospholipids were investigated as structural tools. Previously, determination of the acyl chains at the two phospholipid esterification sites has been performed based on the R(1)COO(-)/R(2)COO(-) ratio in negative ion mode CAD tandem mass spectrometry. However, the observed product ion ratio is dependent on the extent of unsaturation of the fatty acyl group at sn-2 as well as on the total chain length. Similarly, in positive ion mode CAD with/without alkaline or alkaline earth metal adduction, the ratio of product ions resulting from either R(1)COOH or R(2)COOH neutral losses is dependent on the nature of the phospholipid polar headgroup. Ag(+) ion chromatography, in which silver ions are part of the stationary phase, can provide information on double bond number/distribution as well as double bond configuration (cis/trans) because of interaction between Ag(+) ions and olefinic π electrons of fatty acids and lipids. We hypothesized that interactions between double bonds and Ag(+) may be utilized to also reveal phospholipid esterification site information in tandem mass spectrometry. CAD and IRMPD of Ag-adducted phospholipids with unsaturated fatty acids (R(x)COOH, x = 1 or 2) provided characteristic product ions, [R(x)COOH + Ag](+), and their neutral losses. The characteristic product ions and their abundances do not depend on the type of polar headgroup or the number of double bonds of unsaturated acyl chains. Tandem mass spectrometry of Cu-adducted phospholipids was also performed for comparison based on the Lewis acid and base properties of Cu(+) and phospholipid double bonds, respectively.

  1. Electrochemical preconcentration and hydride generation methods for trace determination of selenium by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Bye, R.

    1986-01-01

    The use of atomic absorption spectrometry in combination with two different preconcentration/separation techniques for the determination of trace concentrations of selenium is described. Electrochemical preconcentration onto a platinum electrode with a subsequent atomization of selenium is discussed briefly. Several parameters are considered such as the presence of depolarizers, and the temperature of the electrolyzed solutions. Special attention is payed to the efficiency of the atomization step, and a method to improve this is proposed. Applications of the technique to real samples are also reported. Secondly, the separation of the selenium as the volatile selenium hydride from the sample solution is considered. Several papers in this thesis deal with commonly occurring interferants as nickel and copper and with ways of minimizing or avoiding the interferring effects, whereas other papers relate to more theoretical aspects of the hydride generation process. New methods for the determination of selenium in technical samples with high contents of nickel and copper are also presented

  2. Determination of vanadium in mussels by electrothermal atomic absorption spectrometry without chemical modifiers

    Energy Technology Data Exchange (ETDEWEB)

    Saavedra, Y.; Fernandez, P. [Centro de Control do Medio Marino, Peirao de Vilaxoan s/n, Vilagarcia de Arousa, 36611 Pontevedra (Spain); Gonzalez, A. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Quimica, 15706, Santiago de Compostela (Spain)

    2004-05-01

    A method was developed for the quantitative determination of total vanadium concentration in mussels via electrothermal atomic absorption spectrometry (ETAAS). After the microwave digestion of the samples, a program using temperatures of 1600 C and 2600 C for ashing and atomization respectively, without any matrix modifiers, allowed us to obtain results that were satisfactory since they agreed closely with certified reference material values. The detection limit was 0.03 mg kg{sup -1} (dry weight), indicating that the method is suitable for the analysis of mussel samples. This determination was compared with matrix modifiers that have been reported previously. The method was applied to various cultivated and wild mussels from the Galician coast, yielding levels below 1 mg kg{sup -1} (wet weight). (orig.)

  3. Direct isotope determination of isotopically labelled lipids by field desorption mass spectrometry

    International Nuclear Information System (INIS)

    Lehmann, W.D.; Kessler, M.

    1982-01-01

    Lipids labelled with deuterium or carbon-14 have been investigated by field desorption mass spectrometry for determination of their degree of labelling. This application is demonstrated for free fatty acids, cholesterol, cholesteryl esters, triglycerides, and L-α-phosphatidylcholines. Comparison of the molecular ion groups of the non-labelled and of the labelled compounds enables a fast and reliable determination of the degree of labelling. For multiply labelled compounds the label distribution is also obtained from the molecular ion group. In addition, for cholesteryl esters and for phosphatidylcholines structurally significant fragment ions provide information about the position of the label. Several hundred nanograms of the compound are typically required for a single analysis with a relative standard error of 0.5-2% in the value calculated for atom% hydrogen-2 or for the specific carbon-14 activity. (orig.) [de

  4. Liquid-Liquid Extraction and Determination of Trace Elements in Iron Minerals by Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    Taseska, Milena; Stafilov, Trajche; Makreski, Petre; Jacimovic, Radojko; Jovanovski, Gligor

    2006-01-01

    Various trace elements (cadmium, chromium, cobalt, nickel, manganese) in some iron minerals were determined by flame (FAAS) and electrothermal atomic absorption spectrometry (ETAAS). The studied minerals were chalcopyrite (CuFeS 2 ), hematite (Fe 2 O 3 ) and pyrite (FeS 2 ). To avoid the interference of iron, a method for liquid-liquid extraction of iron and determination of investigated elements in the inorganic phase was proposed. Iron was extracted by diisopropyl ether in hydrochloride acid solution and the extraction method was optimized. Some parameters were obtained to be significantly important: Fe mass in the sample should not exceed 0.3 g, the optimal concentration of HCI should be 7.8 mol 1 -1 and ratio of the inorganic and organic phase should be 1: 1. The procedure was verified by the method of standard additions and by its applications to reference standard samples. The investigated minerals originate from various mines in the Republic of Macedonia. (Author)

  5. Hot vacuum extraction-isotopic dilution mass spectrometry for determination of hydrogen isotopes in zircaloys

    International Nuclear Information System (INIS)

    Shi, Y.; Leeson, P.K.; Wilkin, D.; Britton, A.; Macleod, R.

    2016-01-01

    A hot vacuum extraction-isotope dilution mass spectrometry (HVE-IDMS) was studied for determination of hydrogen isotopes in zirconium metal and alloys as nuclear reactor materials. A theoretical assessment of the completeness of the extraction of hydrogen isotopes under the chosen condition was carried out based on the hydrogen and deuterium solubility data for zirconium. The optimal isotopic spiking condition for conventional IDMS was further explored for the special case IDMS where the isotope abundance of the samples is varied and non-natural. Applying the optimal conditions, the accurate IDMS determination was realized. The agreement between the measured values and the certified or prepared values of standard reference materials and homemade standard materials validate the method developed. (author)

  6. Determination of moisture in black coal using pulsed nuclear magnetic resonance spectrometry

    International Nuclear Information System (INIS)

    Cutmore, N.G.; Sowerby, B.D.; Lynch, L.J.; Webster, D.S.

    1987-01-01

    Pulsed nuclear magnetic resonance (n.m.r.) spectrometry was investigated as a technique for moisture determination in fine product coal from eight Australian coal washeries. Measurements were made on samples of diameter 8 and 12 mm and length 10 and 120 mm at frequencies from 6.5 to 60 MHz. The ratio of intensities of the water and coal components in the free-induction decay signal can be used to determine moisture to within approx. 0.4-0.7 wt% over the range 0-26 wt% moisture, independent of sample density. This accuracy is independent of particle size (up to 1 mm) and little affected by coal rank, sample length or n.m.r. frequency. (author)

  7. 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

  8. Simultaneous determination of Magnolol and Honokiol by amino acid ionic liquid synchronous fluorescence spectrometry

    Science.gov (United States)

    Liu, Wei; Zhu, Xiashi

    2018-05-01

    A novel method based on amino acid ionic liquids (AAILs) as an additive synchronous fluorescence spectrometry is proposed for simultaneous determination of magnolol (MN) and honokiol (HN) in traditional Chinese medicine Houpu. The overlapping fluorescence spectrum of MN and HN could be completely separated in the AAILs medium. Experiment parameters (the type and concentration of AAILs, pH values and temperature) were discussed. The detection limits of MN and HN reached 1.46 ng/mL, 0.92 ng/mL and the recovery rates ranged from 98.6%-100.7%, 99.7%-100.6%, respectively. This methods was successfully employed for simultaneously determination of MN and HN in real samples. No significant differences could be found in the results of this method and the pharmacopoeia of People's Republic of China 2015 (Ch.P.2015). The experiment mechanisms were discussed by the Gaussian simulation and fluorescence quantum yield.

  9. Determination of trimethoprim in tissues using liquid chromatography-thermospray mass spectrometry.

    Science.gov (United States)

    Cannavan, A; Hewitt, S A; Floyd, S D; Kennedy, D G

    1997-11-01

    A method is described for the determination of the antibacterial drug trimethoprim in tissues. Minced tissue is homogenised with chloroform-acetone (1 + 1 v/v), filtered, and the filtrate evaporated to an oily residue using a rotary evaporator. The residue is redissolved in methanol-water-acetic acid (50 + 48.7 + 1.3 v/v) and any fats present are partitioned into hexane. The aqueous phase is analysed by liquid chromatography-thermospray mass spectrometry in positive mode with the protonated molecular ion at m/z 291 being monitored. Recoveries ranged between 60% in liver and 79% in muscle. The limit of determination was 25 micrograms kg-1 and the limit of detection was approximately 4 micrograms kg-1. The method is suitable for monitoring tissues taken under national surveillance schemes for veterinary drug residues.

  10. The determination of long life radionuclides by means of sector field ICP mass spectrometry

    International Nuclear Information System (INIS)

    Kerl, W.; Becker, J.S.; Dietze, H.J.; Dannecker, W.

    1996-01-01

    Different analytical processes for determining long life radionuclides by means of double-focussing sector field ICP mass spectrometry are described. In determining long life radionuclides by means of ICP-MS, on the one hand the analytical problem areas are in the interference of isobaric atom or molecule ions (eg: 151 Eu + - 151 Sm + , 79 Se + - 39 Ar 40 ArH + ) and on the other hand in the high detection limits when using commercial sample introduction systems (eg: For 129 I). An online coupling of HPLC and ICP-MS was built up for the separation of isobaric atom ions and was tested for the separation of isobaric atom ions and was tested for its efficiency in the separation of lanthanides. Special sample introduction systems for ICP-MS were developed for the analysis of 129 I, by which the sensitivity of detection can be appreciably improved compared to commercial sample introduction systems. (orig.) [de

  11. Determination of natural radioactivity in building materials used in Tunisian dwellings by gamma ray spectrometry

    International Nuclear Information System (INIS)

    Hizem, N.; Fredj, A. B.; Ghedira, L.

    2005-01-01

    The radioisotopic content of 17 samples of natural and manufactured building materials collected in Tunisia have been analysed by using gamma spectrometry. From the measured gamma ray spectra, activity concentrations are determined for 232 Th, 226 Ra, 235 U and 40 K. The total effective dose and the activity concentration index are calculated applying the dose criteria recommended by the European Union for building materials. The results of 226 Ra, 232 Th and 40 K found in Tunisian building materials indicate that radium and thorium concentrations do not exceed 40 Bq kg -1 , but potassium concentration varies between 50 and 1215 Bq kg -1 . The total effective dose rates per person indoors are determined to be between 0.07 and 0.86 mSv y -1 . Only two materials exceed the reference level of 0.3 mSv y -1 . The activity concentration index is <1. (authors)

  12. Determining picogram quantities of U in human urine by thermal ionization mass spectrometry

    International Nuclear Information System (INIS)

    Kelly, W.R.; Fassett, J.D.; Hotes, S.A.

    1987-01-01

    The U concentration in Standard Reference Material 2670 (Toxic Metals in Freeze-Dried Urine) and the urine of two preschool-age children were determined by measuring the chemically separated U by isotope dilution thermal ionization mass spectrometry using ion counting detection. This procedure can detect about 1% of the U atoms loaded into the mass spectrometer and has a total chemical blank of about 5 pg U. The U concentration in SRM 2670 was found to be 113 +/- 2 pg 238 U/ml (1 s). At this concentration, a 1-ml sample is sufficient for a determination with a total uncertainty of less than 5%. The U concentrations in the two children were 3.1 +/- 0.9 and 3.6 +/- 0.9 pg 238 U/g. These values suggest that the U concentration in urine of unexposed persons may be at this low level or lower

  13. Spectrophotometric determination of cobalt(II), nickel(II) and copper (II) with 1-(2 pyridylazo)-2-naphthol in micellar medium

    International Nuclear Information System (INIS)

    Shar, G.A.; Soomro, G.A.

    2004-01-01

    Spectrophotometric determination of cobalt(II), nickel(II) and copper(II) is carried out with 1-(2 pyridylazo)-2-naphthol as a complexing reagent in aqueous phase using non-ionic surfactant Tween 80. Beer's law is obeyed for Co(II), Ni(II) and Cu(II) over the range 0.5 - 4.0, 0.5 - 4.0 and 0.5 - 3.0 ngmL/sup -1/ with detection limit (2 σ) of 6.7, 3.2 and 3.9 ngmL/sup -1/. The max molar absorption, molar absorptivity, Sandell's sensitivity of Co(II), Ni(II) and Cu(II) are 580 nm, 570 nm and 555 nm; max (104 mol/sup -1/ cm /sup -1/) is 0.87, 1.8 and 1.6 and 6.8, 3.3 and 3.9 ng cm-2 respectively. The pH at which complex is formed for Co(II), Ni(II) and Cu(II) is 5, 5.5 and 6.5 respectively. The critical micelle concentration (CMC) of Tween 80 is 5%. The present method is compared with that of atomic absorption spectroscopy and no significant difference is noted between the two methods at 95% confidence level. The method has been applied to the determination of Co(II), Ni(II) and Cu(II) in industrial waste water and pharmaceutical samples. (author)

  14. SDSS-II: Determination of shape and color parameter coefficients for SALT-II fit model

    Energy Technology Data Exchange (ETDEWEB)

    Dojcsak, L.; Marriner, J.; /Fermilab

    2010-08-01

    In this study we look at the SALT-II model of Type IA supernova analysis, which determines the distance moduli based on the known absolute standard candle magnitude of the Type IA supernovae. We take a look at the determination of the shape and color parameter coefficients, {alpha} and {beta} respectively, in the SALT-II model with the intrinsic error that is determined from the data. Using the SNANA software package provided for the analysis of Type IA supernovae, we use a standard Monte Carlo simulation to generate data with known parameters to use as a tool for analyzing the trends in the model based on certain assumptions about the intrinsic error. In order to find the best standard candle model, we try to minimize the residuals on the Hubble diagram by calculating the correct shape and color parameter coefficients. We can estimate the magnitude of the intrinsic errors required to obtain results with {chi}{sup 2}/degree of freedom = 1. We can use the simulation to estimate the amount of color smearing as indicated by the data for our model. We find that the color smearing model works as a general estimate of the color smearing, and that we are able to use the RMS distribution in the variables as one method of estimating the correct intrinsic errors needed by the data to obtain the correct results for {alpha} and {beta}. We then apply the resultant intrinsic error matrix to the real data and show our results.

  15. 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

  16. Separation and determination of copper in bottled water samples by combination of dispersive liquid--liquid microextraction and microsample introduction flame atomic absorption spectrometry.

    Science.gov (United States)

    Citak, Demirhan; Tuzen, Mustafa

    2013-01-01

    A new and simple method for the determination of trace amounts of Cu(II) was developed by combination of dispersive liquid-liquid microextraction (DLLME) preconcentration and microsample introduction flame atomic absorption spectrometry. In this method, ethanol and chloroform were chosen as disperser and extraction solvents, respectively, and 1-nitroso-2-naphthol was used as the complexing agent. The factors affecting the extraction efficiency and determination of Cu(II), including extraction and disperser solvent nature and volume, concentration of the complexing agent, pH of the solution, extraction time, and matrix ions, were investigated. Under optimal conditions, the LOD for Cu(II) was 0.95 microg/L with a preconcentration factor of 70. The RSD was 1.9%. The accuracy of the developed DLLME method was verified by determination of Cu(II) in a certified reference material (NRCC-SLRS-4 river water). The relative error was -3.31%. The developed preconcentration procedure was successfully applied to the analysis of bottled drinking water samples.

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

    International Nuclear Information System (INIS)

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

    2011-08-01

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

  18. 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)

  19. Determination of parabens in serum by liquid chromatography-tandem mass spectrometry: Correlation with lipstick use.

    Science.gov (United States)

    Tahan, Gabriella Padovani; Santos, Nayara de Kássia Souza; Albuquerque, Ana Carolina; Martins, Isarita

    2016-08-01

    Parabens are the most widely used preservative and are considered to be relatively safe compounds. However, studies have demonstrated that they may have estrogenic activity, and there is ongoing debate regarding the safety and potential cancer risk of using products containing these compounds. In the present work, liquid chromatography-tandem mass spectrometry was applied to determine methylparaben and propylparaben concentrations in serum, and the results were correlated with lipstick application. Samples were analyzed using liquid-liquid extraction, followed by liquid chromatography-tandem mass spectrometry. The validation results demonstrated the linearity of the method over a range of 1-20 ng/mL, in addition to the method's precision and accuracy. A statistically significant difference was demonstrated between serum parabens in women who used lipstick containing these substances compared with those not using this cosmetic (p = 0.0005 and 0.0016, respectively), and a strong association was observed between serum parabens and lipstick use (Spearman correlation = 0.7202). Copyright © 2016 Elsevier Inc. All rights reserved.

  20. Applications of Tandem Mass Spectrometry in the Structure Determination of Permethylated Sialic Acid-containing Oligosaccharides

    International Nuclear Information System (INIS)

    Yoo, Eun Sun; Yoon, In Mo

    2005-01-01

    Sets of sialic acid-containing trisaccharides having different internal and terminal linkages have been synthesized to develop a sensitive method for analysis of the reducing terminal linkage positions. The trisaccharides, sialyl(α 2-3)Gal(β 1-3)GalNAc and sialyl(α 2-3)Gal(β 1-X)GlcNAc where X=3, 4 and 6, were synthesized and examined using electrospray ionization (ESI)-collision induced dissociation (CID) tandem mass spectrometry (MS/MS). The compounds chosen for this study are related to terminal groups likely to be found on polylactosamine-like glycoproteins and glycolipids which occur on the surface of mammalian cells. The purpose of this study is to develop tandem mass spectrometral methods to determine detailed carbohydrate structures on permethylated or partially methylated oligosaccharides for future applications on biologically active glycoconjugates and to exploit a faster method of synthesizing a series of structural isomeric oligosaccharides to be used for further mass spectrometry and instrumental analysis

  1. Stable carbon isotopic composition of gasolines determined by isotope ratio monitoring gas chromatography mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Smallwood, B.J.; Philp, R.P.; Allen, J.D. [University of Oklahoma, Norman, OK (United States). School of Geology and Geophysics

    2002-07-01

    A large number of underground gasoline storage facilities in the United States continuously leak gasoline into the subsurface, which makes gasoline a major groundwater contaminant. Gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) are used currently to characterize contaminated groundwater and soils. Correlations of contaminants with suspected source(s) are extremely difficult by these techniques because many gasolines have similar hydrocarbon distributions. The present study applied the technique of isotope ratio monitoring gas chromatography-mass spectrometry (irmGC-MS) to 19 gasoline samples from different areas of the USA. This allows a much better correlation of gasoline contaminants to source. Data obtained indicate a wide range of {sup {delta}}{sup 13}C values for 16 ubiquitous compounds in the gasolines. The majority of samples could be distinguished from each other on the basis of {sup {delta}}{sup 13}C hydrocarbon composition. The oxygenated additive methyl tertiary butyl ether (MTBE) was present in ten of the gasolines analyzed, and had a relatively narrow range of {sup {delta}}{sup 13}C values (-30.4 to -28.3 per mille). Preliminary investigations were also made to determine the extent of carbon isotopic fractionation after simple water washing and evaporation experiments. Results indicate that the majority of compounds did not undergo significant carbon isotopic fractionation as a result of these processes. (author)

  2. Daily cortisol production rate in man determined by stable isotope dilution/mass spectrometry

    International Nuclear Information System (INIS)

    Esteban, N.V.; Loughlin, T.; Yergey, A.L.; Zawadzki, J.K.; Booth, J.D.; Winterer, J.C.; Loriaux, D.L.

    1991-01-01

    Growth retardation as well as the development of Cushingoid features in adrenally insufficient patients treated with the currently accepted replacement dose of cortisol (33-41 mumol/day.m2; 12-15 mg/m2.day) prompted us to reevaluate the cortisol production rate (FPR) in normal subjects and patients with Cushing's syndrome, using a recently developed thermospray liquid chromatography-mass spectrometry method. The stable isotope [9,12,12-2H3]cortisol was infused continuously for 31 h at about 5% of the anticipated FPR. Blood samples were obtained at 20-min intervals for 24 h, spun, and pooled in 4-h groups. Tracer dilution in plasma was determined by liquid chromatography/mass spectrometry. The method was validated with controlled infusions in 6 patients with adrenal insufficiency. Results from 12 normal volunteers revealed a FPR of 27.3 +/- 7.5 mumol/day (9.9 +/- 2.7 mg/day) or 15.7 mumol/day.m2; 5.7 mg/m2. day. A previously unreported circadian variation in FPR was observed. Patients with Cushing's syndrome demonstrated unequivocal elevation of FPR and cortisol concentration correlated during each sample period in normal volunteers, indicating that cortisol secretion, rather than metabolism, is mainly responsible for changes in plasma cortisol. Our data suggest that the FPR in normal subjects may be lower than previously believed

  3. Determination of 20 synthetic dyes in chili powders and syrup-preserved fruits by liquid chromatography/tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Chia-Fen Tsai

    2015-09-01

    Full Text Available A liquid chromatography/tandem mass spectrometry (LC-MS/MS method is developed to simultaneously determine 20 synthetic dyes (New Coccine, Indigo Carmine, Erythrosine, Tartrazine, Sunset Yellow FCF, Fast Green FCF, Brilliant Blue FCF, Allura Red AC, Amaranth, Dimethyl Yellow, Fast Garnet GBC, Para Red, Sudan I, Sudan II, Sudan III, Sudan IV, Sudan Orange G, Sudan Red 7B, Sudan Red B, and Sudan Red G in food samples. This method offers high sensitivity and selectivity through the selection of two fragment ion transitions under multiple reaction monitoring mode to satisfy the requirements of both quantitation and qualitation. Using LC-MS/MS, the newly developed extraction protocol used in this study is rapid and simple and does not require the use of solid-phase extraction cartridges. The linearities and recoveries of the method are observed at the concentration range of 0.10–200 μg/kg and more than 90% for all dyes, respectively. The method has been successfully applied to screen 18 commercial chili powders and six commercial syrup-preserved fruits purchased from retail establishments in Taipei City. The results show that three legal food dyes, Tartrazine, and/or Sunset Yellow FCF, and/or New Coccine, are present in some syrup-preserved fruits. Amaranth, an illegal food dye in certain countries but declared illegal in Taiwan, is found in an imported syrup-preserved fruit.

  4. Flow injection analysis-flame atomic absorption spectrometry system for indirect determination of sulfite after on-line reduction of solid-phase manganese (IV) dioxide reactor.

    Science.gov (United States)

    Zare-Dorabei, Rouholah; Boroun, Shokoufeh; Noroozifar, Meissam

    2018-02-01

    A new and simple flow injection method followed by atomic absorption spectrometry was developed for indirect determination of sulfite. The proposed method is based on the oxidation of sulfite to sulphate ion using solid-phase manganese dioxide (30% W/W suspended on silica gel beads) reactor. MnO 2 will be reduced to Mn(II) by sample injection in to the column under acidic carrier stream of HNO 3 (pH 2) with flow rate of 3.5mLmin -1 at room temperature. Absorption measurement of Mn(II) which is proportional to the concentration of sulfite in the sample was carried out by atomic absorption spectrometry. The calibration curve was linear up to 25mgL -1 with a detection limit (DL) of 0.08mgL -1 for 400µL injection sample volume. The presented method is efficient toward sulfite determination in sugar and water samples with a relative standard deviation (RSD) less than 1.2% and a sampling rate of about 60h -1 . Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Comparison of STIM and particle backscattering spectrometry mass determination for quantitative microanalysis of cultured cells

    International Nuclear Information System (INIS)

    Deves, G.; Ortega, R.

    2001-01-01

    In biological sample microanalysis, a mass-normalisation method is commonly used as a quantitative index of elemental concentrations determined by particle-induced X-ray emission (PIXE). The organic mass can either be determined using particle backscattering spectrometry (BS) or scanning transmission ion microscopy (STIM). However, the accuracy of quantitative microanalysis in samples such as cultured cells is affected by beam-induced loss of organic mass during analysis. The aim of this paper is to compare mass measurements determined by particle BS or by STIM. In order to calibrate STIM and BS analyses, we measured by both techniques the thickness of standard foils of polycarbonate (3 and 6 μm), Mylar[reg] (4 μm), Kapton[reg] (7.5 μm) and Nylon[reg] (15 μm), as well as biological samples of mono-layered cultured cells. Non-damaging STIM analysis of samples before PIXE irradiation is certainly one of the most accurate ways to determine the sample mass, however, this requires strong experimental handling. On the other hand, BS performed simultaneously to PIXE is the simplest method to determine the local mass in polymer foils, but appears less accurate in the case of cultured cells

  6. [Rapid determination of 8 urinary carbamate pesticides by liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Liu, Hualiang; Wang, Yuan; Zhu, Baoli

    2015-11-01

    To establish a method for simultaneously determining the urinary concentrations of 8 carbamate pesticides. After being purified by acetonitrile precipitation, urine samples were transferred to a liquid chromatography-tandem mass spectrometry system, and the concentrations of 8 carbamate pesticides were determined by external standard method. A C18 column was used for ultra-high-performance liquid chromatography; methanol/ammonium acetate solution was used as the mobile phase for gradient elution; the mass spectrometer was operated in a multi-reaction monitoring mode. The calibration curves were linear when the urinary concentrations of these carbamate pesticides were 20~800 µg/L, and the recovery rates were 61.0%~121% at spiked levels of 20, 200 and 800 µg/L, with a relative standard deviation of 1.7%~5.5%. This determination method meets the Guide for establishing occupational health standards-part 5: Determination methods of chemicals in biological materials, and can be used for simultaneous determination of 8 carbamate pesticides in the urine of poisoning patients.

  7. Utilization of electrodeposition for electrothermal atomic absorption spectrometry determination of gold

    International Nuclear Information System (INIS)

    Konecna, Marie; Komarek, Josef

    2007-01-01

    Gold was determined by electrothermal atomic absorption spectrometry after electrochemical preconcentration on the graphite ridge probe used as a working electrode and sample support. The probe surface was electrochemically modified with Pd, Re and the mixture of both. The electrolysis of gold was performed under galvanostatic control at 0.5 mA. Maximum pyrolysis temperature for the probe surface modified with Pd was 1200 deg. C, with Re 1300 deg. C. The relative standard deviation for the determination of 2 μg l -1 Au was not higher than 5.6% (n = 8) for 2 min electrodeposition. The sensitivity of gold determination was reproducible for 300 electrodeposition and atomization cycles. When the probe surface was modified with a mixture of Pd and Re the detection limit was 31 ng l -1 for 2 min electrodeposition, 3.7 ng l -1 for 30 min, 1.5 ng l -1 for 1 h and 0.4 ng l -1 for 4 h electrodeposition, respectively. The procedure was applied to the determination of gold in river water samples. The relative standard deviation for the determination of 2.5 ng l -1 Au at 4 h electrodeposition time at 0.5 mA was 7.5%

  8. Determination of trace amounts of boron in steel by high frequency plasma torch spectrometry

    International Nuclear Information System (INIS)

    Akiyoshi, Takanori; Tsukamoto, Takako

    1978-01-01

    Trace amount of boron in steel were determined by means of emission spectrometry using high frequency plasma torch. The sensitivity of this method depended on the kind of solvent used, and methyl alcohol gave the best sensitivity. The determination limit of boron in methanol was 0.002 μg/ml. The established method utilized the high sensibility of the plasma torch and the easy distillation of boron in methanol as trimethyl-borate (B(OCH 3 ) 3 ). The sample was dissolved by acids and dehydrated by hot H 2 SO 4 and H 3 Po 4 . After cooling and addition of methanol (60 ml), the solution was distilled to obtain 40 ml of the distillate. The amount of boron in the distillate was determined by the intensity of the spectral line of B 2497.73 A excited by plasma torch. This method was rapid and accurate, particularly in determining trace amounts of boron and the determination range of boron in steel was 0.2 to 150 ppm. This method was also appliciable to stainless steels and other alloys. (auth.)

  9. Determination of non-ionic surfactants in technologic liquors and effluents by X-ray fluorescent spectrometry

    International Nuclear Information System (INIS)

    Dankowski, P.; Majda, J.

    1977-01-01

    The method has been worked out for determination of non-ionic surfactants in technological liquors and effluents, based on the X-ray fluorescent spectrometry with an initial concentration by means of the phosphomolybdic acid. The method is suitable for a quantitative determination of ethylene oxide adducts in a wide range of applicable concentrations, the trace-ones included. (M.Z.)

  10. Determination of Cr, Mn, Si, and Ni in carbon steels by optical emission spectrometry with spark source

    International Nuclear Information System (INIS)

    Garcia Gonzalez, M.A.; Pomares Alfonso, M.; Mora Lopez, L.

    1995-01-01

    Elemental composition of steels determines some important of his characteristic moreover it is necessary to obtain their quality certification. Analytical procedure has performed for determination of Cr, Mn, Si and Ni in carbon steels by optical emission spectrometry with spark source. reproducibility of results is 5-11 %. Exactitude has tested with results that have obtained by internationally recognised methods-

  11. Determination of Th and U by neutron activation for gamma spectrometry calibration in situ

    International Nuclear Information System (INIS)

    Nava M, F.; Rios M, C.; Mireles G, F.; Saucedo A, S.; Davila R, I.; Pinedo, J. L.; Landsberger, S.

    2012-10-01

    Using the analysis by neutron activation to determine the profile of the thorium and uranium concentration calibration factors were obtained for their use in the gamma spectrometry in situ. Three sites were selected (San Ramon, Villa de Cos y la Zacatecana) and the analysis by activation was development in the Laboratory of Nuclear Engineering Teaching of the Texas University in Austin with the nuclear reactor Ut-TRIGA. Starting from the gamma spectra in situ, the areas of normalized photo-pick of the radioisotopes were: 208 Tl and 228 Ac for the thorium series and 214 Pb and 214 Bi for the uranium series. The averages of the factors found in units of (cpm/Bq/Kg) are of 105.63±8.32 and 75.87±4.61 for the thorium and uranium, respectively. (Author)

  12. Combined discrete nebulization and microextraction process for molybdenum determination by flame atomic absorption spectrometry (FAAS)

    International Nuclear Information System (INIS)

    Oviedo, Jenny A.; Jesus, Amanda M.D. de; Fialho, Lucimar L.; Pereira-Filho, Edenir R.

    2014-01-01

    Simple and sensitive procedures for the extraction/preconcentration of molybdenum based on vortex-assisted solidified floating organic drop microextraction (VA-SFODME) and cloud point combined with flame absorption atomic spectrometry (FAAS) and discrete nebulization were developed. The influence of the discrete nebulization on the sensitivity of the molybdenum preconcentration processes was studied. An injection volume of 200 μ resulted in a lower relative standard deviation with both preconcentration procedures. Enrichment factors of 31 and 67 and limits of detection of 25 and 5 μ L -1 were obtained for cloud point and VA-SFODME, respectively. The developed procedures were applied to the determination of Mo in mineral water and multivitamin samples. (author)

  13. Determination of Chlorpyrifos in Human Blood by Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Xinhua Dai

    2017-01-01

    Full Text Available Gas chromatography-mass spectrometry method was developed for the qualitative and quantitative analyses of chlorpyrifos in human blood samples. The chlorpyrifos and parathion (internal standard in human blood were extracted with a mixed solvent of hexane and acetonitrile. Chlorpyrifos was well separated from the internal standard. The linear range of chlorpyrifos was 0.01–2 μg/ml in blood. The limit of detection and limit of quantification were estimated at 0.002 and 0.01 μg/ml, respectively. The inter- and intra-day precisions, accuracy, and recovery were assessed to verify this method. The results showed that the developed method is rapid, sensitive, and reliable. It is suitable for the determination of chlorpyrifos in forensic toxicological analysis and clinical diagnosis.

  14. Determination of dapsone in meat and milk by liquid chromatography tandem mass spectrometry

    International Nuclear Information System (INIS)

    Hadjigeorgiou, M.; Papachrysostomou, Ch.; Theodorou, Z.; Kanari, P.; Constantinou, S.

    2009-01-01

    Within the EU the use of dapsone (4,4-diaminodiphenylsulfone) is prohibited in food-producing animals and consequently it's included in the Annex IV of the Directive 90/2377/EC. A quantitative confirmatory method has been developed and validated according to the criteria defined in the Commission Decision 2002/657/EC, for the determination of dapsone in meat and milk. Samples, after homogenization in alkaline conditions and organic solvent extraction, were purified on silica gel solid phase extraction cartridges. The eluate was evaporated and redissolved in mobile phase and was analysed by liquid chromatography tandem mass spectrometry (LC-MS/MS) in positive electrospray ionisation (ESI) using deuterium labelled Sulphadimidine-d7 as internal standard. The calculated value for, decision limit, CCα is 0.12 μg kg -1 , and the detection capability; CCβ value is 0.16 μg kg -1

  15. Simultaneous Determination of Alkoxyalcohols in Wet Wipes Using Static Headspace Gas Chromatography and Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lee, So Jin; Pyo, Hee Soo; Chung, Bong Chul; Lee, Jeon Gae [KIST, Seoul (Korea, Republic of); Kim, Hai Dong [Kyung Hee University, Seoul (Korea, Republic of)

    2014-09-15

    Alkoxyalcohols are used as solvents or preservatives in various consumer products such as wet wipes. The metabolites of alkoxyalcohols are known to be chronically toxic and carcinogenic to animals. Thus, an analytical method is needed to monitor alkoxyalcohols in wet wipes. The aim of this study was to develop a simultaneous analytical method for 14 alkoxyalcohols using headspace gas chromatography coupled with mass spectrometry to analyze the wet wipes. This method was developed by comparing with various headspace extraction parameters. The linear calibration curves were obtained for the method (r2 > 0.995). The limit of detection of alkoxyalcohols ranged from 2 to 200 ng mL-1. The precision of the determinative method was less than 18.20% coefficient of variation both intra and inter days. The accuracy of the method ranged from 82.86% to 119.83%. (2-Methoxymethylethoxy)propanol, 2-phenoxyethanol, and 1-phenoxy-2-propanol were mainly detected in wet wipes.

  16. Thin coating thickness determination using radioisotope-excited x-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Del Castillo, Lorena A.; Calix, Virginia S.

    2001-01-01

    Three different approaches on thin coating thickness determination using a radioisotope-excited x-ray fluorescence spectrometry were demonstrated and results were compared. A standard of thin layer of gold (Au) on a nickel (Ni) substrate from the US National Bureau of Standards (with a nominal thickness of 0.300505 microns of at least 99.9% Au electrodeposited over 2 nils of Ni) on low carbon steel (1010) was analyzed using a Cd 109-excited XRF system. Au thickness computations were done using the (a) thin standard approach, (b) thick standard approach, and (c) x-ray absorption method (ASTM A754-79 1982). These three methods yielded results within the limit set by the American Society for Testing Materials (ASTM), which is +/-3%. Of the three methods, the thick standard yielded the best result with 0.124% error. (Author)

  17. Determination of rare-earth elements content in granitic rocks by argon plasma emission spectrometry

    International Nuclear Information System (INIS)

    Merodio, J.C.; Martinez, J.M.

    1990-01-01

    A method has been developed that enables the rare-earth elements in granitic rocks to be measured sequentially, using an inductively coupled plasma (ICP) source spectrometer with medium spectral resolution (0,02nm). The rocks were dissolved in an open system with a mixture of nitric-hydrofluoric-perchloric acids. Any residues remaining at this stage were removed by filtration and digested using a mini-fusion method with lithium tetraborate. Prior to the excitation in the spectrometer the rare-earth group was separated from other constituents using cation-exchange chromatography. A detailed study of spectral interferences and the evaluation of the detection limits have been performed. Five geochemical reference sample (granitic rocks) were analyzed and the obtained results agree favourably with recommended values and with reported determinations, using high spectral resolution ICP spectrometry. (Author) [es

  18. Determination of long-chain fatty acids in serum by gas chromatography coupled to mass spectrometry

    International Nuclear Information System (INIS)

    Nuevas Paz, Lauro; Camayd Viera, Ivette

    2014-01-01

    The quantification of long-chain fatty acids is fundamental for the diagnosis of several peroxisome disorders, particularly those in which the β-oxidation peroxisome of fatty acids is affected. In this work the implementation of an analytical method for the determination of these markers in serum by gas chromatography coupled to mass spectrometry is described. Besides, samples from patients with a diagnostic impression of adrenoleukodystrophy linked to the X chromosome were analyzed. The necessary experimental conditions were achieved for the separation and quantification of C22:0, C24:0 and C26:0 fatty acids in serum, which are biochemical markers of various peroxisome diseases. The application of this method allowed confirming the diagnosis of three patients with a diagnostic impression of adrenoleukodystrophy linked to the X chromosome. The application of the method in daily practice will allow the Cuban medical system to count on a new laboratory parameter for the diagnosis of peroxisome disorders

  19. Heavy metal determination by X-rays spectrometry for superficial sediments at Guantanamo bay

    International Nuclear Information System (INIS)

    Gelen, A.; Izquierdo; Corrales, W. Y.; Lopez, N.; Casanova, A. O.; Diaz, O.; Manso, M.V.; D Alessandro, K.; Reyes, E.; Toledo, C.; Ruiz, F.; Ramirez, M.; Beltran, J.; Martin, A.

    2007-01-01

    Twelve surface samples of the Guantanamo Bay (Cuba) were collected and analysed by X-Rays Spectrometry. Twenty one elements (Si, Ca, K, Na, P, S, Cl, Al, Fe, Mg, Ti, Mn, C, O, Cr, Cu, Ni, Co, Pb, V and Zn) have been determined. The distribution of the metals is associated with the wastewater from anthropogenic origin that receives the bay, mainly by fluvial currents. Multivariate statistical were used for the analysis of the results. Finally the results analysed were compared with the analysis performed by Engineering Centre for Environmental Management of Bays and Coasts (Cimab) using Inductively Coupled Plasma Emission (ICP) for some elements such as: Cr, Cu, Fe, Ni, Pb, V and Zn. The results show the Guantanamo Bay is less polluted than others Cuban Bays. (Author)

  20. Determination of impurities in magnesium and aluminium by X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Roca, M.; Diaz-Guerra, J.P.

    1979-01-01

    The determination of traces of Al, Cr, Cu, Fe, Mn, Ni, Pb, Si and of Bi, Cr, Cu, Fe, Ga, Mg, Mn, Ni, Pb, Si, Sn, Ti, V and Zn in samples of magnesium and aluminium, respectively, by means of X-ray fluorescence spectrometry, are studied. An automatic sequential spectrometer with an on-line computer for the treatment of data has been employed. The most suitable measurement parameters have been chosen for each element in order to achieve detection limits to a few p.p.m. For magnesium in the form of drillings the analyses are performed with satisfactory results for most impurities by pressing the samples into briquettes and employing metallic discs as standards. Correction methods for the spectral interferences of Ti on V, and V on Cr have been applied. (author)

  1. Determination of trace metals in nuclear-grade uranium dioxide by X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Salvador, V.L.R.; Imakuma, K.

    1988-04-01

    A method is described for the simultaneous determination of low concentrations of Ca, Cr, Cu, Fe, Mn and Ni in nuclear-grade uranium dioxide by X-ray fluorescence spectrometry, without the use of chemical treatment. The lower limits of detection range from 2 μg g -1 for nickel and manganese to 5 μg g -1 for copper. Samples are prepared in the form of double-layer pellets with boric acid as a binding agent. Standards are prepared in a U 3 O 8 matrix, which is more chemically stable than UO 2 and has similar matrix behaviour. The correlation coefficients for calibration curves are better than 0.999. Erros range from 2.4 % for chromium to 6.8 % for nickel. (author) [pt

  2. [Determination of inorganic elements in different parts of Sonchus oleraceus L by flame atomic absorption spectrometry].

    Science.gov (United States)

    Wang, Nai-Xing; Cui, Xue-Gui; Du, Ai-Qin; Mao, Hong-Zhi

    2007-06-01

    Flame atomic absorption spectrometry with air-acetylene flame was used for the determination of inorganic metal elements in different parts ( flower, leaf, stem and root) of Sonchus oleraceus L. The contents of Ca, Mg, K, Na, Fe, Mn, Cu, Zn, Cr, Co, Ni, Pb and Cd in the flower, leaf, stem and root of Sonchus oleraceus L were compared. The order from high to low of the additive weight (microg x g(-1)) for the 13 kinds of metal elements is as follows: leaf (77 213.72) > flower (47 927.15) > stem(42 280.99) > root (28 131.18). From the experimental results it was found that there were considerable differences in the contents of the metal elements in different parts, and there were richer contents of Fe, Zn, Mn and Cu in root and flower, which are necessary to human health, than in other parts.

  3. Determination of Aluminum in Dialysis Concentrates by Atomic Absorption Spectrometry after Coprecipitation with Lanthanum Phosphate.

    Science.gov (United States)

    Selvi, Emine Kılıçkaya; Şahin, Uğur; Şahan, Serkan

    2017-01-01

    This method was developed for the determination of trace amounts of aluminum(III) in dialysis concentrates using atomic absorption spectrometry after coprecipitation with lanthanum phosphate. The analytical parameters that influenced the quantitative coprecipitation of analyte including amount of lanthanum, amount of phosfate, pH and duration time were optimized. The % recoveries of the analyte ion were in the range of 95-105 % with limit of detection (3s) of 0.5 µg l -1 . Preconcentration factor was found as 1000 and Relative Standard Deviation (RSD) % value obtained from model solutions was 2.5% for 0.02 mg L -1 . The accuracy of the method was evaluated with standard reference material (CWW-TMD Waste Water). The method was also applied to most concentrated acidic and basic dialysis concentrates with satisfactory results.

  4. The determination of precious metals in geological samples by ICP - Mass Spectrometry

    International Nuclear Information System (INIS)

    Denoyer, E.; Ediger, R.; Hager, J.

    1989-01-01

    ICP - mass spectrometry with laser sampling has been used to determine gold directly in solid fire assay beads. A small portion of the lead bead is vaporized by Nd: YAG laser, and the resulting particulate material is passed by a flow of argon an ICP-mass spectrometer for quantitation of the gold content. Calibration with known geological materials gives linear calibration curves, and detection limits for gols are estimated to be 0.07 micrograms/gram in the original ore sample. The repeatability of the method is similar to that expected for traditional fire assay methods, and the analysis time for the solid lead bead is less than five minutes per sample. (author) [pt

  5. Determination of Te in soldering tin using continuous flowing electrochemical hydride generation atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    Jiang Xianjuan; Gan Wuer; Han Suping; He Youzhao

    2008-01-01

    An electrochemical hydride generation system was developed for the detection of Te by coupling an electrochemical hydride generator with atomic fluorescence spectrometry. Since TeH 2 is unstable and easily decomposes in solution, a reticular W filament cathode was used in the present system. The TeH 2 generated on the cathode surface was effectively driven out by sweeping gas from the cathode chamber. In addition, a low temperature electrochemical cell (10 deg. C) was applied to reduce the decomposition of TeH 2 in solution. The limit of detection (LOD) was 2.2 ng ml -1 and the relative standard deviation (RSD) was 3.9% for nine consecutive measurements of standard solution. This method was successfully employed for determination of Te in soldering tin material

  6. Serum/plasma methylmercury determination by isotope dilution gas chromatography-inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Baxter, Douglas C., E-mail: douglas.baxter@alsglobal.com [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Faarinen, Mikko [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Osterlund, Helene; Rodushkin, Ilia [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Division of Geosciences, Lulea University of Technology, 977 87 Lulea (Sweden); Christensen, Morten [ALS Scandinavia AB, Maskinvaegen 2, 183 53 Taeby (Sweden)

    2011-09-09

    Highlights: {center_dot} We determine methylmercury in serum and plasma using isotope dilution calibration. {center_dot} Separation by gas chromatography and detection by inductively coupled plasma mass spectrometry. {center_dot} Data for 50 specimens provides first reference range for methylmercury in serum. {center_dot} Serum samples shown to be stable for 11 months in refrigerator. - Abstract: A method for the determination of methylmercury in plasma and serum samples was developed. The method uses isotope dilution with {sup 198}Hg-labeled methylmercury, extraction into dichloromethane, back-extraction into water, aqueous-phase ethylation, purge and trap collection, thermal desorption, separation by gas chromatography, and mercury isotope specific detection by inductively coupled plasma mass spectrometry. By spiking 2 mL sample with 1.2 ng tracer, measurements in a concentration interval of (0.007-2.9) {mu}g L{sup -1} could be performed with uncertainty amplification factors <2. A limit of quantification of 0.03 {mu}g L{sup -1} was estimated at 10 times the standard deviation of concentrations measured in preparation blanks. Within- and between-run relative standard deviations were <10% at added concentration levels of 0.14 {mu}g L{sup -1}, 0.35 {mu}g L{sup -1} and 2.8 {mu}g L{sup -1}, with recoveries in the range 82-110%. Application of the method to 50 plasma/serum samples yielded a median (mean; range) concentration of methylmercury of 0.081 (0.091; <0.03-0.19) {mu}g L{sup -1}. This is the first time methylmercury has been directly measured in this kind of specimen, and is therefore the first estimate of a reference range.

  7. Capillary electrophoresis tandem mass spectrometry determination of glutamic acid and homocysteine's metabolites: Potential biomarkers of amyotrophic lateral sclerosis.

    Science.gov (United States)

    Cieslarova, Zuzana; Lopes, Fernando Silva; do Lago, Claudimir Lucio; França, Marcondes Cavalcante; Colnaghi Simionato, Ana Valéria

    2017-08-01

    Amyotrophic lateral sclerosis (ALS) is a neurodegenerative disease that affects both lower and upper motor neurons, leading to muscle atrophy, paralysis, and death caused by respiratory failure or infectious complications. Altered levels of homocysteine, cysteine, methionine, and glutamic acid have been observed in plasma of ALS patients. In this context, a method for determination of these potential biomarkers in plasma by capillary electrophoresis tandem mass spectrometry (CE-MS/MS) is proposed herein. Sample preparation was carefully investigated, since sulfur-containing amino acids may interact with plasma proteins. Owing to the non-thiol sulfur atom in methionine, it was necessary to split sample preparation into two methods: i) determination of homocysteine and cysteine as S-acetyl amino acids; ii) determination of glutamic acid and methionine. All amino acids were separated within 25min by CE-MS/MS using 5molL -1 acetic acid as background electrolyte and 5mmolL -1 acetic acid in 50% methanol/H 2 O (v/v) as sheath liquid. The proposed CE-MS/MS method was validated, presenting RSD values below 6% and 11% for intra- and inter-day precision, respectively, for the middle concentration level within the linear range. The limits of detection ranged from 35 (homocysteine) to 268nmolL -1 (glutamic acid). The validated method was applied to the analysis of plasma samples from a group of healthy individuals and patients with ALS, showing the potential of glutamic acid and homocysteine metabolites as biomarkers of ALS. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Cadmium, copper, lead, and zinc determination in precipitation: A comparison of inductively coupled plasma atomic emission spectrometry and graphite furnace atomization atomic absorption spectrometry

    Science.gov (United States)

    Reddy, M.M.; Benefiel, M.A.; Claassen, H.C.

    1987-01-01

    Selected trace element analysis for cadmium, copper, lead, and zinc in precipitation samples by inductively coupled plasma atomic emission Spectrometry (ICP) and by atomic absorption spectrometry with graphite furnace atomization (AAGF) have been evaluated. This task was conducted in conjunction with a longterm study of precipitation chemistry at high altitude sites located in remote areas of the southwestern United States. Coefficients of variation and recovery values were determined for a standard reference water sample for all metals examined for both techniques. At concentration levels less than 10 micrograms per liter AAGF analyses exhibited better precision and accuracy than ICP. Both methods appear to offer the potential for cost-effective analysis of trace metal ions in precipitation. ?? 1987 Springer-Verlag.

  9. Determination of Trace Iron in Red Wine by Isotope Dilution Mass Spectrometry Using Multiple-Collector Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    Zhou Tao; Wang Jun; Lu Hai; Zhou Yuanjing; Li Haifeng

    2009-01-01

    This paper introduces determination of trace iron in red wine certified reference material by isotope dilution mass spectrometry (IDMS) method using a multiplecollector inductively coupled plasma mass spectrometry, equipped with a hexapole collision cell. The measurement procedure of iron isotopic abundance ratios was deeply researched. Reduced polyatomic ion interferences to iron isotopes ion by collision reaction using Ar and H 2 gas, high precise isotopic abundance ratios were achieved. Two relative measurement methods (ICP-MS and ICP-OES) were used to analyze trace iron in red wine. The results are compared with IDMS results, which indicate that they are accordant. The uncertainty analyses include each uncertainty factor in whole experiment and the uncertainty of used certified reference material and it shows that the procedure blank is not neglectable to detect limit and precision of the method. The establishment of IDMS method for analysis of trace iron in red wine supports the certification of certified reference materials. (authors)

  10. Determination of calcium in Mashhad city tap water by flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Mashhadian, N.V.

    2012-01-01

    Summary: Calcium in drinking water is one of the sources of calcium that may contribute significantly to the daily calcium intake. In this study, the samples of tap water were randomly taken from five zones of Mashhad city. Calcium concentration was determined by flame atomic absorption spectrometry (FAAS) technique. The precision of the method was evaluated. The CV% of 6 replicate determinations at 5 macro g/ml Ca was 4.2 in one day and 4.5, among 6 consecutive days. The recovery of spiked samples (98.7%) also showed that the proposed method is reliable for the determination of amounts of calcium in water samples. The mean of calcium in tap water in the city of Mashhad was 52.61+-12.91 (SD) macro g/ml. At present, the amount of calcium in Mashhad tap waters is within the national standard. However, due to the climate and environmental changes, determination of calcium in tap water of Mashhad in different seasons is recommended. (author)

  11. Cold excitation and determination of hydrogen sulfide by dielectric barrier discharge molecular emission spectrometry.

    Science.gov (United States)

    Wu, Zhongchen; Jiang, Jie; Li, Na

    2015-11-01

    A low-temperature microplasma generated in a dielectric barrier discharge (DBD) was used as a radiation source for the excitation of hydrogen sulfide and its determination by molecular emission spectrometry (MES). The excitation/emission chamber was enclosed to eliminate spectral interference from ambient air. The spectral emission lines of hydrogen sulfide were clearly discriminated from the background spectrum, and the emission line at 365.06 nm was selected for parameter optimization and quantitative analysis. The S(2-) ions in aqueous samples were reacted with acid to generate hydrogen sulfide and then determined. The experimental parameters affecting the determination of hydrogen sulfide and S(2-) were optimized. The limits of detection were 1.4 mg m(-3) for H2S and 11.2 mg L(-1) for S(2-). The repeatability of the method was satisfactory, as the RSD values were 2.3% for H2S and 1.8% for S(2-). The enclosed DBD-MES system was demonstrated to be a useful tool for the determination of hydrogen sulfide in gas samples and S(2-) in aqueous samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. [Determination of 21 fragrance allergens in toys by gas chromatography-ion trap mass spectrometry].

    Science.gov (United States)

    Lü, Qing; Zang, Qing; Bai, Hua; Li, Haiyu; Kang, Suyuan; Wang, Chao

    2012-05-01

    A method of gas chromatography-ion trap mass spectrometry (GC-IT-MS) was developed for the determination of 21 fragrance allergens in sticker toys, plush toys and plastic toys. The experimental conditions, such as sample pretreatment conditions, and the analytical conditions of GC-IT-MS, were optimized. The sticker toy samples and plush toy samples were extracted with acetone by ultrasonic wave, and the extracts were separated on an Agilent HP-1 MS column (50 m x 0.2 mm x 0.5 microm), then determined by IT-MS and quantified by external standard method. The plastic toy samples were extracted by the dissolution-precipitation approach, cleaned up with an Envi-carb solid phase extraction column and concentrated by rotary evaporation and nitrogen blowing, then determined by GC-IT-MS and quantified by external standard method. The calibration curves showed good linearity in the range of 0.002-50 mg/L with the correlation coefficients greater than 0.996 8. The limits of quantification (LOQ, S/N > 10) were 0.02-40 mg/kg. The average recoveries of the target compounds spiked in the sample at three concentration levels were in the range of 82.2%-110.8% with the relative standard deviations (RSDs) of 0.6%-10.5%. These results show that this method is accurate and sensitive for the qualitative and quantitative determination of the 21 fragrance allergens in the 3 types of toys.

  13. Progress in determination of long-lived radionuclides by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

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

    2000-01-01

    Mass spectrometric methods (such as inductively coupled plasma mass spectrometry - ICP-MS and laser ablation (LA)-ICP-MS) with their ability to provide a very sensitive multielemental and precise isotopic analysis have become established for the determination of radionuclides in quite different sample materials. The determination of long-lived radionuclides is of increasing interest for the characterization of radioactive waste materials and for the detection of radionuclide contamination in environmental materials in which several radioactive nuclides are present from fallout due to nuclear weapons testing, nuclear power plants or nuclear accidents. Due to its multielement capability, excellent sensitivity, low detection limits (up to sub pg I 1 range), very good precision, easy sample preparation and measurement procedures ICP-MS of aqueous solutions has been increasingly applied for the ultrasensitive determination of long-lived radionuclides such as 99 Tc, 129 I, 230 Th, 232 Th, 234 U, 235 U, 236 U, 239 Pu, 240 Pu and 241 Am and precise isotope ratio measurements of U,Th and Pu. The application especially of microanalytical methods (analysis of some MU by flow injection and on-line coupling techniques as capillary electrophoresis (CE-ICP-MS) or HPLC-ICP-MS) for the precise determination nuclide abundances and concentration of long-lived radionuclides at ultra trace concentration levels in radioactive waste and also for controlling contamination from radioactive waste in the environment is a challenging task

  14. Determination of iron in natural and mineral waters by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    ROLANDAS KAZLAUSKAS

    2004-05-01

    Full Text Available Simple methods for the determination of Fe in natural and mineral waters by flame atomic absorption spectrometry (AAS are suggested. The results of the investigation of selectivity of the proposed AAS method proved that this procedure is not affected by high concentrations of other metals. The calibration graph for iron was linear at levels near the detection limit up to at least 0.10 mg ml-1. For the determination of microamounts of iron in mineral waters, an extraction AAS technique was developed. Iron was retained as Fe-8-oxyquinoline complex and extracted into chloroform. The optimal conditions for the extraction of the iron complex were determined. The AAS method was applied to the determination of Fe in mineral waters and natural waters from different areas of Lithuania. The accuracy of the developed method was sufficient and evaluated in comparison with a photometric method. The obtained results demonstrated that the procedure could be successfully applied for the analysis of water samples with satisfactory accuracy.

  15. 210Pb and 210Po determination in environmental samples using liquid scintillation counting and alpha spectrometry

    International Nuclear Information System (INIS)

    Perez Sanchez, D.; Martin Sanchez, A.; Jurado Vargas, M.

    2003-01-01

    A simple radiochemical procedure has been developed to determine 210 Pb and 210 Po in environmental samples from the same matrix. Sediment samples are decomposed by leaching with mineral acids or by microwave digestion, while water samples are pre-concentrated. One part of the resulting solution, spiked with 209 Po, is used for 210 Po determination by spontaneous deposition onto nickel disks (a-spectrometry). The other part is assayed for 210 Pb, separating the Pb either by anion-exchange (sediment samples), or by solvent extraction (water samples). The 210 Pb source is finally prepared by precipitation as oxalate and the chemical recovery determined by gravimetry. The 210 Pb activity concentration is determined by liquid scintillation. A standard sediment sample supplied by IAEA and spiked water samples were analysed to check the procedure. The 210 Pb and 210 Po measurements agreed well with the certifications, deviations being less than 10%. The mean recoveries for Pb and Po were (70±12)% and (77±8)% for sediments, and (70±10)% and (81±7)% for waters, respectively. (author)

  16. Rapid determination of radium-224/226 in seawater sample by alpha spectrometry.

    Science.gov (United States)

    Song, Lijuan; Yang, Yonggang; Luo, Maoyi; Ma, Yan; Dai, Xiongxin

    2017-05-01

    A new radiochemical separation method has been developed for rapid determination of alpha-emitting radium isotopes in seawater samples. This method can be applied for the measurement of 226 Ra in seawater samples when 224 Ra is used as tracer for chemical recovery correction. Likewise, 226 Ra can also be added as tracer for the determination of 224 Ra in seawater sample. In the method, radium is first pre-concentrated with hydrous titanium oxide (HTiO) and is purified by combined anion/cation exchange column chromatographic separation. The radium in the eluate is then co-precipitated with HTiO, dissolved in 9 M H 2 SO 4 , and followed through a BaSO 4 micro-precipitation step to prepare a thin-layer counting source to determine the activities of 224 Ra/ 226 Ra by alpha spectrometry. Replicate spike and blank samples were measured to evaluate the performance of the procedure. The minimum detectable activity concentration was determined to be 0.5 mBq·L -1 for 226 Ra and 0.4 mBq·L -1 for 224 Ra in 1 L of seawater sample with a counting time of 48 h. The method is a promising candidate for rapid measurement for alpha-emitting Ra isotopes in a large population of environment water samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

  17. Chlorine determination in (U, Pu)C fuel by total reflection X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Misra, Nand Lal; Dhara, Sangita; Mudher, Khush Dev Singh; Aggarwal, Suresh K.; Thakur, Uday Kumar; Shah, Dipti; Sawant, R.M.; Ramakumar, K.L.

    2007-01-01

    A Total Reflection X-ray Fluorescence (TXRF) method for the determination of chlorine in (U,Pu)C has been developed. The method involves calibration of the instrument with standard solutions and validation of TXRF determination of chlorine using synthetic standard solutions. Cl K α line excited with W L α source was used for TXRF determinations of chlorine. Chlorine present in trace amounts in (U,Pu)C samples was first separated by pyro hydrolysis. The evolved chlorine, in form of HCl, was collected in 5 mM NaOH solution. This solution was analyzed for chlorine by Total Reflection X-ray Fluorescence Spectrometry using cobalt as an internal standard. The TXRF detection limit of chlorine was found to be 3.6 pg with sample size of 30 μL. In order to assess the applicability of TXRF method for chlorine determinations in other nuclear materials, one U 3 O 8 trace element standard was also analyzed for chlorine in similar way. The precision of the method was found to be 25% (1 σ) at ng level in most of the cases. (author)

  18. Preliminary studies of laser-induced breakdown spectrometry for the determination of Ba, Cd, Cr and Pb in toys

    International Nuclear Information System (INIS)

    Godoi, Quienly; Santos, Dario; Nunes, Lidiane C.; Leme, Flavio O.; Rufini, Iolanda A.; Agnelli, Jose A.M.; Trevizan, Lilian C.; Krug, Francisco J.

    2009-01-01

    The performance of laser-induced breakdown spectrometry (LIBS) for the determination of Ba, Cd, Cr and Pb in toys has been evaluated by using a Nd:YAG laser operating at 1064 nm and an Echelle spectrometer with intensified charge-coupled device detector. Samples were purchased in different cities of Sao Paulo State market and analyzed directly without sample preparation. Laser-induced breakdown spectrometry experimental conditions (number of pulses, delay time, integration time gate and pulse energy) were optimized by using a Doehlert design. Laser-induced breakdown spectrometry signals correlated reasonably well with inductively coupled plasma optical emission spectrometry (ICP OES) concentrations after microwave-assisted acid digestion of selected samples. Thermal analysis was used for polymer identification and scanning electron microscopy to visualize differences in crater geometry of different polymers employed for toy fabrication. Results indicate that laser-induced breakdown spectrometry can be proposed as a rapid screening method for investigation of potentially toxic elements in toys. The unique application of laser-induced breakdown spectrometry for identification of contaminants in successive layers of ink and polymer is also demonstrated.

  19. Cu,Cr and As determination in preserved woods (Eucalyptus ssp.) by X-ray fluorescence spectrometries

    International Nuclear Information System (INIS)

    Pereira Junior, Sergio Matias

    2014-01-01

    Brazil produces around 2.2 millions of cubic meters of treated wood to meet the annual demand of railway, electric, rural and construction sectors. The most used wood species are eucalyptus (Eucalyptus ssp.) and pine (Pinus ssp.).The treated woods used for poles, sleepers, fence posts and plywoods should be according to Brazilian norms requirements. The most usual wood preservative products used in Brazil are CCA (chromated copper arsenate) and CCB (copper chromium and boron salt). The analytical methods, such as flame atomic absorption spectrometry (FAAS), plasma inductively coupled optical emission spectrometry (ICPOES) and X-ray fluorescence spectrometry (XRFS) have been used for the analytical control of those treatment processes. In this work, the eucalyptus trees (Eucalyptus ssp) samples was obtained from Minas Gerais State, Brazil, cut plantation areas. Under pressure, eucalyptus wood samples were submitted to different concentration of CCA solution reaching 3.9, 6.7, 9.1, 12.4 and 14.0 kg of CCA by m-³ sapwood retentions. Samples in cylinders and sawdust forms were obtained from treated wood samples. Copper, chromium and arsenic determination was performed using the energy dispersive X-ray fluorescence spectrometry (EDXRFS), portable X-ray fluorescence spectrometry (PXRFS), flame atomic absorption spectrometry (FAAS) and instrumental neutron activation analysis. In this work, the method of analysis, sensitivity, precision and accuracy performances of the related techniques were outlined. (author)

  20. Determination of thiopurine S-methyltransferase activity by hydrophilic interaction liquid chromatography hyphenated with mass spectrometry.

    Science.gov (United States)

    Pecher, Daniel; Dokupilová, Svetlana; Zelinková, Zuzana; Peppelenbosch, Maikel; Mikušová, Veronika; Mikuš, Peter

    2017-08-05

    Thiopurine S-methyltransferase (TPMT) plays an important role in the metabolism of thiopurines used in the therapy of inflammatory bowel diseases (IBD). In this work a new progressive method for the determination of TPMT activity in red blood cells lysates was developed. Analysis was carried out by means of hydrophilic interaction liquid chromatography (HILIC) hyphenated with mass spectrometry (MS). In comparison with reversed-phase high-performance liquid chromatography (RP-HPLC), that has been typically applied in determination of TPMT activity, the HILIC significantly improved the analytical signal provided by MS, shortened analysis time, and improved chromatographic resolution. The HILIC-HPLC-MS method was optimized and validated, providing favorable parameters of detection and quantitation limits (5.5 and 16.5pmol/mL, respectively), linearity (coefficient of determination 0.9999 in the range of 0.01-1.0nmol/mL), recovery and precision (93.25-100.37% with RSD 1.06-1.32% in the whole concentration range of QC samples). Moreover, in contrast to the conventional RP-HPLC-UV approach, the complex phenotype TPMT profiles can be reliably and without interferences monitored using the HILIC-HPLC-MS method. Such advanced monitoring can provide valuable detail information on the thiopurines (e.g. evaluating ratio of methylated and non-methylated 6-mercaptopurine) and, by that, TPMT action in biological systems before and during the therapy of IBD. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. The Determination of Thorium Contents in Urine With Neutron Activation Analysis and Alpha Spectrometry

    International Nuclear Information System (INIS)

    Mukh-Syaifudin

    2007-01-01

    Internal contamination by a radionuclide that entered into body through inhalation is most conveniently determined by using urine as sample. The aim of this research was developing a fast and simple method to determine thorium content in urine. The method was based on comparison of the activities between the sample added with and without standard thorium. Urine sample was divided into two parts, one of which was added with Th-232 standard, and then both were simultaneously proceed which was consist of decomposition of organic materials, precipitation of thorium by adding ammonium hydroxide, wash with aquadest, and then dissolution in nitric acid. The solution was then activated for 15 minutes with neutron flux of 10 12 ncm -2 second -1 and the activated product was co-precipitated two times with lanthanum carrier and sodium chloride by addition of ammonium hydroxide. Finally, the precipitate was dissolved in nitric acid and the gamma emission of Th-233 was analyzed with gamma spectrometry. The results of analysis showed that the concentration of four urine samples analyzed was below detection limit (BDL); 200.40; 273.88 and 22.03 pg/l, respectively. With the simple procedure, neutron activation analysis can be used in the determining the actinide contents in several types of biological sample. (author)

  2. Determination of cadmium in real water samples by flame atomic absorption spectrometry after cloud point extraction

    International Nuclear Information System (INIS)

    Naeemullah, A.; Kazi, T.G.

    2011-01-01

    Water pollution is a global threat and it is the leading world wide cause of death and diseases. The awareness of the potential danger posed by heavy metals to the ecosystems and in particular to human health has grown tremendously in the past decades. Separation and preconcentration procedures are considered of great importance in analytical and environmental chemistry. Cloud point is one of the most reliable and sophisticated separation methods for determination of traces quantities of heavy metals. Cloud point methodology was successfully employed for preconcentration of trace quantities of cadmium prior to their determination by flame atomic absorption spectrometry (FAAS). The metals react with 8-hydroxquinoline in a surfactant Triton X-114 medium. The following parameters such as pH, concentration of the reagent and Triton X-114, equilibrating temperature and centrifuging time were evaluated and optimized to enhance the sensitivity and extraction efficiency of the proposed method. Dilution of the surfactant-rich phase with acidified ethanol was performed after phase separation and the cadmium content was measured by FAAS. The validation of the procedure was carried out by spiking addition methods. The method was applied for determination of Cd in water samples of different ecosystems (lake and river). (author)

  3. Determination of uranium and polonium in Spa rus aura ta by alpha spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Luna P, M.; Renteria, M.; Montero C, M. E. [Centro de Investigacion en Materiales Avanzados, S. C., Miguel de Cervantes No. 120, Complejo Industrial Chihuahua, 31109 Chihuahua (Mexico); Manjon C, G.; Diaz, I., E-mail: elena.montero@cimav.edu.mx [Universidad de Sevilla, Escuela Tecnica Superior de Arquitectura, Departamento de Fisica Aplicada II, San Fernando No. 4, 41004 Sevilla (Spain)

    2012-06-15

    The aim of this study was optimizing conditions for the specific activities determination of some uranium-series radionuclides present in Spa rus aura ta by alpha spectrometry. Determinations of specific activities were conducted varying the type of digestion: acid attack on hot plate, controlled microwave digestion and acid attack after calcination of the sample. The latter procedure was applied only to the case of uranium isotopes determination. The variation in the isotope extraction method consisted of applying the techniques of liquid-liquid extracting using Tributyl phosphate or chromatographic UTEVA resin. Results depending on the type of treatment given to the samples were compared based on obtained chemical yields. The results reveal a higher bioaccumulation of polonium in the liver sample, with activities of 0.809, 2.495 and 2.439 Bq kg{sup -1} fresh wt compared with the fillet. The best chemical yields of polonium were close to 60% for samples that were digested by microwave. In the case of uranium the best chemical yields, close to 80% for fillet, were obtained with a previous calcination of the sample and using the UTEVA resin. (Author)

  4. Determination of uranium and polonium in Spa rus aura ta by alpha spectrometry

    International Nuclear Information System (INIS)

    Luna P, M.; Renteria, M.; Montero C, M. E.; Manjon C, G.; Diaz, I.

    2012-01-01

    The aim of this study was optimizing conditions for the specific activities determination of some uranium-series radionuclides present in Spa rus aura ta by alpha spectrometry. Determinations of specific activities were conducted varying the type of digestion: acid attack on hot plate, controlled microwave digestion and acid attack after calcination of the sample. The latter procedure was applied only to the case of uranium isotopes determination. The variation in the isotope extraction method consisted of applying the techniques of liquid-liquid extracting using Tributyl phosphate or chromatographic UTEVA resin. Results depending on the type of treatment given to the samples were compared based on obtained chemical yields. The results reveal a higher bioaccumulation of polonium in the liver sample, with activities of 0.809, 2.495 and 2.439 Bq kg -1 fresh wt compared with the fillet. The best chemical yields of polonium were close to 60% for samples that were digested by microwave. In the case of uranium the best chemical yields, close to 80% for fillet, were obtained with a previous calcination of the sample and using the UTEVA resin. (Author)

  5. Simulation of the isotopic ratio determination of plutonium by Ge(Li) gamma-ray spectrometry

    International Nuclear Information System (INIS)

    Baba, Hiroshi; Yagi, Hideyuki

    1979-09-01

    A simulation program ''SIMPUG'' was developed for assessing feasibility of the isotopic ratio determination of plutonium by Ge(Li) γ-ray spectrometry. The program consists of (1) construction of the spectrum profiles for eight peak groupings of interest with a given set of isotopic compositions and by the use of the known nuclear data for emitting γ rays and (2) determination of the intensity of each participating nuclide following a presently developed algorithm of spectrum unfolding. Effects of various factors on the reliability of the results were examined with the simulation program. Accuracy of the results was found to be little affected by the change of the detector resolution if the spectrum was taken with sufficient expansion. Counting statistics was concluded to be the most essential factor for the precision of the results, while the aging effect was not found significant. Contamination of fission products beyond a certain level brought about fatal errors in the determined values, particularly in the case of minor components. (author)

  6. Determination of carbon in natural freshwater biofilms with total reflection X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

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

    2009-01-01

    There is a growing interest in determination of low Z elements, i.e., carbon to phosphorus, in biological samples. Total reflection X-ray fluorescence spectrometry (TXRF) has been already established as suitable trace element analytical method with low sample demand and quite good quantification limits. Recently, the determinable element range was extended towards Z = 6 (carbon). Biofilms can be used for biomonioring purposes in the aquatic environment. Besides the trace metals, especially the determination of the carbon content is important for the better understanding of the early stage of biofilm formation. For this, an ATI low Z spectrometer equipped with Cr-anode X-ray tube, multilayer monochromator, vacuum chamber, and a Si(Li) detector with ultra thin window was used. Biofilms were grown on two different artificial supports (granite and plexiglass), freeze dried, suspended in high purity water and analyzed. As an internal standard the natural titanium content of the biofilms was used. The accuracy of the method was checked by total carbon measurement using a combusting carbon analyzer.

  7. Determination of carbon in natural freshwater biofilms with total reflection X-ray fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ovari, M. [Department of Analytical Chemistry, Eoetvoes University, Budapest, H-1117, Budapest, Pazmany Peter stny. 1/a. (Hungary)], E-mail: ovari@chem.elte.hu; Streli, C.; Wobrauschek, P. [Atominstitut of the Austrian Universities, TU-Wien, Stadionallee 2, A-1020, Wien (Austria); Zaray, Gy. [Department of Analytical Chemistry, Eoetvoes University, Budapest, H-1117, Budapest, Pazmany Peter stny. 1/a. (Hungary); Cooperative Research Centre of Environmental Chemistry, Eoetvoes University, Budapest, H-1117, Budapest, Pazmany Peter stny. 1/a. (Hungary)

    2009-08-15

    There is a growing interest in determination of low Z elements, i.e., carbon to phosphorus, in biological samples. Total reflection X-ray fluorescence spectrometry (TXRF) has been already established as suitable trace element analytical method with low sample demand and quite good quantification limits. Recently, the determinable element range was extended towards Z = 6 (carbon). Biofilms can be used for biomonioring purposes in the aquatic environment. Besides the trace metals, especially the determination of the carbon content is important for the better understanding of the early stage of biofilm formation. For this, an ATI low Z spectrometer equipped with Cr-anode X-ray tube, multilayer monochromator, vacuum chamber, and a Si(Li) detector with ultra thin window was used. Biofilms were grown on two different artificial supports (granite and plexiglass), freeze dried, suspended in high purity water and analyzed. As an internal standard the natural titanium content of the biofilms was used. The accuracy of the method was checked by total carbon measurement using a combusting carbon analyzer.

  8. Determination of impurity elements in steel by spark source mass spectrometry using powdered salts

    International Nuclear Information System (INIS)

    Saito, Morimasa; Sudo, Emiko

    1975-01-01

    Determination of impurity elements in steel by speak source mass spectrometry using powdered salts sample electrode was studied. The instrument used in this study was an AEI MS-7 mass spectrograph and the ion detector was Ilford Q2 photograph. Sample, (0.5--1) gram, was dissolved in hydrochloric acid (1 : 1) or nitric acid (1 : 1) together with yttrium of 1 microgram as the internal standard and then the solution was evaporated to dryness without baking. The salt residues were dried at 70 0 C for 30 minutes under vacuum. They were mixed with an equal amount of graphite powder for 5 minutes in a mixer mill, and then pressed into electrodes. When the relative sensitivity coefficient (Fe=1) was determined by using NBS 460 series standard samples, the results obtained by the proposed method for elements of Mo, Sn, Cu, Cr, Co, Ni, Mn, V, P, Si, and B were in good agreement with those obtained by the conventional method using solid sample electrodes (the solid method) and the precision of this method for 11 elements mentioned above was about 10% better than those of the solid method. However, both the accuracy and precision for elements of Nb, Ti, S and W were not good. This method was applied to the determination of impurities in NBS stainless steel and others. The relative standard deviations were within 20%. (auth.)

  9. Plutonium determination in seawater by inductively coupled plasma mass spectrometry: A review.

    Science.gov (United States)

    Cao, Liguo; Bu, Wenting; Zheng, Jian; Pan, Shaoming; Wang, Zhongtang; Uchida, Shigeo

    2016-05-01

    Knowing the concentration and isotopic ratio of Pu in seawater is of critical importance for assessing Pu contamination and investigating oceanic processes. In recent decades, the concentration of (239+240)Pu in seawater, particularly for surface seawater, has presented an exponential decreasing trend with time; thus determination of Pu in seawater has become a challenge nowadays. Here, we have summarized and critically discussed a variety of reported analytical methods for Pu determination in seawater sample based on inductively coupled plasma mass spectrometry (ICP-MS) analytical technique for rapid ultra-trace detection of Pu. Generally, pretreatments for seawater sample include co-precipitation, valence adjustment and chemical separation and purification procedures, all of which are comprehensively reviewed. Overall, the selected anion-exchange, extraction resins and operation condition are important for decontamination of interference from matrix elements and achieving satisfactory chemical yields. In addition, other mass spectrometric and radiometric detections are briefly addressed and compared with the focus on assessing ICP-MS. Finally, we discuss some issues and prospects in determination and application of Pu isotopes in seawater samples for future research. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Calibration of a Gamma Spectrometry System Used for the Determination of Cs-137 in Spanish Soils

    International Nuclear Information System (INIS)

    Barreraa, M.; Romero, M. L.; Valino, F.

    2008-01-01

    The document describes the methodology used at CIEMAT in order to determine, by gamma spectrometry, the background levels of the radionuclide Cs-137 in soils of the Spanish peninsular territory. the work is a part of an extensive research project developed jointly by the University of the Basque Country (UPV-EHU) and the CIEMAT, endellite Content and migration of radiocaesium and radiostrontium in Spanish soils, which is funded by the Plan I+D of the Spanish Nuclear Security Council (CSN). The objective of the project is to establish the reference levels of man-made radionuclides in Spanish soils, with respect to which the evaluation of a possible posterior accidental release of radioactive material could be appraised. The activity concentration of the fission products Cs-137 has been determined in 34 soil cores extracted from representative Spanish soils type zones. This publication describes the experimental system employed, its calibration, the particular conditions applied to perform the measurements, as well as the experimental validation of the methodology. The activity profiles and inventories of the radioactive element so obtained are also presented. The estimation of the background Cs-137 reference levels, will provide a basis for later applications as the study of the spatial distribution in the region, the determination of the correlation between the deposited activity and the meteorological conditions, or the calculation of the specific migration parameters of the radioactive elements in Mediterranean conditions. (Author) 15 refs

  11. Laser ablation inductively coupled plasma mass spectrometry for the determination of trace elements in soil

    International Nuclear Information System (INIS)

    Lee Yiling; Chang Chaochiang; Jiang Shiuhjen

    2003-01-01

    Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) has been applied to the determination of Cr, Cu, Zn, Cd and Pb in soil samples. The dried soil powder was pressed into a pellet for LA-ICP-MS analysis. Triton X-100 was added to work as the modifier to enhance the ion signals. The influences of instrument operating conditions (LA and ICP-MS) and pellet preparation on the ion signals were reported. For Cr determination, the ICP-MS was operated under the dynamic reaction cell mode which alleviated the mass overlap interference. Standard addition method and isotope dilution method were used for the quantitation work. The powder sample was spiked with suitable amounts of element standards and/or enriched isotopes, well-mixed, dried and then pressed into a pellet for LA-ICP-MS analysis. This method has been applied to determine Cr, Cu, Zn, Cd and Pb in NIST SRM 2711 Montana soil and NIST SRM 2709 San Joaquin soil reference materials. The analysis results were in agreement with the certified values. The precision between sample replicates was better than 5% with LA-ICP-MS method. Detection limits estimated from standard addition curves were approximately 0.9, 2, 9, 0.7 and 0.3 ng g -1 for Cr, Cu, Zn, Cd and Pb, respectively

  12. Determination of pyrrolizidine alkaloids in selected feed materials with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Kowalczyk, Ewelina; Kwiatek, Krzysztof

    2017-05-01

    1,2-Dehydropyrrolizidine alkaloids are known to be toxic to many animals and humans. To provide safety of feeds a method based on gas chromatography-mass spectrometry enabling the determination of a content of 1,2-unsaturated PAs in feed materials was developed. After extraction with aqueous solution of HCl and purification of the extract, 1,2-unsaturated alkaloids are reduced to their common backbone structures and subsequently derivatised with heptafluorobutyric anhydride (HFBA). The method was validated according to SANTE/11945/2015. All received parameters are consistent with the document requirements as recovery of a final compound retronecine derivative was from 81.8% to 94.4% when retrosine was used for spiking and from 72.7% to 85.5% when retrorsine N-oxide was spiked. The repeatability was calculated as relative standards deviation and ranged from 7.5% to 14.4%, for N-oxide was from 7.9% to 15.4%. The reproducibility was in the range from 14.2% to 16.3% and from 17.0% to 18.1% for free base and N-oxide respectively. The limit of quantification was determined as 10 µg kg - 1 . Good linearity of the method was obtained with coefficient of determination R 2  > 0.99. The method was applied to 35 silage and two hay samples analysis.

  13. Determining Membrane Protein-Lipid Binding Thermodynamics Using Native Mass Spectrometry.

    Science.gov (United States)

    Cong, Xiao; Liu, Yang; Liu, Wen; Liang, Xiaowen; Russell, David H; Laganowsky, Arthur

    2016-04-06

    Membrane proteins are embedded in the biological membrane where the chemically diverse lipid environment can modulate their structure and function. However, the thermodynamics governing the molecular recognition and interaction of lipids with membrane proteins is poorly understood. Here, we report a method using native mass spectrometry (MS), to determine thermodynamics of individual ligand binding events to proteins. Unlike conventional methods, native MS can resolve individual ligand binding events and, coupled with an apparatus to control the temperature, determine binding thermodynamic parameters, such as for protein-lipid interactions. We validated our approach using three soluble protein-ligand systems (maltose binding protein, lysozyme, and nitrogen regulatory protein) and obtained similar results to those using isothermal titration calorimetry and surface plasmon resonance. We also determined for the first time the thermodynamics of individual lipid binding to the ammonia channel (AmtB), an integral membrane protein from Escherichia coli. Remarkably, we observed distinct thermodynamic signatures for the binding of different lipids and entropy-enthalpy compensation for binding lipids of variable chain length. Additionally, using a mutant form of AmtB that abolishes a specific phosphatidylglycerol (PG) binding site, we observed distinct changes in the thermodynamic signatures for binding PG, implying these signatures can identify key residues involved in specific lipid binding and potentially differentiate between specific lipid binding sites.

  14. 210Pb and 210Po determination in environmental samples using liquid scintillation counting and alpha spectrometry

    International Nuclear Information System (INIS)

    Sanchez, D.P.; Sanchez, A.M.; Vargas, M.J.

    2002-01-01

    A simple radiochemical procedure has been developed to determine 210 Pb and 210 Po in environmental samples. After adding 209 Po tracer and Pb carrier, an aliquot of the sample is decomposed by microwave digestion or by evaporation with mineral acids (depending on the expected activity of the sample). Part of the leaching solution must be used for 210 Po determination, preparing a polonium source by spontaneous deposition onto a nickel disk. The quantitative recoveries are determined using a standard 209 Po tracer, and the activity concentration is determined by isotopic dilution alpha spectrometry. The remaining part of the leaching solution is used for 210 Pb determination by means of two alternative methods: lead can be retained from 1.5 M HCl by the DOWEX 1 X 8, Cl - form resin in a chromatographic column, and stripped with deionised water, or it can be separated by solvent extraction as a lead bromide complex with the organic compound ALIQUAT-336 in toluene (this second method is used preferably in water samples). The Pb source for measurement is prepared by precipitation as oxalate and the chemical recovery determined by gravimetry. The activity concentration of 210 Pb is calculated from the spectra measured with a liquid scintillation spectrometer. Several certified material samples supplied by IAEA were analysed to check the procedure. The measured values for 210 Pb and 210 Po were in good agreement with the certified values presenting deviations lower than 5%. Several environmental samples (river and well waters and also sediments) from zones impacted by Uranium mine exploitation were analysed using the described procedure. The mean yields of Pb and Po were (70 ± 10)% and (81 ± 7)% for waters and (70 ± 12)% and (77 ± 8)% for sediments. (author)

  15. Resin bead-thermal ionization mass spectrometry for determination of plutonium concentration in irradiated fuel dissolver solution

    International Nuclear Information System (INIS)

    Paul, Sumana; Shah, R.V.; Aggarwal, S.K.; Pandey, A.K.

    2015-01-01

    Determination of isotopic composition (IC) and concentration of plutonium (Pu) is necessary at various stages of nuclear fuel cycle which involves analysis of complex matrices like dissolver solution of irradiated fuel, nuclear waste stream etc. Mass spectrometry, e.g. thermal ionization mass spectrometry (TIMS) and inductively coupled plasma mass spectrometry (ICP-MS) are commonly used for determination of IC and concentration of plutonium. However, to circumvent matrix interferences, efficient separation as well as preconcentration of Pu is required prior to mass spectrometric analysis. Purification steps employing ion-exchange resins are widely used for the separation of Pu from dissolver solution or from mixture of other actinides e.g. U, Am. However, an alternative way is to selectively preconcentrate Pu on a resin bead, followed by direct loading of the bead on the filament of thermal ionization mass spectrometer

  16. Determination of fluoroquinolones in fish tissues, biological fluids, and environmental waters by liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Ziarrusta, Haizea; Val, Nahia; Dominguez, Haizea; Mijangos, Leire; Prieto, Ailette; Usobiaga, Aresatz; Etxebarria, Nestor; Zuloaga, Olatz; Olivares, Maitane

    2017-11-01

    This work describes the optimization, validation, and application in real samples of accurate and precise analytical methods to determine ten fluoroquinolones (FQs) (norfloxacin, enoxacin, pefloxacin, ofloxacin, levofloxacin, ciprofloxacin, danofloxacin, lomefloxacin, enrofloxacin, and sparfloxacin) in different environmental matrices, such as water (estuarine, seawater, and wastewater treatment plant effluent), fish tissues (muscle and liver), and fish biofluids (plasma and bile). The analysis step performed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was fully optimized to improve the separation and detection steps. The extraction of analytes from fish tissues was accomplished using focused ultrasound solid-liquid extraction using methanol/acetic acid (95:5 v/v) as extractant. The preconcentration and clean-up steps were optimized in terms of extraction efficiency and cleanliness and the best strategy for each matrix was selected: (i) Oasis HLB for seawater and muscle, (ii) liquid-liquid extraction combined with Oasis HLB for the lipid-rich liver, (iii) the combination of Evolute-WAX and Oasis HLB for estuarine water and wastewater treatment plant effluent, and (iv) molecular imprinted polymers for biofluids. The methods afforded satisfactory apparent recoveries (80-126%) and repeatability (RSD < 15%), except for sparfloxacin, which showed a lack of correction with the available isotopically labeled surrogates ([ 2 H 8 ]-ciprofloxacin and [ 2 H 5 ]-enrofloxacin). Ciprofloxacin, norfloxacin, and ofloxacin were detected in both water and fish liver samples from the Biscay Coast at concentrations up to 278 ng/L and 4 ng/g, respectively. To the best of our knowledge, this work is one of the few analyzing up to ten FQs and in so many fish tissues and biofluids. Graphical abstract Determination of fluoroquinolones in different environmental matrices, such as water (estuarine, seawater, and wastewater treatment plant effluent), fish tissues (muscle

  17. Feasibility of high-resolution continuum source molecular absorption spectrometry in flame and furnace for sulphur determination in petroleum products

    Science.gov (United States)

    Kowalewska, Zofia

    2011-07-01

    For the first time, high-resolution molecular absorption spectrometry with a high-intensity xenon lamp as radiation source has been applied for the determination of sulphur in crude oil and petroleum products. The samples were analysed as xylene solutions using vaporisation in acetylene-air flame or in an electrothermally heated graphite furnace. The sensitive rotational lines of the CS molecule, belonging to the ∆ν = 0 vibrational sequence within the electronic transition X 1∑ + → A 1П, were applied. For graphite furnace molecular absorption spectrometry, the Pd + Mg organic modifier was selected. Strong interactions with Pd atoms enable easier decomposition of sulphur-containing compounds, likely through the temporal formation of Pd xS y molecules. At the 258.056 nm line, with the wavelength range covering central pixel ± 5 pixels and with application of interactive background correction, the detection limit was 14 ng in graphite furnace molecular absorption spectrometry and 18 mg kg -1 in flame molecular absorption spectrometry. Meanwhile, application of 2-points background correction found a characteristic mass of 12 ng in graphite furnace molecular absorption spectrometry and a characteristic concentration of 104 mg kg -1 in flame molecular absorption spectrometry. The range of application of the proposed methods turned out to be significantly limited by the properties of the sulphur compounds of interest. In the case of volatile sulphur compounds, which can be present in light petroleum products, severe difficulties were encountered. On the contrary, heavy oils and residues from distillation as well as crude oil could be analysed using both flame and graphite furnace vaporisation. The good accuracy of the proposed methods for these samples was confirmed by their mutual consistency and the results from analysis of reference samples (certified reference materials and home reference materials with sulphur content determined by X-ray fluorescence

  18. Feasibility of high-resolution continuum source molecular absorption spectrometry in flame and furnace for sulphur determination in petroleum products

    Energy Technology Data Exchange (ETDEWEB)

    Kowalewska, Zofia, E-mail: zofia.kowalewska@obr.pl

    2011-07-15

    For the first time, high-resolution molecular absorption spectrometry with a high-intensity xenon lamp as radiation source has been applied for the determination of sulphur in crude oil and petroleum products. The samples were analysed as xylene solutions using vaporisation in acetylene-air flame or in an electrothermally heated graphite furnace. The sensitive rotational lines of the CS molecule, belonging to the {Delta}{nu} = 0 vibrational sequence within the electronic transition X{sup 1}{Sigma}{sup +} {yields} A{sup 1}{Pi}, were applied. For graphite furnace molecular absorption spectrometry, the Pd + Mg organic modifier was selected. Strong interactions with Pd atoms enable easier decomposition of sulphur-containing compounds, likely through the temporal formation of Pd{sub x}S{sub y} molecules. At the 258.056 nm line, with the wavelength range covering central pixel {+-} 5 pixels and with application of interactive background correction, the detection limit was 14 ng in graphite furnace molecular absorption spectrometry and 18 mg kg{sup -1} in flame molecular absorption spectrometry. Meanwhile, application of 2-points background correction found a characteristic mass of 12 ng in graphite furnace molecular absorption spectrometry and a characteristic concentration of 104 mg kg{sup -1} in flame molecular absorption spectrometry. The range of application of the proposed methods turned out to be significantly limited by the properties of the sulphur compounds of interest. In the case of volatile sulphur compounds, which can be present in light petroleum products, severe difficulties were encountered. On the contrary, heavy oils and residues from distillation as well as crude oil could be analysed using both flame and graphite furnace vaporisation. The good accuracy of the proposed methods for these samples was confirmed by their mutual consistency and the results from analysis of reference samples (certified reference materials and home reference materials with

  19. Determination of cadmium, lead and zinc in a candidate reference materials using isotope dilution mass spectrometry

    International Nuclear Information System (INIS)

    Munoz, Luis; Gras, Nuri; Quejido, Alberto; Fernandez, Marta

    2001-01-01

    The growing demands placed on analytical laboratories to ensure the reliability of their results, due to the introduction of systems of quality and to the increasing use of metrology in chemical measurements has led most laboratories to validate their methodologies and to control them statistically. One of the techniques used most often for these purposes is based on the use of reference materials. The proper use of these materials means that laboratory results may be traced to the International System of Units, analytical methodologies can be validated, instruments calibrated and chemical measurements harmonized. One of the biggest challenges in developing reference materials is that of certifying their properties, a process that has been defined as assigning a concentration value that is as close as possible to the true value together with its uncertainty. Organizations that produce reference materials use several options for their certification process, and among these is the use of a primary method. Among the primary methods recognized by the International Office of Weights and Measures is the Isotope Dilution Mass Spectrometry technique. The Chilean Nuclear Energy Commission, through its Reference Materials Program, has prepared a reference material of clam tissue, which has been chemically defined by different analytical methodologies applied in different national and international laboratories. This work describes the methodology developed with the CIEMAT for determining the elements lead, cadmium and zinc in the clam tissue reference material using the primary technique of Isotope Dilution Mass Spectrometry. The calculation is described for obtaining the spike amounts to be added to the sample and the procedure is explained for carrying out the isotopic exchange. The isotopic relationships 204 Pb/ 205 Pb, 111 Cd/ 114 Cd and 66 Zn/ 67 Zn were determined in an atomic emission spectrometer with a plasma source with the following characteristics: plasma

  20. Simultaneous preconcentration of Co(II), Ni(II), Cu(II), and Cd(II) from environmental samples on Amberlite XAD-2000 column and determination by FAAS

    International Nuclear Information System (INIS)

    Duran, Celal; Senturk, Hasan Basri; Elci, Latif; Soylak, Mustafa; Tufekci, Mehmet

    2009-01-01

    A new method for the preconcentration of some trace metals (Co, Ni, Cu, and Cd) as complexed with ammonium pyrrolidynedithiocarbamate (APDC) was developed using a mini-column filled with Amberlite XAD-2000 resin. Metal contents were determined by flame atomic absorption spectrometry (FAAS) after the metal complexes accumulated on the resin were eluted with 1 M HNO 3 in acetone. The effects of the analytical parameters such as sample pH, quantity of complexing agent, eluent type, resin quantity, sample volume, sample flow rate, and matrix ions were investigated on the recovery of the metals from aqueous solutions. The relative standard deviation (R.S.D.) of the method was <6%. The validation of the method was confirmed using two certified reference materials (CRM TMDW-500 Drinking Water and CRM SA-C Sandy Soil C). The method was successfully applied to some stream waters and mushroom samples from Eastern Black Sea Region (Trabzon city) of Turkey

  1. Determination of serum calcium levels by 42Ca isotope dilution inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Han, Bingqing; Ge, Menglei; Zhao, Haijian; Yan, Ying; Zeng, Jie; Zhang, Tianjiao; Zhou, Weiyan; Zhang, Jiangtao; Wang, Jing; Zhang, Chuanbao

    2017-11-27

    Serum calcium level is an important clinical index that reflects pathophysiological states. However, detection accuracy in laboratory tests is not ideal; as such, a high accuracy method is needed. We developed a reference method for measuring serum calcium levels by isotope dilution inductively coupled plasma mass spectrometry (ID ICP-MS), using 42Ca as the enriched isotope. Serum was digested with 69% ultrapure nitric acid and diluted to a suitable concentration. The 44Ca/42Ca ratio was detected in H2 mode; spike concentration was calibrated by reverse IDMS using standard reference material (SRM) 3109a, and sample concentration was measured by a bracketing procedure. We compared the performance of ID ICP-MS with those of three other reference methods in China using the same serum and aqueous samples. The relative expanded uncertainty of the sample concentration was 0.414% (k=2). The range of repeatability (within-run imprecision), intermediate imprecision (between-run imprecision), and intra-laboratory imprecision were 0.12%-0.19%, 0.07%-0.09%, and 0.16%-0.17%, respectively, for two of the serum samples. SRM909bI, SRM909bII, SRM909c, and GBW09152 were found to be within the certified value interval, with mean relative bias values of 0.29%, -0.02%, 0.10%, and -0.19%, respectively. The range of recovery was 99.87%-100.37%. Results obtained by ID ICP-MS showed a better accuracy than and were highly correlated with those of other reference methods. ID ICP-MS is a simple and accurate candidate reference method for serum calcium measurement and can be used to establish and improve serum calcium reference system in China.

  2. Determination of 5-fluorouracil in plasma with HPLC-tandem mass spectrometry

    NARCIS (Netherlands)

    van Kuilenburg, A. B. P.; van Lenthe, H.; Maring, J. G.; van Gennip, A. H.

    2006-01-01

    In this article, we describe a fast and specific method to measure 5FU with HPLC tandem-mass spectrometry. Reversed-phase HPLC was combined with electrospray ionization tandem mass spectrometry and detection was performed by multiple-reaction monitoring. Stable-isotope-labeled 5FU (1,3-15N2-5FU) was

  3. Incorporating Biological Mass Spectrometry into Undergraduate Teaching Labs, Part 2: Peptide Identification via Molecular Mass Determination

    Science.gov (United States)

    Arnquist, Isaac J.; Beussman, Douglas J.

    2009-01-01

    Mass spectrometry has become a routine analytical tool in the undergraduate curriculum in the form of GC-MS. While relatively few undergraduate programs have incorporated biological mass spectrometry into their programs, the importance of these techniques, as demonstrated by their recognition with the 2002 Nobel Prize, will hopefully lead to…

  4. Direct rare earth determination by inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Marin, Sergio; Cornejo, Silvia; Rojas, Jacqueline

    2003-01-01

    In the present work, the use of the inductively coupled plasma optical emission spectrometry (ICP-OES), for the sequential determination of Rare Earth elements in the metallurgical process samples is described. In the first place, the optimum parameters for the determination of the elements in study are established, like instrumental calibration, wavelengths spectral selection and interference of matrix. Next, the methodology for the digestion of solid samples (system of digestion with pressure) and the recovery of the interest elements are presented. Two material rocks as of reference Syenite SY3 are used. In order to assure the validity of the obtained data, the reference materials SY2 and SY3 were analyzed by means of two different techniques, ICP-OES and ICP-Mass, this last one was made by an international laboratory and a fusion with lithium metaborate was used with digestion method. Finally, the obtained results demonstrate that the reproducibility in the recovery of rare earth analyzed by both techniques is comparable, and that the methodology of digestion used for these elements is statistically valid (author)

  5. Application of ion mobility spectrometry for the determination of tramadol in biological samples

    Directory of Open Access Journals (Sweden)

    Ali Sheibani

    2014-12-01

    Full Text Available In this study, a simple and rapid ion mobility spectrometry (IMS method has been described for the determination of tramadol. The operating instrumental parameters that could influence IMS were investigated and optimized (temperature; injection: 220 and IMS cell: 190°C, flow rate; carrier: 300 and drift: 600 mL/minute, voltage; corona: 2300 and drift: 7000 V, pulse width: 100 μs. Under optimum conditions, the calibration curves were linear within two orders of magnitude with R2 ≥ 0.998 for the determination of tramadol in human plasma, saliva, serum, and urine samples. The limits of detection and the limits of quantitation were between 0.1 and 0.3 and 0.3 and 1 ng/mL, respectively. The relative standard deviations were between 7.5 and 8.8%. The recovery results (90–103.9% indicate that the proposed method can be applied for tramadol analysis in different biological samples.

  6. In-situ gamma spectrometry method for determination of environmental gamma dose

    International Nuclear Information System (INIS)

    Conti, Claudio de Carvalho

    1995-07-01

    This work tries to establish a methodology for germanium detectors calibration, normally used for in situ gamma ray spectrometry, for determining the environmental exposure rate in function of the energy of the incident photons. For this purpose a computer code has been developed, based on the stripping method, for the computational spectra analysis to calculate the contribution of the partial absorption of the gamma rays (Compton effect) in the active and nonactive parts of the detector. The resulting total absorption spectrum is then converted to fluence distribution in function of the energy for the photons reaching the detector, which is then used to calculate the exposure rate or kerma in air. The unfolding and fluency convention parameters are determined by detector calibration using point gamma sources. The method is validated by comparison of the results against the calculated exposure rate at a point of interest for the standards. This method is used for the direct measurement of the exposure rate distribution in function of the energy at the site, in situ measurement technic, leading to rapid results during an emergency situation and also used for indoor measurements. (author)

  7. [Simultaneous determination of ten organotin compounds in polyvinyl chloride plastics using gas chromatography-mass spectrometry].

    Science.gov (United States)

    Li, Ying; Li, Bin; Liu, Li; Zhang, Chen; Wu, Jingwu; Liu, Zhihong; Li, Xintian

    2009-01-01

    A rapid and effective gas chromatography coupled with mass spectrometry method has been developed systematically and studied for the simultaneous determination of 10 organotin compounds, dibutyltin-dichloride (DBT), n-butyltin-trichloride (MBT), triethyltinchloride (TET), fentin-chloride (TPhT), chlorotributylstannane (TBT), tri-n-propyltinchloride (TPrT), diphenyltin-dichloride (DPhT), tetrabutyltin (TeBT), di-n-octyltin-dichloride (DOT), phenyltin trichloride (MPhT)), in polyvinyl chloride (PVC) plastics. The PVC sample was dissolved with tetrahydrofuran and the polymer in the sample was precipitated with methanol, and then the target compounds were derivatized with sodium tetraethylborate and extracted with hexane under ultrasonication. The qualitative and quantitative analysis were carried out by GC-MS and the total ion chromatogram and selected ion chromatogram were obtained. The derivatization and extraction conditions, such as the derivatization time, derivatization pH value, dosages of derivatization reagent and precipitation reagent were optimized. The good linearities, recoveries and precisions were obtained. The linearity ranges were 0.5 - 50 mg/L. The linearity correlation coefficients of 10 organotin compounds were between 0.997 8 and 0.999 7. The average recoveries were 84.23% - 109.1% with relative standard deviations of 4.24% - 10.75%. The established method has been successfully applied to the determination of organotin compounds in PVC plastics.

  8. Determination of tellurium by hydride generation with in situ trapping flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Matusiewicz, H.; Krawczyk, M. [Politechn Poznanska, Poznan (Poland)

    2007-03-15

    The analytical performance of coupled hydride generation - integrated atom trap (HG-IAT) atomizer flame atomic absorption spectrometry (FAAS) system was evaluated for determination of Te in reference material (GBW 07302 Stream Sediment), coal fly ash and garlic. Tellurium, using formation of H{sub 2}Te vapors, is atomized in air-acetylene flame-heated IAT. A new design HG-IAT-FAAS hyphenated technique that would exceed the operational capabilities of existing arrangernents (a water-cooled single silica tube, double-slotted quartz tube or an 'integrated trap') was investigated. An improvement in detection limit was achieved compared with using either of the above atom trapping techniques separately. The concentration detection limit, defined as 3 times the blank standard deviation (3{sigma}), was 0.9 ng mL{sup -1} for Te. For a 2 min in situ preconcentration time (sample volume of 2 mL), sensitivity enhancement compared to flame AAS, was 222 fold, using the hydride generation atom trapping technique. The sensitivity can be further improved by increasing the collection time. The precision, expressed as RSD, was 7.0% (n = 6) for Te. The accuracy of the method was verified using a certified reference material (GBW 07302 Stream Sediment) by aqueous standard calibration curves. The measured Te contents of the reference material was in agreement with the information value. The method was successfully applied to the determination of tellurium in coal fly ash and garlic.

  9. {sup 222}Rn determination in water and brine samples using liquid scintillation spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Thiago C.; Oliveira, Arno H., E-mail: oliveiratco2010@gmail.com [Universidade Federal de Minas Gerais (DEN/UFMG), Belo Horizonte (Brazil). Departamento de Engenharia Nuclear; Monteiro, Roberto P.G.; Moreira, Rubens M., E-mail: rpgm@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN-CNEN-MG), Belo Horizonte, MG (Brazil)

    2017-07-01

    Liquid scintillation spectrometry (LSC) is the most common technique used for {sup 222}Rn determination in environmental aqueous sample. In this study, the performance of water-miscible (Ultima Gold AB) and immiscible (Optiscint) liquid scintillation cocktails has been compared for different matrices. {sup 241}Am, {sup 90}Sr and {sup 226}Ra standard solutions were used for LSC calibration. {sup 214}Po region was defined as better for both cocktails. Counting efficiency of 76 % and optimum PSA level of 95 for Ultima Gold AB cocktail, and counting efficiency of 82 % and optimum PSA level of 85 for Optiscint cocktail were obtained. Both cocktails showed similar results when applied for {sup 222}Rn activity determination in water and brine samples. However the Optiscint is recommended due to its quenching resistance. Limit of detection of 0.08 and 0.06 Bq l{sup -1} were obtained for water samples using a sample:cocktail ratio of 10:12 mL for Ultima Gold AB and Optiscint cocktails, respectively. Limit of detection of 0.08 and 0.04 Bq l{sup -1} were obtained for brine samples using a sample:cocktail ratio of 8:12 mL for Ultima Gold AB and Optiscint cocktails, respectively. (author)

  10. 222Rn determination in water and brine samples using liquid scintillation spectrometry

    International Nuclear Information System (INIS)

    Oliveira, Thiago C.; Oliveira, Arno H.

    2017-01-01

    Liquid scintillation spectrometry (LSC) is the most common technique used for 222 Rn determination in environmental aqueous sample. In this study, the performance of water-miscible (Ultima Gold AB) and immiscible (Optiscint) liquid scintillation cocktails has been compared for different matrices. 241 Am, 90 Sr and 226 Ra standard solutions were used for LSC calibration. 214 Po region was defined as better for both cocktails. Counting efficiency of 76 % and optimum PSA level of 95 for Ultima Gold AB cocktail, and counting efficiency of 82 % and optimum PSA level of 85 for Optiscint cocktail were obtained. Both cocktails showed similar results when applied for 222 Rn activity determination in water and brine samples. However the Optiscint is recommended due to its quenching resistance. Limit of detection of 0.08 and 0.06 Bq l -1 were obtained for water samples using a sample:cocktail ratio of 10:12 mL for Ultima Gold AB and Optiscint cocktails, respectively. Limit of detection of 0.08 and 0.04 Bq l -1 were obtained for brine samples using a sample:cocktail ratio of 8:12 mL for Ultima Gold AB and Optiscint cocktails, respectively. (author)

  11. Determination of cadmium in human urine by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Shimizu, Tokuo; Shijo, Yoshio; Sakai, Kaoru

    1981-01-01

    A trace amount of cadmium in human urine was determined by graphite furnace atomic absorption spectrometry. A urine sample (25 ml) was digested with 5 ml of HNO 3 and 30 ml of H 2 O 2 in a long-neck flask on a hot-plate (200 0 C), then diluted to 50 ml. The standard addition method was carried out before digesting. Ten μl of the resulted solution was injected into a tube treated with tungsten carbide, and the cadmium signal was measured with the ramp mode atomization. Interference induced by organic materials in urine was avoided by HNO 3 -H 2 O 2 digestion. Interference induced by inorganic salts could be reduced by 2-fold dilution and tungsten carbide treatment. The cadmium signal was separated sufficiently from the molecular absorption due to NaCl etc. by the ramp mode atomization. Since the blank level of H 2 O 2 was relatively high, the determination was limited to about 0.1 μg/l. The coefficient of variation was 1.76% at 0.36 μg/l in 24 h human urine (n = 4). The time required was (8 -- 10)h. The precision of this method was higher than those of direct methods, and the reasonable values of urine levels of cadmium were obtained. (author)

  12. Accelerator mass spectrometry 14C determination in CO2 produced from laser decomposition of aragonite.

    Science.gov (United States)

    Rosenheim, Brad E; Thorrold, Simon R; Roberts, Mark L

    2008-11-01

    The determination of (14)C in aragonite (CaCO(3)) decomposed thermally to CO(2) using an yttrium-aluminum-garnet doped neodymium laser is reported. Laser decomposition accelerator mass spectrometry (LD-AMS) measurements reproduce AMS determinations of (14)C from the conventional reaction of aragonite with concentrated phosphoric acid. The lack of significant differences between these sets of measurements indicates that LD-AMS radiocarbon dating can overcome the significant fractionation that has been observed during stable isotope (C and O) laser decomposition analysis of different carbonate minerals. The laser regularly converted nearly 30% of material removed into CO(2) despite it being optimized for ablation, where laser energy breaks material apart rather than chemically altering it. These results illustrate promise for using laser decomposition on the front-end of AMS systems that directly measure CO(2) gas. The feasibility of such measurements depends on (1) the improvement of material removal and/or CO(2) generation efficiency of the laser decomposition system and (2) the ionization efficiency of AMS systems measuring continuously flowing CO(2).

  13. [Determination of endogenous agmatine in rat plasma by isotope dilution-gas chromatography-mass spectrometry].

    Science.gov (United States)

    Qiu, Zhongli; Lin, Ying; Xiong, Zhili; Xie, Jianwei

    2014-07-01

    A method for the determination of endogenous agmatine in rat plasma was developed by isotope dilution-gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS). The plasma samples were analyzed after protein precipitation, evaporation, derivatization by hexafluoroacetone (HFAA), and clean-up on a Florisil SPE column. The GC-MS analysis utilized stable isotope d8-agmatine as internal standard. The samples after treatme were tested by negative chemical ionization with selected ion monitoring (SIM) which was set at m/z 492 (molecular ion of agmatine) and m/z 500 (molecular ion of internal standard). The limit of detection (LOD) of agmatine standard solution was 0.005 7 ng/mL. The calibration curve of the agmatine spiked in rat plasma showed a good linear relationship at the range of 1.14-57.0 ng/mL (r = 0.997). The recoveries of agmatine spiked in rat plasma ranged from 92.3% to 109.8%. Inter-day and intra-day precisions were less than 15%. The average concentration level of agmatine in rat plasma was (22 +/- 9) ng/mL, and there was no significant difference between male and female SD rats (p > 0.05). The method is high sensitive and specific, and can be used for the determination of endogenous agmatine in plasma. It provides a strong support for the subsequent research of agmatine.

  14. [Determination of five representative ultraviolet filters in water by gas chromatography-mass spectrometry].

    Science.gov (United States)

    Ding, Yiran; Huang, Yun; Zhao, Tingting; Cai, Qian; Luo, Yu; Huang, Bin; Zhang, Yuxia; Pan, Xuejun

    2014-06-01

    A method for the determination of five representative organic UV filters: ethylhexyl methoxycinnamate (EHMC), benzophenone-3 (BP-3), 4-methylbenzylidene camphor (4-MBC), octocrylene (OC), homosalate (HMS) in water was investigated. The method was ased on derivatization, solid phase extraction (SPE), followed by determination with gas chromatography-mass spectrometry (GC-MS). The variables involved in the derivatization of BP-3 and HMS were optimized, and SPE conditions were studied. For derivatization, 100 microL N,O-bis(trimethylsilyl) trifluoroacetamide (BSTFA) was used as derivatization reagent and reacted with BP-3 and HMS at 100 degrees C for 100 min. For SPE, the pH value of water sample was adjusted to 3-5. The Oasis HLB cartridges were employed and the solution of ethyl acetate and dichloromethane (1 : 1, v/v) was used as the eluting solvent, and good recoveries of the target compounds were obtained. The limits of detection (LODs) and the limits of quantification (LOQs) for the five target compounds in water samples were 0.5-1.2 ng/L and 1.4-4.0 ng/L, respectively. The recoveries of spiked water samples were 87.85%-102.34% with good repeatability and reproducibility (RSD < 5%, n = 3) for all the target compounds. Finally, the validated method was applied to analysis the representative UV filters in water samples collected from a wastewater treatment plant in Kunming city of Yunnan province.

  15. Accurate determination of silver nanoparticles in animal tissues by inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Veverková, Lenka [Regional Centre of Advanced Technologies and Materials, Department of Analytical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); Hradilová, Šárka [Regional Centre of Advanced Technologies and Materials, Department of Physical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); Milde, David, E-mail: david.mlde@upol.cz [Regional Centre of Advanced Technologies and Materials, Department of Analytical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); Panáček, Aleš [Regional Centre of Advanced Technologies and Materials, Department of Physical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); Skopalová, Jana [Regional Centre of Advanced Technologies and Materials, Department of Analytical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); Kvítek, Libor [Regional Centre of Advanced Technologies and Materials, Department of Physical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); Petrželová, Kamila [Regional Centre of Advanced Technologies and Materials, Department of Analytical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); National Reference Laboratory for Chemical Elements, Department of Residues in Kroměříž, State Veterinary Institute Olomouc, Hulínská 2286, CZ 767 60 Kroměříž (Czech Republic); and others

    2014-12-01

    This study examined recoveries of silver determination in animal tissues after wet digestion by inductively coupled plasma mass spectrometry. The composition of the mineralization mixture for microwave assisted digestion was optimized and the best recoveries were obtained for mineralization with HNO{sub 3} and addition of HCl promptly after digestion. The optimization was performed on model samples of chicken meat spiked with silver nanoparticles and a solution of ionic silver. Basic calculations of theoretical distribution of Ag among various silver-containing species were implemented and the results showed that most of the silver is in the form of soluble complexes AgCl{sub 2}{sup −} and AgCl{sub 3}{sup 2−} for the optimized composition of the mineralization mixture. Three animal tissue certified reference materials were then analyzed to verify the trueness and precision of the results. - Highlights: • We performed detailed optimization of microwave assisted digestion procedure of animal tissue used prior to Ag determination by ICP-MS. • We provide basic equilibrium calculations to give theoretical explanation of results from optimization of tested mineralization mixtures. • Results from method validation that was done by analysis of several matrix CRMs are presented.

  16. Solid-phase microextraction gas chromatography-mass spectrometry determination of fragrance allergens in baby bathwater.

    Science.gov (United States)

    Lamas, J Pablo; Sanchez-Prado, Lucia; Garcia-Jares, Carmen; Llompart, Maria

    2009-07-01

    A method based on solid-phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) has been optimized for the determination of fragrance allergens in water samples. This is the first study devoted to this family of cosmetic ingredients performed by SPME. The influence of parameters such as fibre coating, extraction and desorption temperatures, salting-out effect and sampling mode on the extraction efficiency has been studied by means of a mixed-level factorial design, which allowed the study of the main effects as well as two-factor interactions. Excluding desorption temperature, the other parameters were, in general, very important for the achievement of high response. The final procedure was based on headspace sampling at 100 degrees C, using polydimethylsiloxane/divinylbenzene fibres. The method showed good linearity and precision for all compounds, with detection limits ranging from 0.001 to 0.3 ng mL(-1). Reliability was demonstrated through the evaluation of the recoveries in different real water samples, including baby bathwater and swimming pool water. The absence of matrix effects allowed the use of external standard calibration to quantify the target compounds in the samples. The proposed procedure was applied to the determination of allergens in several real samples. All the target compounds were found in the samples, and, in some cases, at quite high concentrations. The presence and the levels of these chemicals in baby bathwater should be a matter of concern.

  17. Electrochemical separation and isotopic determination of thallium at the nanogram level by surface ionisation mass spectrometry

    International Nuclear Information System (INIS)

    Arden, J.W.

    1983-01-01

    A rapid low-blank procedure is described for the co-separation of thallium and lead by sequential cathodic and anodic electrodeposition from natural samples, especially complex natural silicates, for subsequent mass spectrometry. A micro anion-exchange procedure is also described for the separation of thallium and lead. Ion currents of 10 - 10 A can be obtained from 1 ng of thallium. The isotopic composition of 1 ng of thallium can be measured on a Faraday detector with a precision of 0.05-0.1%. The total procedural blank is 3 pg. By using stable isotope dilution, 0.2 ng of thallium can be measured with a precision of 0.6% with only a 2% blank correction. This allows the accurate determination of thallium in natural samples down to concentration levels of about 50 pg g - 1 . The detection limit is 50 fg. This procedure has been applied to meteorites and terrestrial rocks. The stable isotope dilution technique is suitable for geochemical, environmental and toxicological studies requiring a highly sensitive, accurate and precise method for the determination of thallium. (Auth.)

  18. The determination of magnesium in simulated PWR coolant by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Gatford, C.; Torrance, K.

    1988-06-01

    The determination of magnesium in simulated PWR coolant has been investigated by graphite furnace atomic absorption spectrometry with atomization from a L'vov platform. The presence of boric acid in the coolant suppresses the magnesium absorption to such an extent that removal of the boron is necessary and three variations of a methyl borate volatilization technique for the in situ removal of boron from the sample platform were investigated. This work has shown that dilution of the sample with an equal volume of acidified methanol and volatilization of the methyl borate was adequate for the determination of magnesium in coolant samples containing up to 2000 mg 1 -1 of boron. In simulated coolant samples containing 25 and 4 μg 1 -1 of magnesium, positive biases of about 2 and 0.5 μg 1 -1 were measured and these errors were considered to be due to contamination. The limit of detection in the presence of 100 and 2000 mg 1 -1 boron were 0.14 and 0.93 μg 1 -1 respectively. These performance characteristics suggest the method is completely acceptable for monitoring the chemical purity of PWR coolant and associated waters containing boric acid. If, however, more precise analyses were to be required for research purposes then any significant improvement in the above figures would require increased purity of reagents, clean-room conditions to reduce contamination and a more versatile atomic absorption spectrophotometer. (author)

  19. The determination of molybdenum and tungsten in resin by x-ray-fluorescence spectrometry

    International Nuclear Information System (INIS)

    Eddy, B.T.

    1985-01-01

    This report describes a method using X-ray-fluorescence spectrometry for the determination of molybdenum and tungsten in ion-exchange resins. The dried resin is milled with sand, binder, and an internal-standard mixture before being briquetted. Niobium and zinc are used as the internal standards for molybdenum and tungsten respectively. Intensity measurements are made with the gold anode tube. Corrections are made for the interference of the Mo Kα analytical line on the background intensities used for the Mo Kα and Nb Kα lines. The precision of the analysis for molybdenum ranges from a relative standard deviation 0,02 at 5 mg/g to 0.045 at 55μg/g; for tungsten, the relative standard deviation ranges from 0,04 at 5 mg/g to 0,055 at 55μg/g. The limits of determination in the original resin sample were found to be 40μg/g for molybdenum and 80μg/g for tungsten. The laboratory method is given in an appendix

  20. [Determination of olive oil content in olive blend oil by headspace gas chromatography-mass spectrometry].

    Science.gov (United States)

    Jiang, Wanfeng; Zhang, Ning; Zhang, Fengyan; Yang, Zhao

    2017-07-08

    A method for the determination of the content of olive oil in olive blend oil by headspace gas chromatography-mass spectrometry (SH-GC/MS) was established. The amount of the sample, the heating temperature, the heating time, the amount of injection, the injection mode and the chromatographic column were optimized. The characteristic compounds of olive oil were found by chemometric method. A sample of 1.0 g was placed in a 20 mL headspace flask, and heated at 180℃ for 2700 s. Then, 1.0 mL headspace gas was taken into the instrument. An HP-88 chromatographic column was used for the separation and the analysis was performed by GC/MS. The results showed that the linear range was 0-100%(olive oil content). The linear correlation coefficient ( r 2 ) was more than 0.995, and the limits of detection were 1.26%-2.13%. The deviations of olive oil contents in the olive blend oil were from -0.65% to 1.02%, with the relative deviations from -1.3% to 6.8% and the relative standard deviations from 1.18% to 4.26% ( n =6). The method is simple, rapid, environment friendly, sensitive and accurate. It is suitable for the determination of the content of olive oil in olive blend oil.

  1. Determination of metals content from wines by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Iordache, Andreea-Maria; Geana, Elisabeta-Irina

    2009-01-01

    Full text: Wine is a widely consumed beverage with thousands of years of tradition. Wine composition strongly determines its quality besides having a great relevance on wine characterization, tipyfication and frauds detection. Wine composition is influenced by many and diverse factors corresponding to the specific production area, such as grape variety, soil and climate, culture, yeast, winemaking practices, transport and storage. Daily consumption of wine in moderate quantities contributes significantly to the requirements of the human organism for essential elements such as Cr, Cu, Zn, Fe, Mn, Co, Ni and Sr. On the other hand, several metals, such as Pb and Cd , are known to be potentially toxic. The objective of this work was to develop a method to determine the metals content in wine samples from Romania. Three samples of difference white wines available in the supermarket was analyzed for identify the presence of: Cr, Cu, Zn, Fe, Mn, Pb, Cd, Co, Ni and Sr by inductively coupled plasma mass spectrometry (ICP-MS). (authors)

  2. Determination of sulfur in steels by isotope dilution mass spectrometry after dissolution with sealed tube

    International Nuclear Information System (INIS)

    Watanabe, Kazuo

    1981-01-01

    The scaled tube dissolution technique was studied for the complete conversion of sulfur in steels to sulfate. Isotope dilution mass spectrometry was used for the determination of sulfur in the sulfate. Sample (0.5 g) was dissolved in nitric acid (7 ml) and hydrochloric acid (3 ml) in a scaled borosilicate glass tube on being heated above 180 0 C overnight. Nitrate ions were removed by repeated evaporation with hydrochloric acid. The residue was dissolved in hydrochloric acid. Sulfate was reduced with a mixture of hydrochloric, hydroiodic and hypophosphorous acids; hydrogen sulfide evolved was absorbed in cadmium acetate solution, then converted to silver sulfide, which was burned to sulfur dioxide in pure oxygen at low pressure, for isotopic analysis. Analytical blank in whole procedure was 0.8 μg of sulfur. This technique was applied to the determination of sulfur in NBS low alloy steels. The principal cause of low values obtained by the open beaker dissolution technique was evaporation losses of sulfur as sulfur dioxide during the dissolution. (author)

  3. Coordination chemistry of nickel(II) nitrate with superbasic guanidines studied by electrospray mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Glasovac, Z.; Štrukil, V.; Eckert-Maksič, M.; Schröder, Detlef; Schlangen, M.; Schwarz, H.

    2010-01-01

    Roč. 290, č. 1 (2010), s. 22-31 ISSN 1387-3806 R&D Projects: GA ČR GA203/08/1487 Grant - others: ERC (XE) HORIZOMS AdG226373 Institutional research plan: CEZ:AV0Z40550506 Keywords : electrospray ionization * guanidine * ion association * nickel(II) nitrate * solvation Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.009, year: 2010

  4. Trends in preconcentration procedures for metal determination using atomic spectrometry techniques

    International Nuclear Information System (INIS)

    Godoi Pereira, M. de; Arruda, M.A.Z.

    2003-01-01

    Methods for metal preconcentration are often described in the literature. However, purposes are often different, depending on whether the methods are applied in environmental, clinical or technological fields. The respective method needs to be efficient, give high sensitivity, and ideally also is selective which is useful when used in combination with atomic spectroscopy. This review presents the actual tendencies in metal preconcentration using techniques such as flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS), hydride generation atomic absorption spectrometry (HGAAS), inductively coupled plasma optical emission spectrometry (ICP OES) and inductively coupled plasma mass spectrometry (ICP-MS). Procedures based on related to electrochemical, coprecipitation/precipitation, liquid-liquid and solid-liquid extraction and atom trapping mechanisms are presented. (author)

  5. Fast mass spectrometry-based enantiomeric excess determination of proteinogenic amino acids.

    Science.gov (United States)

    Fleischer, Heidi; Thurow, Kerstin

    2013-03-01

    A rapid determination of the enantiomeric excess of proteinogenic amino acids is of great importance in various fields of chemical and biologic research and industries. Owing to their different biologic effects, enantiomers are interesting research subjects in drug development for the design of new and more efficient pharmaceuticals. Usually, the enantiomeric composition of amino acids is determined by conventional analytical methods such as liquid or gas chromatography or capillary electrophoresis. These analytical techniques do not fulfill the requirements of high-throughput screening due to their relative long analysis times. The method presented allows a fast analysis of chiral amino acids without previous time consuming chromatographic separation. The analytical measurements base on parallel kinetic resolution with pseudoenantiomeric mass tagged auxiliaries and were carried out by mass spectrometry with electrospray ionization. All 19 chiral proteinogenic amino acids were tested and Pro, Ser, Trp, His, and Glu were selected as model substrates for verification measurements. The enantiomeric excesses of amino acids with non-polar and aliphatic side chains as well as Trp and Phe (aromatic side chains) were determined with maximum deviations of the expected value less than or equal to 10ee%. Ser, Cys, His, Glu, and Asp were determined with deviations lower or equal to 14ee% and the enantiomeric excess of Tyr were calculated with 17ee% deviation. The total screening process is fully automated from the sample pretreatment to the data processing. The method presented enables fast measurement times about 1.38 min per sample and is applicable in the scope of high-throughput screenings.

  6. Determination of 36Cl/Cl ratio in ground water using the accelerator mass spectrometry technique

    International Nuclear Information System (INIS)

    Sharma, Suman; Deodhar, A.S.; Saravana Kumar, U.; Surendran, P.; Shrivastava, A.; Gupta, A.K.; Nair, J.P.; Yadav, M.L.; Hemalatha, M.; Sparrow, H.; Mahata, K.; Thomas, R.G.; Bhagwat, P.V.; Kailas, S.; Kale, R.M.

    2009-01-01

    The Accelerator Mass Spectrometry (AMS) programme using the 14 MV Pelletron Accelerator at Mumbai has been initiated with major emphasis on the determination of 36 Cl in water samples, of interest to hydrology and environment. In order to carry out the AMS measurement, a beam chopper to cut down beam intensity by a factor of 20 has been developed and commissioned. A multi-anode gas -si detector has been built to separate 36 Cl from the interfering 36 S. A new TPS system has been procured to operate the machine in the GVM mode. Standard and blank samples from Prime lab, Purdue have been employed in these measurements to standardise the technique for 36 Cl/Cl ratio determination. The detector was calibrated using the stable 35,37 Cl ions. The background 36 Cl in the system has been measured using the blank sample from Purdue and it was estimated that the ratio of 36 Cl/Cl was of the order of 10 -13 in the present setup. Ground water samples collected from South India were converted to AgCl and put in the SNICS ion source for the AMS measurements. These ground water samples, with 14 C content estimated to be in the range of 1 to 4 pMC indicate that the samples may be more than 35,000 years old. Using the AMS technique we have determined the 36 Cl/Cl ratio values for these ground water samples. They are found to range between 2 to 5 x 10 -12 . Additional measurements are planned to determine the age of the water samples and to understand the reasons for the observed high values of 36 Cl in these samples. (author)

  7. Determination of 129I using distillation method and liquid scintillation spectrometry

    International Nuclear Information System (INIS)

    Horvathova, B.; Dulanska, S.; Remenec, B.; Matel, L.; Gardonova, V.

    2014-01-01

    The conditions for effective distillation of iodine as a screening method for the determination of 129 I by liquid scintillation spectrometry were optimized. By distillation of iodine it is possible to achieve high-purity fraction without interferences needed for measuring 129 I for liquid scintillation spectrometer. Yields of separation were determined gravimetrically using PdI 2 ·H 2 O. The environment that was found to be effective for distillation of iodine is made up of 1 - 2 mol dm -3 HNO 3 together with 0.4 g of NaNO 2 as an oxidizing agent (I . →I 2 ). For testing of distillation, suitable apparatus for distillation of iodine was designed. The apparatus was connected to a vacuum box, which sucks iodine of the distilled solution. Then the iodine was captured in a solution of NaOH at a concentration of 1.5 mol dm -3 . As part of the optimization methodology, it was found that the concentration of NaOH solution for adsorption I 2 (g) does not have any influence on the yields, as opposed to its volume, where it is necessary to use a maximum amount of NaOH in the holding flask for maximum adsorption of iodine. It was determined, that time needed for coagulation PdI 2 ·H 2 O is 24 hours and suitable time for distillation was 20 minutes. Optimized method for the determination of 129 I was applied for various matrices from NPPs in Slovak Republic. Values of 129 I for all analyzed samples were less than the minimum detectable activity (0.043 Bq). The separation yields were in the range (73.14 to 82.04)% and 129 I was measured on a liquid scintillation spectrometer TRI CARB 2900TR with high detection efficiency of 95%. (authors)

  8. Determination of ifosfamide, 2-and 3-dechloroethyifosfamide using gas chromatography with nitrogen-phosphorus or mass spectrometry detection

    NARCIS (Netherlands)

    Kerbusch, T; Jeuken, MJ; Derraz, J; van Putten, JWG; Huitema, ADR; Beijnen, JH

    2000-01-01

    A comparison was made between methods for determining ifosfamide (IF), 2- (2DCE) and 3-dechloroethylifosfamide (3DCE) using gas chromatography with nitrogen-phosphorus detection (GC-NPD) versus positive ion electron-impact ion-trap mass spectrometry (GC-MS'). Sample pretreatment involved

  9. Determination of uranium in urine - Measurement of isotope ratios and quantification by use of inductively coupled plasma mass spectrometry

    NARCIS (Netherlands)

    Krystek, Petra; Ritsema, R.

    2002-01-01

    For analysis of uranium in urine determination of the isotope ratio and quantification were investigated by high-resolution inductively coupled plasma mass spectrometry (HR ICP-MS). The instrument used (ThermoFinniganMAT ELEMENT2) is a single-collector MS and, therefore, a stable sample-introduction

  10. Determination of ten carbamate pesticides in aquatic and sediment samples by liquid chromatography-ionspray and thermospray mass spectrometry.

    NARCIS (Netherlands)

    Honing, M.; Riu, J.; Barceló, D.; van Baar, B.L.M.; Brinkman, U.A.T.

    1996-01-01

    Ten carbamate pesticides which exhibit large differences in polarity were determined simultaneously in various environmental samples, using both column liquid chromatography (LC)-thermospray (TSP) mass spectrometry (MS) and LC-ionspray (ISP) MS. For sample clean-up, column chromatography with three

  11. Simultaneous determination of estrogens and progestogens in honey using high performance liquid chromatography-tandem mass spectrometry

    Science.gov (United States)

    This work describes the development and validation of a method for the simultaneous determination of 13 estrogens and progestogens in honey by high performance liquid chromatography-tandem mass spectrometry. The target compounds were preconcentrated by solid phase extraction. Pretreatment variables ...

  12. Studies on the determination of surface deuterium in AISI 1062, 4037, and 4140 steels by secondary ion mass spectrometry

    Science.gov (United States)

    Sastri, V. S.; Donepudi, V. S.; McIntyre, N. S.; Johnston, D.; Revie, R. W.

    1988-12-01

    The concentration of deuterium at the surface of cathodically charged high strength steels AISI 1062, 4037, and 4140 has been determined by secondary ion mass spectrometry (SIMS). The beneficial effects of pickling in NAP (a mixture of nitric, acetic, and phosphoric acids) to remove surfacebound deuterium have been observed.

  13. [Determination of 24 minerals in human milk by inductively coupled plasma mass spectrometry with microwave digestion].

    Science.gov (United States)

    Sun, Zhongqing; Yue, Bing; Yang, Zhenyu; Li, Xiaowei; Wu, Yongning; Yin, Shian

    2013-05-01

    To determine the levels of 24 minerals in human milk by inductively coupled plasma mass spectrometry with microwave digestion. The samples were digested by microwave. The contents of minerals were determined by inductively coupled plasma mass spectrometry. The standard reference minerals of 1849a and 1568a from National Institute of Science and Technology were used for quality control. The accuracy and reproduability for this method were evaluated with mix standards and 1849a and 1568a standard reference materials. The ranges of the levels of sodium, magnesium, phosphorus, potassium, calcium, aluminum, chromium, arsenic, selenium, iron, zinc, manganese, copper, molybdenum, vanadium, cobalt, nickel, gallium, cadmium, silver, strontium, cesium, barium, lead in human milk was 34.97-415.83 mg/kg, 19.00-39.52 mg/kg, 102.13-274.53 mg/kg, 351.19-713.99 mg/kg, 180.08-349.64 mg/kg, 0.06-0.44 mg/kg, 0.9-7.37 microg/kg, 0.92-2.72 microg/kg, 0.20-21.15 microg/kg, 0.10-0.70 mg/kg, 0.56-3.25 mg/kg, 3.00-16.12 micro.g/kg, 62.16-591.69 microg/kg, 0.02-6.91 microg/kg, 5.99-13.70 microg/kg, 0.07-2.11 microg/kg, 0.77-209.26 microg/kg, 0.005-0.28 microg/kg, 0.02-0.23 microg/kg, 0.02-0.71 microg/kg, 36.89-132.26 microg/kg, 0.01-4.72 microg/kg, 0.83-28.16 microg/kg, 2.5-5.3 microg/kg, respectively. The levels of minerals in human milk in present study were consisted with other similar studies. The experiment examined the levels of minerals in human milk satisfactorily. The method has high accuracy and good reproducibility, which could be used for understanding the levels of minerals in human milk.

  14. Determination of 4-Chloroindole-3-Acetic Acid Methyl Ester in Lathyrus Vicia and Pisum by Gas Chromatography - Mass Spectrometry

    DEFF Research Database (Denmark)

    Engvild, Kjeld Christensen; Egsgaard, Helge; Larsen, Elfinn

    1980-01-01

    4-Chloroindole-3-acetic acid methyl ester was identified unequivocally in Lathyrus latifolius L., Vicia faba L. and Pisum sativum L. by thin layer chromatography, gas chromatography and mass spectrometry. The gas chromatographic system was able to separate underivatized chloroindole-3-acetic acid...... methyl ester isomers. The quantitative determination of 4-chloroindole-3-acetic acid methyl ester in immature seeds of these three species was performed by gas chromatography – mass spectrometry using deuterium labelled 4-chloro-indole-3-acetic acid methyl ester as an internal standard. P. sativum...

  15. Comparison of the radiochemical separation procedures od plutonium applied for its determination in the environmental samples using alpha spectrometry

    International Nuclear Information System (INIS)

    Komosa, A.; Michalik, S.

    2006-01-01

    Alpha spectrometry of the plutonium isotopes can be performed only after the perfect plutonium separation from other components of the matrix. So, till now numerous procedures have been elaborated and tested. The communication presents comparison of the plutonium content determination in soil, bones, eggshells and in the reference materials obtained by alpha spectrometry combined with two different separation procedures. The samples were mineralized in the concentrated HCl or HF prior to plutonium electrodeposition or coprecipitation with NdF 3 . Some other details were also tested in various variants. Quality of the spectra is discussed in terms of all these pre-treatment methods

  16. Plasma-related matrix effects in inductively coupled plasma--atomic emission spectrometry by group I and group II matrix-elements

    International Nuclear Information System (INIS)

    Chan, George C.-Y.; Chan, W.-T.

    2003-01-01

    The effects of Na, K, Ca and Ba matrices on the plasma excitation conditions in inductively coupled plasma-atomic emission spectrometry (ICP-AES) were studied. Normalized relative intensity was used to indicate the extent of the plasma-related matrix effects. The group I matrices have no effects on the plasma excitation conditions. In contrast, the group II matrices depress the normalized relative intensities of some spectral lines. Specifically, the Group II matrices have no effects on the normalized relative intensity of atomic lines of low upper energy level (soft lines), but reduce the normalized relative intensity of some ionic lines and atomic lines of high energy level (hard lines). The Group II matrices seem to shift the Saha balance of the analytes only; no shift in the Boltzmann balance was observed experimentally. Moreover, for some ionic lines with sum of ionization and excitation potentials close to the ionization potential of argon (15.75 eV), the matrix effect is smaller than other ionic lines of the same element. The reduced matrix effects may be attributed qualitatively to charge transfer excitation mechanism of these ionic lines. Charge transfer reaction renders ionic emission lines from the quasi-resonant levels similar in characteristics of atomic lines. The contribution of charge transfer relative to excitation by other non-specific excitation mechanisms (via Saha balance and Boltzmann balance) determines the degree of atomic behavior of a quasi-resonant level. A significant conclusion of this study is that plasma-related matrix effect depends strongly on the excitation mechanism of a spectral line. Since, in general, more than one excitation mechanism may contribute to the overall excitation of an emission line, the observed matrix effects reflect the sum of the effects due to individual excitation mechanisms. Excitation mechanisms, in addition to the often-used total excitation energy, should be considered in matrix effect studies

  17. A new generation of x-ray spectrometry UHV instruments at the SR facilities BESSY II, ELETTRA and SOLEIL

    Energy Technology Data Exchange (ETDEWEB)

    Lubeck, J., E-mail: janin.lubeck@ptb.de; Fliegauf, R.; Holfelder, I.; Hönicke, P.; Müller, M.; Pollakowski, B.; Ulm, G.; Weser, J.; Beckhoff, B. [Physikalisch-Technische Bundesanstalt (PTB), Abbestr. 2-12, 10587 Berlin (Germany); Bogovac, M.; Kaiser, R. B.; Karydas, A. G.; Leani, J. J.; Migliori, A.; Sghaier, H. [Nuclear Science and Instrumentation Laboratory, IAEA Laboratories, A-2444, Seibersdorf (Austria); Boyer, B.; Lépy, M. C.; Ménesguen, Y. [CEA, LIST, Laboratoire National Henri Becquerel, Bât. 602 PC 111, CEA-Saclay 91191 Gif-sur-Yvette c. (France); Detlefs, B. [CEA-LETI, Minatec Campus, 17 rue des Martyrs, 38054 Grenoble (France); Eichert, D. [Elettra - Sincrotrone Trieste (EST) S.C.p.A., 34149 Basovizza, Trieste (Italy); and others

    2016-07-27

    A novel type of ultra-high vacuum instrument for X-ray reflectometry and spectrometry-related techniques for nanoanalytics by means of synchrotron radiation (SR) has been constructed and commissioned at BESSY II. This versa-tile instrument was developed by the PTB, Germany’s national metrology institute, and includes a 9-axis manipulator that allows for an independent alignment of the samples with respect to all degrees of freedom. In addition, it integrates a rotational and translational movement of several photodiodes as well as a translational movement of a beam-geometry-defining aperture system. Thus, the new instrument enables various analytical techniques based on energy dispersive X-ray detectors such as reference-free X-Ray Fluorescence (XRF) analysis, total-reflection XRF, grazing-incidence XRF, in addition to optional X-Ray Reflectometry (XRR) measurements or polarization-dependent X-ray absorption fine structure analyses (XAFS). Samples having a size of up to (100 × 100) mm{sup 2}; can be analyzed with respect to their mass deposition, elemental, spatial or species composition. Surface contamination, nanolayer composition and thickness, depth pro-file of matrix elements or implants, nanoparticles or buried interfaces as well as molecular orientation of bonds can be accessed. Three technology transfer projects of adapted instruments have enhanced X-Ray Spectrometry (XRS) research activities within Europe at the synchrotron radiation facilities ELETTRA (IAEA) and SOLEIL (CEA/LNE-LNHB) as well as at the X-ray innovation laboratory BLiX (TU Berlin) where different laboratory sources are used. Here, smaller chamber requirements led PTB in cooperation with TU Berlin to develop a modified instrument equipped with a 7-axis manipulator: reduced freedom in the choice of experimental geometry modifications (absence of out-of-SR-plane and reference-free XRS options) has been compensated by encoder-enhanced angular accuracy for GIXRF and XRR.

  18. Triple sorbent thermal desorption/gas chromatography/mass spectrometry determination of vapor phase organic contaminants

    International Nuclear Information System (INIS)

    Ma, C.Y.; Skeen, J.T.; Dindal, A.B.; Higgins, C.E.; Jenkins, R.A.

    1994-05-01

    A thermal desorption/ps chromatography/mass spectrometry (TD/GC/MS) has been evaluated for the determination of volatile organic compounds (VOCS) in vapor phase samples using Carbosieve S-III/Carbotrap/Carotrap C triple sorbent traps (TST) similar to those available from a commercial source. The analysis was carried out with a Hewlett-Packard 5985A or 5995 GC/MS system with a modified injector to adapt an inhouse manufactured short-path desorber for transferring desorbate directly onto a cryofocusing loop for subsequent GC/MS analysis. Vapor phase standards generated from twenty six compounds were used for method validation, including alkanes, alkyl alcohols, alkyl ketones, and alkyl nitrites, a group of representative compounds that have previously been identified in a target airborne matrix. The method was validated based on the satisfactory results in terms of reproducibility, recovery rate, stability, and linearity. A relative, standard deviation of 0.55 to 24.3 % was obtained for the entire TD process (generation of gas phase standards, spiking the standards on and desorbing from TST) over a concentration range of 20 to 500 ng/trap. Linear correlation coefficients for the calibration curves as determined ranged from 0.81 to 0.99 and limits of detection ranged from 3 to 76 ng. For a majority of standards, recoveries of greater than 90% were observed. For three selected standards spiked on TSTS, minimal loss (10 to 22%) was observed after storing the spiked in, a 4 degree C refrigerator for 29 days. The only chromatographable artifact observed was a 5% conversion of isopropanol to acetone. The validated method been successfully applied, to the determination of VOCs collected from various emission sources in a diversified concentration range

  19. Determination of sulfur in food by high resolution continuum source flame molecular absorption spectrometry

    Science.gov (United States)

    Zambrzycka, Elżbieta; Godlewska-Żyłkiewicz, Beata

    2014-11-01

    In the present work, a fast, simple and sensitive analytical method for determination of sulfur in food and beverages by high resolution continuum source flame molecular absorption spectrometry was developed. The determination was performed via molecular absorption of carbon monosulfide, CS. Different CS rotational lines (257.959 nm, 258.033 nm, 258.055 nm), number of pixels and types of standard solution of sulfur, namely: sulfuric acid, sodium sulfate, ammonium sulfate, sodium sulfite, sodium sulfide, DL-cysteine, and L-cystine, were studied in terms of sensitivity, repeatability of results as well as limit of detection and limit of quantification. The best results were obtained for measurements of absorption of the CS molecule at 258.055 nm at the wavelength range covering 3 pixels and DL-cysteine in 0.2 mol L- 1 HNO3 solution as a calibration standard. Under optimized conditions the limit of detection and the limit of quantification achieved for sulfur were 10.9 mg L- 1 and 36.4 mg L- 1, respectively. The repeatability of the results expressed as relative standard deviation was typically beverage samples with added known amount of sulfur standard. The recovery of analyte from such samples was in the range of 93-105% with the repeatability in the range of 4.1-5.0%. The developed method was applied for the determination of sulfur in milk (194 ± 10 mg kg- 1), egg white (2188 ± 29 mg kg- 1), mineral water (31.0 ± 0.9 mg L- 1), white wine (260 ± 4 mg L- 1) and red wine (82 ± 2 mg L- 1), as well as in sample rich in ions, such as bitter mineral water (6900 ± 100 mg L- 1).

  20. Structural features of lipoarabinomannan from Mycobacterium bovis BCG. Determination of molecular mass by laser desorption mass spectrometry.

    Science.gov (United States)

    Venisse, A; Berjeaud, J M; Chaurand, P; Gilleron, M; Puzo, G

    1993-06-15

    It was recently shown that mycobacterial lipoarabinomannan (LAM) can be classified into two types (Chatterjee, D., Lowell, K., Rivoire B., McNeil M. R., and Brennan, P. J. (1992) J. Biol. Chem. 267, 6234-6239) according to the presence or absence of mannosyl residues (Manp) located at the nonreducing end of the oligoarabinosyl side chains. These two types of LAM were found in a pathogenic Mycobacterium tuberculosis strain and in an avirulent M. tuberculosis strain, respectively, suggesting that LAM with Manp characterizes virulent and "disease-inducing strains." We now report the structure of the LAM from Mycobacterium bovis Bacille Calmette-Guérin (BCG) strain Pasteur, largely used throughout the world as vaccine against tuberculosis. Using an up-to-date analytical approach, we found that the LAM of M. bovis BCG belongs to the class of LAMs capped with Manp. By means of two-dimensional homonuclear and heteronuclear scalar coupling NMR analysis and methylation data, the sugar spin system assignments were partially established, revealing that the LAM contained two types of terminal Manp and 2-O-linked Manp. From the following four-step process: (i) partial hydrolysis of deacylated LAM (dLAM), (ii) oligosaccharide derivatization with aminobenzoic ethyl ester, (iii) HPLC purification, (iv) FAB/MS-MS analysis; it was shown that the dimannosyl unit alpha-D-Manp-(1-->2)-alpha-D-Manp is the major residue capping the termini of the arabinan of the LAM. In this report, LAM molecular mass determination was established using matrix-assisted UV-laser desorption/ionization mass spectrometry which reveals that the LAM molecular mass is around 17.4 kDa. The similarity of the LAM structures between M. bovis BCG and M. tuberculosis H37Rv is discussed in regard to their function in the immunopathology of mycobacterial infection.

  1. Quantitative determination of hederagenin in rat plasma and cerebrospinal fluid by ultra fast liquid chromatography-tandem mass spectrometry method.

    Science.gov (United States)

    Yang, Xuemei; Li, Guoliang; Chen, Lingyun; Zhang, Cong; Wan, Xinxiang; Xu, Jiangping

    2011-07-01

    A rapid, sensitive and selective method was developed for the quantitative determination of hederagenin in rat plasma and cerebrospinal fluid (CSF) by ultra fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS). It has been successfully applied in a pharmacokinetic study of hederagenin in the central nervous system (CNS). Sample pretreatment involved a simple protein precipitation with methanol and a one-step extraction with ethyl acetate. Separation was carried out in a Shim-pack XR-ODS II (75 mm × 2.0 mm, i.d., 2.1 μm) column with gradient elution at a flow rate of 0.35 mL/min. The mobile phase was 5mM ammonium acetate and acetonitrile. Detection was performed in a triple-quadruple tandem mass spectrometer by multiple-reaction-monitoring mode via electrospray ionization. A linear calibration curve for hederagenin was obtained over a concentration range of 0.406 (lower limit of quantification, LLOQ) to 203 ng/mL (r² > 0.99) for both plasma and CSF. The intra-day and inter-day precision (relative standard deviation, RSD) values were less than 15%. At all quality control (QC) levels, the accuracy (relative error, RE) was within -9.0% and 11.1% for plasma and CSF, respectively. The pharmacokinetics results indicated that hederagenin could pass through the blood-brain barrier. This UFLC-MS/MS method demonstrates higher sensitivity and sample throughput than previous methods. It was also successfully applied to the pharmacokinetic study of hederagenin following oral administration of Fructus akebiae extract in rats. Copyright © 2011 Elsevier B.V. All rights reserved.

  2. Determination of burnup for IEAR-1 fuel elements by non destructive method of gamma spectrometry

    International Nuclear Information System (INIS)

    Madi Filho, T.; Holland, L.

    1982-01-01

    Burnup determination, by non-destructive gamma spectrometry of spent fuel with high and low activity of IEAR-1 reactor, using Cs-137 as burnup monitor, were done. To measure the Cs-137 distribution in these elements a Ge(Li) detector, with volume equal to 73,7 cm 3 , in two measurement systems with defined geometry and good colimation, was used. The IEA-14 taken from the core about 20 years ago, presents a gamma spectra due to Cs-137. The IEA-80, with cooling time approximately to 5 years, shows a more complex gamma spectrum due to other fission products still found in significant quantities. The IEA-14 measures were done in a measurement system used outside the reactor pool (S.I.), being the global efficiency of this system obtained by using a plane, calibrated and extense Ag-110 m source. Detailed measures of gamma transmission, using Cs-137 as a calibrated and punctiforme source, showed the high homogenity of the fuel plates. (E.G.) [pt

  3. [Determination of arsenic speciation in Scomberomorus niphonius by capillary electrophoresis-inductively coupled plasma mass spectrometry].

    Science.gov (United States)

    Chen, Fa-rong; Zheng, Li; Wang, Zhi-Guang; Sun, Jie; Han, Li-Hui; Wang, Xiao-ru

    2014-06-01

    A method for the detection of arsenocholine (AsC), arsenobetaine (AsB), As(III), dimethylarsinic (DMA), monomethylarsonic (MMA) and As (V) by capillary electrophoresis-inductively coupled plasma mass spectrometry (CE-ICP-MS) was established. The results showed that the six species of arsenic were separated within 20 min under the optimized conditions. Good linearities of 6 arsenic species were observed in the range from 2 to 50 μg x L(-1) with the linear correlation greater than 0.996, the detection limits were 0.10-1.08 μg x L(-1) and the RSDs (n = 5) of the peak areas were smaller than 7%. The method was successfully adopted to the determination of the species in Scomberomorus niphonius. The recoveries were between 93% and 98%, and we found the arsenobetaine (AsB) was the main species in the sample. The method was suitable for the analysis of other biological samples with the advantages of good stability, less sample consumption, short analysis time and convenience.

  4. Determination of levofloxacin in human serum using liquid chromatography tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Samiksha Ghimire

    2018-01-01

    Full Text Available A rapid liquid chromatography tandem-mass spectrometry method was developed for the determination of levofloxacin and its metabolite (desmethyl-levofloxacin in human serum. Sample preparation was done using protein precipitation technique. Our method had a run time of 2.5 min and retention times of 1.6 min for all analytes. The standard curves were linear within the concentration range of 0.10 to 5.00 mg/L for levofloxacin and 0.10 to 4.99 mg/L for desmethyl- levofloxacin; a correlation coefficient (R2 of 0.999 and 0.998 respectively. The lower limit of quantification for both analytes was 0.10 mg/L. Within-day precision ranged from 1.4% and 2.4% for levofloxacin, 1.5% to 5% for desmethyl-levofloxacin and between-day precision ranged from 3.6% to 4.1% for levofloxacin and 0.0% to 3.3% for desmethyl-levofloxacin; whereas, accuracy ranged from 0.1% to 12.7% for levofloxacin and 0.2% to 15.6% for desmethyl-levofloxacin. This method could be a useful asset for routine therapeutic drug monitoring of levofloxacin in multi-drug resistant tuberculosis patients.

  5. Liquid to liquid extraction and liquid chromatography-tandem mass spectrometry determination of hainanmycin in feed.

    Science.gov (United States)

    Wang, Ze Ping; Shen, Jian Zhong; Linhardt, Robert J; Jiang, Hui; Cheng, Lin Li

    2017-03-01

    Hainanmycin is a new veterinary polyether antibiotic and has few sensitive analytical method in present days. In this study, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) relying on multiple reaction monitoring (MRM) detection was developed for analysis of hainanmycin in animal feed. Feed samples were extracted with ethyl acetate and purified by two steps of liquid-liquid extraction (LLE) to get rid of water solvable matrix and lipids one by one. The final simple was analyzed by LC-MS/MS. The LC mobile phase was composed of 0.1% aqueous formic acid and 0.1% formic acidified acetonitrile by gradient elution. Average recoveries ranged from 74.22% to 87.85%, as determined by spiking with 2.0 (LOQ) ∼2500μgkg -1 of hainanmycin. The inter-day and intra-day coefficient of variation was 9.21% to 11.77% and 7.67% to 13.49%, respectively. The limit of detection (LOD) and the limit of quantitation (LOQ) were 0.36μgkg -1 and 2.0μgkg -1 , respectively. Copyright © 2016. Published by Elsevier B.V.

  6. Determination of flomoxef in human plasma by liquid chromatography/electrospray ionization tandem mass spectrometry.

    Science.gov (United States)

    Kravtsova, Oxana Yu; Paramonov, Sergey A; Vasilevich, Natalya I; Kazyulkin, Denis N; Vlasova, Ekaterina; Engsig, Michael

    2013-12-01

    A specific, sensitive, rapid and reproducible method for the determination of flomoxef in human plasma using high-performance liquid chromatography-tandem mass spectrometry was developed and validated. Flomoxef was detected using an electrospay ionization method operated in negative-ion mode. Chromatographic separation was performed in gradient elution mode on a Luna® C18(2) column (3 μM, 20 × 4.0 mm) at a flow rate of 1 mL/min and runtime 3.5 min. The mobile phase consisted of acetonitrile and water containing 0.1% formic acid as additive. Extraction of flomoxef from plasma and precipitation of plasma proteins was performed with acetonitrile with an absolute recovery of 86.4 ± 1.6%. The calibration curve was linear with a correlation coefficient of 0.999 over the concentration range 10-5000 ng/mL and the lower limit of quantification was 10 ng/mL. The intra- and inter-day precisions were flomoxef revealed that it could be successfully analyzed at 4 ºС over 24 h, but it was unstable in solutions at room temperature during short-term storage (4 h) and several freeze-thaw cycles. Copyright © 2013 John Wiley & Sons, Ltd.

  7. Determination of 238U in marine organisms by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Ishii, Toshiaki; Nakahara, Motokazu; Matsuba, Mitsue; Ishikawa, Masafumi

    1991-01-01

    Determination of 238 U in fifty-five species of marine organisms was carried out by inductively coupled plasma mass spectrometry which showed some advantages such as high sensitivity, wide dynamic range and small interferences from matrices for the analysis of high mass elements. The concentrations of 238 U in soft tissues of marine animals ranged from 0.076 to 5000 ng/g wet wt. Especially, the branchial heart of cephalopod molluscs showed the specific accumulation of 238 U. The concentration factor of the branchial heart of Octopus vulgaris, which indicated the highest value, was calculated to be about 10 3 by comparing it with the concentration of 238 U (3.2±0.2 ng/ml) in coastal seawaters of Japan. The concentrations of 238 U in hard tissues of marine invertebrates were similar to those in soft tissues. In contrast, hard tissues like bone, scale, fin, etc. of fishes showed much higher concentrations of 238 U than soft tissues like muscle and liver. The concentrations of 238 U of twenty species of algae ranged from 10 to 3700 ng/g dry wt. (author)

  8. Determination of mercury in rice by cold vapor atomic fluorescence spectrometry after microwave-assisted digestion

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Maria Jose da [Department of Analytical Chemistry, Edificio de Investigacion, University of Valencia, 50 Dr. Moliner Street, E-46100 Burjassot, Valencia (Spain); Departamento de Quimica Fundamental, Universidade Federal de Pernambuco, Cidade Universitaria, 50740-550 Recife, PE (Brazil); Paim, Ana Paula S. [Departamento de Quimica Fundamental, Universidade Federal de Pernambuco, Cidade Universitaria, 50740-550 Recife, PE (Brazil); Pimentel, Maria Fernanda [Departamento de Engenharia Quimica, Universidade Federal de Pernambuco, Recife, PE (Brazil); Cervera, M. Luisa, E-mail: m.luisa.cervera@uv.es [Department of Analytical Chemistry, Edificio de Investigacion, University of Valencia, 50 Dr. Moliner Street, E-46100 Burjassot, Valencia (Spain); Guardia, Miguel de la [Department of Analytical Chemistry, Edificio de Investigacion, University of Valencia, 50 Dr. Moliner Street, E-46100 Burjassot, Valencia (Spain)

    2010-05-14

    A cold vapor atomic fluorescence spectrometry method (CV-AFS) has been developed for the determination of Hg in rice samples at a few ng g{sup -1} concentration level. The method is based on the previous digestion of samples in a microwave oven with HNO{sub 3} and H{sub 2}O{sub 2} followed by dilution with water containing KBr/KBrO{sub 3} and hydroxylamine and reduction with SnCl{sub 2} in HCl using external calibration. The matrix interferences and the effect of nitrogen oxide vapors have been evaluated and the method validated using a certified reference material. The limit of detection of the method was 0.9 ng g{sup -1} with a recovery percentage of 95 {+-} 4% at an added concentration of 5 ng g{sup -1}. The concentration level of Hg found in 24 natural rice samples from different origin ranged between 1.3 and 7.8 ng g{sup -1}.

  9. Determination of molybdenum in human urine by electrothermal atomization atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Pita Calvo, C.; Bermejo Barrera, P.; Bermejo Barrera, A.

    1995-01-01

    Various matrix modifiers were investigated for the determination of molybdenum in human urine samples by electrothermal atomization atomic absorption spectrometry. Methods with nitric acid, barium difluoride, magnesium nitrate, palladium-magnesium nitrate and palladium-hydroxylamine hydrochloride were studied by introducing the urine samples directly into the graphite furnace with 0.3% Triton X-100. The charring and atomization curves, the amount of modifier and the calibration and addition graphs were studied in all instances. The precision, accuracy and chemical interferences of the methods were also investigated. The matrix interferences have been removed with the modifiers barium difluoride, palladium-magnesium nitrate and palladium-hydroxylamine hydrochloride. The limits of detection and quantification were 0.2 and 0.7 μg l -1 , respectively, for these modifiers. The characteristic masses were 14.1, 18.0 and 14.9 pg of Mo for palladium-magnesium nitrate, palladium-hydroxylamine hydrochloride and barium difluoride, respectively. The method with palladium-magnesium nitrate has been applied to the study of the amount of molybdenum in human urine samples. The molybdenum levels found lie between 4.8-205.6 μg l -1

  10. Sulfur isotope in nature. Determination of sulfur isotope ratios in coal and petroleum by mass spectrometry

    International Nuclear Information System (INIS)

    Derda, M.

    1999-01-01

    Elementary sulfur or in chemical compounds is one of the elements widespread in the earth's crust and biosphere. Its participation in earth's crust amounts to 0.26 % by weight. Measurement of isotope composition of natural samples can deliver many information about origin, creation and transformation ranges of rocks and minerals. Sulfur isotope ratio contained in minerals is variable and for this reason investigation of isotope sulfur composition can deliver useful information about the geochemistry of each component. Therefore in the investigated sample it is necessary to determine not only the content of sulfur but also the isotope composition of each component. Differentiation of contents of sulfur-34 in natural sulfur compounds can reach up to 110 per mile. So large divergences can be explained by a kinetic effect or by bacterial reduction of sulphates. In this report a wide review of the results of investigations of isotope sulfur compositions in coal and petroleum are presented as well as the methods for the preparation of samples for mass spectrometry analysis are proposed. (author)

  11. Methods of analysis-Determination of pesticides in sediment using gas chromatography/mass spectrometry

    Science.gov (United States)

    Hladik, Michelle; McWayne, Megan M.

    2012-01-01

    A method for the determination of 119 pesticides in environmental sediment samples is described. The method was developed by the U.S. Geological Survey (USGS) in support of the National Water Quality Assessment (NAWQA) Program. The pesticides included in this method were chosen through prior prioritization. Herbicides, insecticides, and fungicides along with degradates are included in this method and span a variety of chemical classes including, but not limited to, chloroacetanilides, organochlorines, organophosphates, pyrethroids, triazines, and triazoles. Sediment samples are extracted by using an accelerated solvent extraction system (ASE®, and the compounds of interest are separated from co-extracted matrix interferences (including sulfur) by passing the extracts through high performance liquid chromatography (HPLC) with gel-permeation chromatography (GPC) along with the use of either stacked graphitized carbon and alumina solid-phase extraction (SPE) cartridges or packed Florisil®. Chromatographic separation, detection, and quantification of the pesticides from the sediment-sample extracts are done by using gas chromatography with mass spectrometry (GC/MS). Recoveries in test sediment samples fortified at 10 micrograms per kilogram (μg/kg) dry weight ranged from 75 to 102 percent; relative standard deviations ranged from 3 to 13 percent. Method detection limits (MDLs), calculated by using U.S. Environmental Protection Agency procedures (40 CFR 136, Appendix B), ranged from 0.6 to 3.4 μg/kg dry weight.

  12. 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.

  13. Enantiomeric determination of DOPA in dietary supplements containing Mucuna pruriens by liquid chromatography/mass spectrometry.

    Science.gov (United States)

    Hasegawa, Takashi; Takahashi, Kazunaga; Fukiwake, Tomohide; Saijo, Masaaki; Motoki, Yuji

    2013-01-01

    We developed a simple and rapid liquid chromatography/mass spectrometry (LC/MS) method for the enantiomeric determination of DOPA in dietary supplements containing Mucuna pruriens. L- and D-DOPA were ultrasonically extracted with 1% formic acid aqueous solution. The isolated extracts were analyzed by LC/MS using a Crownpak CR (-) column at 30℃. The mass spectrometer was operated in the positive mode of electrospray ionization, and the mobile phase was aqueous formic acid (pH 2.0). L-DOPA-ring-d3 was used as an internal standard. The method was validated for a dietary supplement spiked with L- and D-DOPA at 50 and 500 μg/g, respectively, and the recoveries of the DOPA enantiomers were between 97.5% and 101.3%. Relative standard deviation values of repeatability and intermediate precision were less than 7%. The method was applied to 14 dietary supplements. L-DOPA was detected in these supplements in the range of 0.88-12.8 mg/unit. D-DOPA was not detected.

  14. 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.

  15. Radiochemical determination of zirconium by inductively coupled plasma mass spectrometry (ICPMS)

    International Nuclear Information System (INIS)

    Oliveira, Thiago C.; Oliveira, Arno Heeren de

    2013-01-01

    The zirconium isotope 93 Zr is a long-lived pure β-particle-emitting radionuclide thus occurring as one of the radionuclides found in nuclear reactors. It's produced from 235 U fission and from 92 Zr neutron activation. Due to its long half-life, 93 Zr is one of the interest radionuclides for assessment studies performance of waste storage or disposal. Measurement of 93 Zr is difficult owing to its trace level concentration and its low activity in nuclear wastes and further because its certified standards are not frequently available. The aim of this work was to apply a selective radiochemical separation methodology for 93 Zr determination in nuclear waste and analyze it by Inductively Coupled Plasma Mass Spectrometry (ICPMS). To set up the zirconium radiochemical separation procedure, a zirconium tracer solution was used in order to follow the zirconium behavior during the radiochemical separation. A tracer solution containing the main interferences, Ba, Co, Eu, Fe, Mn, Nb, Ni, Sr, and Y was used in order to verify the decontamination factor during separation process. The limit of detection of 0,039 ppb was obtained for zirconium standard solutions by ICPMS. Then, the protocol will be applied to low level waste (LLW) and intermediate level waste (ILW) from nuclear power plants. (author)

  16. Activity determination in the alumina-dysprosia system by Knudsen effusion mass spectrometry

    International Nuclear Information System (INIS)

    Motalov, V.B.; Butman, M.F.; Kudin, L.S.; Markus, T.

    2011-01-01

    Highlights: → Vaporization of Al-Dy-O mixtures has been investigated by KEMS. → The problem of attainment of thermodynamic equilibrium has been described. → The activities of Al 2 O 3 and Dy 2 O 3 have been measured at T = 2130 K. → The Gibbs energies and enthalpies of compound formation have been determined. - Abstract: The vaporization of Al-Dy-O mixtures has been investigated by the Knudsen effusion mass spectrometry technique. The saturated vapor has been found to consist of the atoms Al, O and the molecules AlO, Al 2 O, DyO. At the initial stage the vaporization of Dy 2 O 3 and Al 2 O 3 -Dy 2 O 3 mixtures was found to be incongruent and accompanied by some loss of oxygen. An attainment of congruently vaporizing composition and equilibrium state takes quite a long time. The activities of binary oxides have been measured at T = 2130 K. The Gibbs energies and enthalpies have been derived for formation of the compounds Dy 4 Al 2 O 9 , DyAlO 3 and Dy 3 Al 5 O 12 from sesquioxides.

  17. Determination of mercury by multisyringe flow injection system with cold-vapor atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Leal, L.O.; Elsholz, O.; Forteza, R.; Cerda, V.

    2006-01-01

    A new software-controlled time-based multisyringe flow injection system for mercury determination by cold-vapor atomic absorption spectrometry is proposed. Precise known volumes of sample, reducing agent (1.1% SnCl 2 in 3% HCl) and carrier (3% HCl) are dispensed into a gas-liquid separation cell with a multisyringe burette coupled with one three-way solenoid valve. An argon flow delivers the reduced mercury to the spectrometer. The optimization of the system was carried out testing reaction coils and gas-liquid separators of different design as well as changing parameters, such as sample and reagents volumes, reagent concentrations and carrier gas flow rate, among others. The analytical curves were obtained within the range 50-5000 ng L -1 . The detection limit (3σ b /S) achieved is 5 ng L -1 . The relative standard deviation (R.S.D.) was 1.4%, evaluated from 16 successive injections of 250 ng L -1 Hg standard solution. The injection and sample throughput per hour were 44 and 11, respectively. This technique was validated by means of solid and water reference materials with good agreement with the certified values and was successfully applied to fish samples

  18. Levels of Essential Elements in Different Medicinal Plants Determined by Using Inductively Coupled Plasma Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Eid I. Brima

    2018-01-01

    Full Text Available The objective of this study was to investigate the content of essential elements in medicinal plants in the Kingdom of Saudi Arabia (KSA. Five different medical plants (mahareeb (Cymbopogon schoenanthus, sheeh (Artemisia vulgaris, harjal (Cynanchum argel delile, nabipoot (Equisetum arvense, and cafmariam (Vitex agnus-castus were collected from Madina city in the KSA. Five elements Fe, Mn, Zn, Cu, and Se were determined by using inductively coupled plasma mass spectrometry (ICP-MS. Fe levels were the highest and Se levels were the lowest in all plants. The range levels of all elements in all plants were as follows: Fe 193.4–1757.9, Mn 23.6–143.7, Zn 15.4–32.7, Se 0.13–0.92, and Cu 11.3–21.8 µg/g. Intakes of essential elements from the medical plants in infusion were calculated: Fe 4.6–13.4, Mn 6.7–123.2, Zn 7.0–42.7, Se 0.14–1.5, and Cu 1.5–5.0 µg/dose. The calculated intakes of essential elements for all plants did not exceed the daily intake set by the World Health Organization (WHO and European Food Safety Authority (EFSA. These medicinal plants may be useful sources of essential elements, which are vital for health.

  19. Determination of melatonin and its isomer in foods by liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Kocadağlı, Tolgahan; Yılmaz, Cemile; Gökmen, Vural

    2014-06-15

    This study aimed to develop a reliable analytical method for the determination of melatonin and its isomers in various food products. The method entails ethanol extraction of solid samples (or dilution of liquid samples) prior to liquid chromatography coupled to triple quadruple mass spectrometry (LC-MS/MS) analysis of target analytes. The method was in-house validated and successfully applied to various food matrices. Recovery of melatonin from different matrices were found to be 86.0 ± 3.6%, 76.9 ± 5.4%, 98.6 ± 6.4%, and 67.0 ± 4.5% for beer, walnut, tomato and sour cherry samples, respectively. No melatonin could be detected in black and green tea, sour cherry, sour cherry concentrate, kefir (a fermented milk drink) and red wine while the highest amount of melatonin (341.7 ± 29.3 pg/g) was detected in crumb. The highest amounts of melatonin isomer were detected in yeast-fermented foods such as 170.7 ± 29.9 ng/ml in red wine, 14.3 ± 0.48 ng/ml in beer, and 15.7 ± 1.4 ng/g in bread crumb. Copyright © 2013 Elsevier Ltd. All rights reserved.

  20. Determination and pharmacokinetic studies of arecoline in dog plasma by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Li, Bing; Zhou, Xu-Zheng; Li, Jian-Yong; Yang, Ya-Jun; Niu, Jian-Rong; Wei, Xiao-Juan; Liu, Xi-Wang; Li, Jin-Shan; Zhang, Ji-Yu

    2014-10-15

    A rapid and sensitive high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the determination of arecoline concentration in dog plasma. Plasma sample was prepared by protein precipitation using n-hexane (containing 1% isoamyl alcohol) with β-pinene as an internal standard. Chromatographic separation was achieved on an Agilent C18 column (4.6×75mm, 3.5μm) using methanol: 5mM ammonium acetate as the mobile phase with isocratic elution. Mass detection was carried out using positive electrospray ionization in multiple reaction monitoring mode. The calibration curve for arecoline was linear over a concentration range of 2-500ng/mL. The intra-day and inter-day accuracy and precision were within the acceptable limits of ±10% at all concentrations. In summary, the LC-MS/MS method described herein was fully validated and successfully applied to the pharmacokinetic study of arecoline hydrobromide tablets in dogs after oral administration. Copyright © 2014. Published by Elsevier B.V.

  1. [Determination of gossypol in edible vegetable oil with high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Zhang, Wenhua; Huang, Chaoqun; Xie, Wen; Shen, Li

    2014-06-01

    A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the determination of gossypol in edible vegetable oil. The sample was extracted with ethyl alcohol by vortex-excited oscillation. The extract was cleaned up by 0.22 microm filter membrane and centrifuged for 5 min at 4 000 r/min after standing in a fridge at 4 degrees C for 30 min. The compound was separated on a C18 column (100 mm x 2.1 mm, 3.5 microm) with acetonitrile and 1% (v/v) formic acid aqueous solution as mobile phase. The detection of gossypol was carried out by LC-MS/MS with positive electrospray ionization under multiple reaction monitoring (MRM) mode using external standard method. The limits of quantification (S/N > 10) of gossypol in edible vegetable oil was 1 mg/kg. The recoveries were from 87.4% to 100% at the spiked levels of 1, 2, 200 mg/kg of gossypol in edible vegetable oil with the relative standard deviations (RSDs) between 3.9% and 12.2%. The method, with high sensitivity, good precision and high recovery, was suitable for the confirmation and quantification of gossypol residue in edible vegetable oil.

  2. Quantitative determination of Sulfur and Chlorine in Crude Oils by x-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Ayala Jimenez, R.E.

    1986-01-01

    Given the importance of sulfur and chlorine content in crude petroleum, and that the actual methods used in the country to its determination are slow and cumbersome, the present work consisted in applying a new method, based on X-ray fluorescence spectrometry, to make this analysis as fast as possible with greater sensibility and precision. Samples of crude petroleum were analyzed using two different quantitative methods: a) through calibration curves elaborated with standard aqueous solutions of inorganic salts of S and Cl and b) through standard addition method using CS 2 as standard for S and CCl 4 for Cl. The measuring system consisted of Fe-55 radioactive source (10 mCi), Si-Li semiconductor detector, spectrum amplifier, multichannel analyzer and a DIGITAL Computer. The peak areas and their deviations were obtained through AXIL software. The values of area and deviation joined to weight of sample and amount of standard added were used to calculate the concentration of the analite and its deviation. In conclusion, calibration curves enable only semiquantitative analysis. However, the standard addition method has advantages over ASTM methods D 129-64 and D 808-63 for sulfur and chlorine respectively. The main advantage is the great speed with which an analysis is made: 20 minutes, while ASTM methods need approximately 16 hours. Likewise it was obtained: sensibility 0.05%; accuracy: maximum 0.02%, minimum 10%; and precision: maximum 2%, minimum 10%. (author)

  3. [Determination of amitrole in agricultural products by high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Li, Li; Fu, Jian; Gao, Hongliang; Ren, Haitao; Lou, Xishan; Guan, Lihui

    2010-03-01

    A high performance liquid chromatography-tandem mass spectrometry method (HPLC-MS/MS) was developed for the analysis of amitrole residues in agricultural products. The samples were extracted by 25% acetone for wheat, fish, pork and liver samples, 1% acetic acid-25% acetone for maize and peanut samples, 1% acetic acid solution for honeysuckle, the powder of ginger, the powder of bunge prickly ash and tea leaves samples, 1% acetic acid solution-dichloromethane for apple, pineapple, spinach, carrot, perilla leaves samples, respectively, followed by liquid-liquid extraction with dichloromethane. The samples were then cleaned up by PCX or Envi-Carb solid-phase extraction cartridge. The amitrole was determined and confirmed by HPLC-MS/MS. The results showed a linear relationship in the range of 0.005 -0.1 mg/kg for amitrole. The correlation coefficient was 0.999 7. The average recoveries of amitrole in wheat, maize, peanut, pineapple, apple, carrot, spinach, pork, the powder of ginger, the powder of bunge prickly ash, perilla, liver, fish, honeysuckle and tea were 67.5% - 98.1%. The relative standard deviations (RSDs) were 1.0% - 9.8%. The limits of quantitation were 10 microg/kg for wheat, maize, peanut, pineapple, apple, carrot, spinach, pork, perilla, liver, fish, honeysuckle and 20 microg/kg for the powder of bunge prickly ash, the powder of ginger and tea, respectively. The method is simple, sensitive and accurate.

  4. Determination of stable cesium and strontium in rice samples by inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Srinuttrakul, W.; Yoshida, S.

    2017-06-01

    For long-term radiation dose assessment models, food ingestion is one of the major exposure pathways to human. In general, the stable isotopes can serve as analogues of radioisotopes. In this study, rice samples were collected from 30 paddy fields in Si Sa Ket, Yasothon and Roi Et in the northeast of Thailand in November 2014. The concentrations of stable cesium (Cs-133) and strontium (Sr-88) in polished rice were determined by inductively coupled plasma mass spectrometry (ICP-MS). The standard reference material of rice flour (NIST 1568a) with spiked Cs and Sr was used to validate the analytical method. The concentration of Cs in polished rice from Si Sa Ket, Yasothon and Roi Et was 0.158 ± 0.167 mg kg-1, 0.090 ± 0.117 mg kg-1 and 0.054 ± 0.031 mg kg-1, respectively. The concentration of Sr in polished rice from Si Sa Ket, Yasothon and Roi Et was 0.351 ± 0.108 mg kg-1, 0.364 ± 0.215 mg kg-1 and 0.287 ± 0.102 mg kg-1, respectively. Comparison of the results with Japanese data before the Fukushima Di-ichi nuclear power plant accident showed that the concentrations of both Cs and Sr for Thai rice were higher than those for Japanese rice.

  5. Determination of stable cesium and strontium in rice samples by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Srinuttrakul, W; Yoshida, S

    2017-01-01

    For long-term radiation dose assessment models, food ingestion is one of the major exposure pathways to human. In general, the stable isotopes can serve as analogues of radioisotopes. In this study, rice samples were collected from 30 paddy fields in Si Sa Ket, Yasothon and Roi Et in the northeast of Thailand in November 2014. The concentrations of stable cesium (Cs-133) and strontium (Sr-88) in polished rice were determined by inductively coupled plasma mass spectrometry (ICP-MS). The standard reference material of rice flour (NIST 1568a) with spiked Cs and Sr was used to validate the analytical method. The concentration of Cs in polished rice from Si Sa Ket, Yasothon and Roi Et was 0.158 ± 0.167 mg kg -1 , 0.090 ± 0.117 mg kg -1 and 0.054 ± 0.031 mg kg -1 , respectively. The concentration of Sr in polished rice from Si Sa Ket, Yasothon and Roi Et was 0.351 ± 0.108 mg kg -1 , 0.364 ± 0.215 mg kg -1 and 0.287 ± 0.102 mg kg -1 , respectively. Comparison of the results with Japanese data before the Fukushima Di-ichi nuclear power plant accident showed that the concentrations of both Cs and Sr for Thai rice were higher than those for Japanese rice. (paper)

  6. Determination of pyrrolizidine alkaloids in comfrey by liquid chromatography-electrospray ionization mass spectrometry.

    Science.gov (United States)

    Liu, Feng; Wan, Sow Yin; Jiang, Zhangjian; Li, Sam Fong Yau; Ong, Eng Shi; Osorio, Jhon Carlos Castaño

    2009-12-15

    Symphytum officinale L. (comfrey) is a medicinal plant commonly used in decoctions and aliments. Besides therapeutic bioactive compounds present in the herb, it is found to contain hepatotoxic pyrrolizidine alkaloids (PAs), such as lycopsamine and others. In the present study, PAs such as lycopsamine, echimidine and lasiocarpine were determined using electrospray liquid chromatography-mass spectrometry (LC-MS) with the method precision (relative standard deviation, RSD) comfrey followed by the comparison with heating under reflux with the RSD ranging from 2.49% to 19.32%. Our results showed a higher extraction efficiency for heating under reflux compared with PHWE. It was proposed that the lower extraction efficiency for PHWE was attributable to dissolved nitrogen from air which caused the reduction in the solubility of lycopsamine in the compressed hot solvent. In this study, quantitative analysis of PAs in comfrey was demonstrated. In addition, it was found that the use of subcritical water for extractions depended on the physical properties of the dissolved solutes and their tendency to degrade under the chosen extraction conditions.

  7. Determination of zinc stable isotopes in biological materials using isotope dilution inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Patterson, K.Y.; Veillon, Claude

    1992-01-01

    A method is described for using isotope dilution to determine both the amount of natural zinc and enriched isotopes of zinc in biological samples. Isotope dilution inductively coupled plasma mass spectrometry offers a way to quantify not only the natural zinc found in a sample but also the enriched isotope tracers of zinc. Accurate values for the enriched isotopes and natural zinc are obtained by adjusting the mass count rate data for measurable instrumental biases. Analytical interferences from the matrix are avoided by extracting the zinc from the sample matrix using diethylammonium diethyldithiocarbamate. The extraction technique separates the zinc from elements which form interfering molecular ions at the same nominal masses as the zinc isotopes. Accuracy of the method is verified using standard reference materials. The detection limit is 0.06 μg Zn per sample. Precision of the abundance ratios range from 0.3-0.8%. R.S.D. for natural zinc concentrations is about 200-600 μg g -1 . The accuracy and precision of the measurements make it possible to follow enriched isotopic tracers of zinc in biological samples in metabolic tracer studies. (author). 19 refs.; 1 fig., 4 tabs

  8. A pre-concentration procedure using coprecipitation for determination of lead and iron in several samples using flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Saracoglu, S.; Soylak, M.; Peker, D.S. Kacar; Elci, L.; Santos, W.N.L. dos; Lemos, V.A.; Ferreira, S.L.C.

    2006-01-01

    The present paper proposes a pre-concentration procedure for determination of lead and iron in several samples by flame atomic absorption spectrometry. In it, lead(II) and iron(III) ions are coprecipitated using the violuric acid-copper(II) system as collector. Afterwards, the precipitate is dissolved with 1 M HNO 3 solution and the metal ions are determined. The optimization step was performed using factorial design involving the variables: pH, violuric acid mass (VA) and copper concentration (Cu). Using the optimized experimental conditions, the proposed procedure allows the determination these metals with detection limits of 0.18 μg L -1 for iron and 0.16 μg L -1 for lead. The effects of foreign ions on the pre-concentration procedure were also evaluated and the results demonstrated that this method could be applied for determination of iron and lead in several real samples. The proposed method was successfully applied to the analysis of seawater, urine, mineral water, soil and physiological solution samples. The concentrations of lead and iron achieved in these samples agree well with others data reported in the literature

  9. Validation of a confirmatory method for the determination of melamine in egg by gas chromatography-mass spectrometry and ultra-performance liquid chromatography-tandem mass spectrometry

    International Nuclear Information System (INIS)

    Xia Xi; Ding Shuangyang; Li Xiaowei; Gong Xiao; Zhang Suxia; Jiang Haiyang; Li Jiancheng; Shen Jianzhong

    2009-01-01

    A sensitive and reliable method was developed and validated for detection and confirmation of melamine in egg based on gas chromatography-mass spectrometry (GC-MS) and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Trichloroacetic acid solution was used for sample extraction and precipitation of proteins. The aqueous extracts were subjected to solid-phase extraction by mixed-mode reversed-phase/strong cation-exchange cartridges. Using ultra-performance liquid chromatography and electrospray ionization in the positive ion mode, melamine was determined by LC-MS/MS, which was completed in 5 min for each injection. For the GC-MS analysis, extracted melamine was derivatized with N,O-bis(trimethylsilyl)trifluoracetamide prior to selected ion monitoring detection in electron impact mode. The average recovery of melamine from fortified samples ranged from 85.2% to 103.2%, with coefficients of variation lower than 12%. The limit of detection obtained by GC-MS and UPLC-MS/MS was 10 and 5 μg kg -1 , respectively. This validated method was successfully applied to the determination of melamine in real samples from market.

  10. Flame atomic absorption spectrometric determination of heavy metals in aqueous solution and surface water preceded by co-precipitation procedure with copper(II) 8-hydroxyquinoline

    Science.gov (United States)

    Ipeaiyeda, Ayodele Rotimi; Ayoade, Abisayo Ruth

    2017-12-01

    Co-precipitation procedure has widely been employed for preconcentration and separation of metal ions from the matrices of environmental samples. This is simply due to its simplicity, low consumption of separating solvent and short duration for analysis. Various organic ligands have been used for this purpose. However, there is dearth of information on the application of 8-hydroxyquinoline (8-HQ) as ligand and Cu(II) as carrier element. The use of Cu(II) is desirable because there is no contamination and background adsorption interference. Therefore, the objective of this study was to use 8-HQ in the presence of Cu(II) for coprecipitation of Cd(II), Co(II), Cr(III), Ni(II) and Pb(II) from standard solutions and surface water prior to their determinations by flame atomic absorption spectrometry (FAAS). The effects of pH, sample volume, amount of 8-HQ and Cu(II) and interfering ions on the recoveries of metal ions from standard solutions were monitored using FAAS. The water samples were treated with 8-HQ under the optimum experimental conditions and metal concentrations were determined by FAAS. The metal concentrations in water samples not treated with 8-HQ were also determined. The optimum recovery values for metal ions were higher than 85.0%. The concentrations (mg/L) of Co(II), Ni(II), Cr(III), and Pb(II) in water samples treated with 8-HQ were 0.014 ± 0.002, 0.03 ± 0.01, 0.04 ± 0.02 and 0.05 ± 0.02, respectively. These concentrations and those obtained without coprecipitation technique were significantly different. Coprecipitation procedure using 8-HQ as ligand and Cu(II) as carrier element enhanced the preconcentration and separation of metal ions from the matrix of water sample.

  11. Sequential injection approach for simultaneous determination of ultratrace plutonium and neptunium in urine with accelerator mass spectrometry

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per

    2013-01-01

    An analytical method was developed for simultaneous determination of ultratrace level plutonium (Pu) and neptunium (Np) using iron hydroxide coprecipitation in combination with automated sequential injection extraction chromatography separation and accelerator mass spectrometry (AMS) measurement...... show that preboiling and aging are important for obtaining high chemical yields for both Pu and Np, which is possibly related to the aggregation and adsorption behavior of organic substances contained in urine. Although the optimal condition for Np and Pu simultaneous determination requires 5-day aging...

  12. Determination of zinc in ammoniacal ore leaching solutions by X-ray fluorescence spectrometry using a radioactive source

    International Nuclear Information System (INIS)

    Cornejo, N.; Afailal, A.; Garcia, F.; Palacios, M.

    1994-01-01

    A method was developed for the fast determination of zinc in leaching solutions by radioisotope energy-dispersive X-ray fluorescence (EDXRF) spectrometry. The measured intensities were used to develop regression models for estimating the zinc concentration. The primary radiation was provided by the 244 Cm radioisotope. Several experimental parameters including the saturation thickness and detection limit were determined. The advantages of the utilization of conditioning agents with elements of low atomic number such as nitric acid were established. (orig.)

  13. DETERMINATION OF TOTAL MERCURY IN FISH TISSUES USING PYROLYSIS ATOMIC ABSORPTION SPECTROMETRY WITH GOLD AMALGAMATION

    Science.gov (United States)

    A simple and rapid procedure for measuring total mercury in fish tissues is evaluated and compared with conventional techniques. Using an automated instrument incorporating combustion, preconcentration by amalgamation with gold, and atomic absorption spectrometry (AAS), mill...

  14. Determination of sulfur in food by high resolution continuum source flame molecular absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zambrzycka, Elżbieta; Godlewska-Żyłkiewicz, Beata, E-mail: bgodlew@uwb.edu.pl

    2014-11-01

    In the present work, a fast, simple and sensitive analytical method for determination of sulfur in food and beverages by high resolution continuum source flame molecular absorption spectrometry was developed. The determination was performed via molecular absorption of carbon monosulfide, CS. Different CS rotational lines (257.959 nm, 258.033 nm, 258.055 nm), number of pixels and types of standard solution of sulfur, namely: sulfuric acid, sodium sulfate, ammonium sulfate, sodium sulfite, sodium sulfide, DL-cysteine, and L-cystine, were studied in terms of sensitivity, repeatability of results as well as limit of detection and limit of quantification. The best results were obtained for measurements of absorption of the CS molecule at 258.055 nm at the wavelength range covering 3 pixels and DL-cysteine in 0.2 mol L{sup −1} HNO{sub 3} solution as a calibration standard. Under optimized conditions the limit of detection and the limit of quantification achieved for sulfur were 10.9 mg L{sup −1} and 36.4 mg L{sup −1}, respectively. The repeatability of the results expressed as relative standard deviation was typically < 5%. The accuracy of the method was tested by analysis of digested biological certified reference materials (soya bean flour, corn flour and herbs) and recovery experiment for beverage samples with added known amount of sulfur standard. The recovery of analyte from such samples was in the range of 93–105% with the repeatability in the range of 4.1–5.0%. The developed method was applied for the determination of sulfur in milk (194 ± 10 mg kg{sup −1}), egg white (2188 ± 29 mg kg{sup −1}), mineral water (31.0 ± 0.9 mg L{sup −1}), white wine (260 ± 4 mg L{sup −1}) and red wine (82 ± 2 mg L{sup −1}), as well as in sample rich in ions, such as bitter mineral water (6900 ± 100 mg L{sup −1}). - Highlights: • HR-CS FMAS technique was used for sulfur measurement via molecular absorption of carbon monosulfide, CS. • Organic DL

  15. Online liquid chromatography-tandem mass spectrometry cyanide determination in blood.

    Science.gov (United States)

    Lacroix, C; Saussereau, E; Boulanger, F; Goullé, J P

    2011-04-01

    An original liquid chromatography-tandem mass spectrometry (LC-MS-MS) method coupled to online extraction has been developed for cyanide determination in blood. A method involving fluorimetric detection after naphthalene-2,3-dicarboxyaldehyde (NDA) complexation by taurine in the presence of cyanide was previously described. Its performance was limited because of the absence of an internal standard (IS). Using cyanide isotope (13)C(15)N as IS allowed quantification in MS-MS. After the addition of (13)C(15)N, 25 μL of blood were diluted in water and deproteinized with methanol. Following derivatization with NDA and taurine for 10 min at 4°C, 100 μL was injected into the online LC-MS-MS system. An Oasis HLB was used as an extraction column, and a C18 Atlantis was the analytical column. The chromatographic cycle was performed with an ammonium formate (20 mM, pH 2.8) (solvent A) and acetonitrile/solvent A (90:10, v/v) gradient in 6 min. Detection was performed in negative electrospray ionization mode (ESI(-)) with a Quattro Micro. For quantification, transitions of derivatives formed with CN and (13)C(15)N were monitored, respectively, as follows: 299.3/191.3 and 301.3/193.3. The procedure was fully validated, linear from 26 to 2600 ng/mL with limit of detection of 10 ng/mL. This method, using a small blood sample, is not only simple, but also time saving. The specificity and sensitivity of LC-MS-MS coupled to online extraction and using (13)C(15)N as the IS make this method very suitable for cyanide determination in blood and could be useful in forensic toxicology.

  16. Gas chromatography–triple quadrupole mass spectrometry for the determination of atmospheric polychlorinated naphthalenes

    Energy Technology Data Exchange (ETDEWEB)

    Li, Fang [Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Jin, Jing [Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023 (China); Sun, Xiaoli [Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Wang, Xueli; Li, Yun; Shah, Syed Mazhar [Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023 (China); Chen, Jiping, E-mail: chenjp@dicp.ac.cn [Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023 (China)

    2014-09-15

    Highlights: • Atmospheric PCNs were detected by isotope-dilution GC–MS/MS. • The pollution levels of PCNs covering from mono- to octa-CNs were investigated comprehensively in air samples. • The dioxin-like toxicity and human exposure levels of PCNs in air samples were estimated. - Abstract: Atmospheric polychlorinated naphthalenes (PCNs) ranging from mono-CNs to octa-CNs were detected using isotope-dilution gas chromatography coupled with triple quadrupole mass spectrometry (GC–MS/MS). The developed instrumental method was successfully applied to the determination of PCNs in technical products. It was observed that there were significant differences in concentrations, homologue profiles, chlorinated contents and total toxic equivalents (∑TEQs) of PCNs for four Halowax products. Subsequently, the validation of the analytical method was evaluated for the determination of PCNs in air samples in terms of method detection limit (MDL), recovery and matrix effect. The results demonstrated that this method could provide satisfactory sensitivity and adequate selectivity with lower cost. It was conducted to comprehensively evaluate the levels, composition patterns, ∑TEQs, and daily intake exposure of PCNs in indoor and outdoor air samples. Concentrations and ∑TEQs of PCNs in air samples ranged 47.7–832.7 pg m{sup −3} and 1.31–5.99 fg m{sup −3}, respectively, and the predominant homologues were di- and tri-CNs in the gas phase. The results indicated that this analytical method was useful for the accurate and specific evaluation of dioxin-like toxicity and human exposure levels of PCNs in the atmosphere.

  17. Committed effective dose determination in cereal flours by gamma-ray spectrometry

    International Nuclear Information System (INIS)

    Scheibel, Viviane

    2006-01-01

    The health impact from radionuclides ingestion of foodstuffs was evaluated by the committed effective doses determined in commercial samples of South-Brazilian cereal flours (soy, wheat, corn, manioc, rye, oat, barley and rice flour). The radioactivity traces of 228 Th, 228 Ra, 226 Ra, 40 K, 7 Be and 137 Cs were measured by gamma-ray spectrometry employing a 66% relative efficiency HPGe detector. The energy resolution for the 1332.46 keV line of 60 Co was 2.03 keV. The committed effective doses were calculated with the activities analyzed in the present flour samples, the foodstuff rates of consumption (Brazilian Institute of Geography and Statistics) and the ingestion dose coefficients (International Commission of Radiological Protection). The reliability median activities were verified with χ 2 tests, assuring the fittings quality. The highest concentration levels of 228 Th and 40 K were 3.5 ± 0.4 and 1469 ± 17 Bq.kg -1 for soy flour, respectively, with 95% of confidence level. The lower limit of detection for 137 Cs ranged from 0.04 to 0.4 Bq.kg -1 . The highest committed effective dose was 0.36 μSv.y -1 for 228 Ra in manioc flour (adults). All committed effective doses determined at the present work were lower than the UNSCEAR limits of 140 μSv.y -1 and much lower than the ICRP (1991) limits of 1 mSv.y -1 , for general public. There are few literature references for natural and artificial radionuclides in foodstuffs and mainly for committed effective doses. This work brings the barley flour data, which is not present at the literature and 7 Be data which is not encountered in foodstuffs at the literature, besides all the other flours data information about activities and committed effective doses. (author)

  18. 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)

  19. Isotope dilution alpha spectrometry for the determination of plutonium concentration in irradiated fuel dissolver solution : IDAS and R-IDAS

    International Nuclear Information System (INIS)

    Ramaniah, M.V.; Jain, H.C.; Aggarwal, S.K.; Chitambar, S.A.; Kavimandan, V.D.; Almaula, A.I.; Shah, P.M.; Parab, A.R.; Sant, V.L.

    1980-01-01

    The report presents a new technique, Isotope Dilution Alpha Spectrometry (IDAS) and Reverse Isotope Dilution Alpha Spectrometry (R-IDAS) for determining the concentration of plutonium in the irradiated fuel dissolver solution. The method exploits sup(238)Pu in IDAS and sup(239)Pu in R-IDAS as a spike and provides an alternative method to Isotope Dilution Mass Spectrometry (IDMS) which requires enriched sup(242)Pu as a spike. Depending upon the burn-up of the fuel, sup(238)Pu or sup(239)Pu is used as a spike to change the sup(238)Pu/(sup(239)Pu+sup(240)Pu)α activity ratio in the sample by a factor of 10. This change is determined by α-spectrometry on electrodeposited sources using a solid state silicon surface barrier detector coupled to a multichannel analyser. The validity of a simple method based on the geometric progression (G.P.) decrease for the far tail of the spectrum to correct for the tail contribution of sup(238)Pu peak (5.50 MeV) to the low energy sup(239)Pu + sup(240)Pu peak (5.17 MeV) is established. Results for the plutonium concentration on different irradiated fuel dissolver solutions with burn-uo ranging from J,000 to 100,000 MWD/TU are presented and compared with those obtained by IDMS. The values obtained by IDAS or R-IDAS and IDMS agree within 0.5%. (auth.)

  20. Final results of the PIDIE intercomparison exercise for the plutonium isotopic determination by gamma-ray spectrometry

    International Nuclear Information System (INIS)

    Morel, J.; Chauvenet, B.; Etcheverry, M.

    1991-01-01

    Final results from the PIDIE intercomparison exercise organised by the ESARDA Working Group on techniques and standards for non-destructive analysis are presented. The aim of this exercise carried out in 1988 was to test the gamma-ray spectroscopy methods used to determine the plutonium isotopic ratios in a large range of isotopic composition, in order to analyse the parameters and the error sources influencing the results. Sets of seven sealed samples of different plutonium isotopic composition were sent to nine participating laboratories. The final results with uncertainty indicators are reported; they are compared with complementary mass-spectrometry determinations. No important bias has been observed from this exercise. Significant improvements in plutonium isotopic determination by gamma-ray spectrometry come from both more elaborate spectrum analysis methods and better equipment

  1. Application of l-cystine modified zeolite for preconcentration and determination of ultra-trace levels of cadmium by flame atomic absorption spectrometry.

    Science.gov (United States)

    Rezvani, Seyyed Ahmad; Soleymanpour, Ahmad

    2016-03-04

    A very convenient, sensitive and precise solid phase extraction (SPE) system was developed for enrichment and determination of ultra-trace of cadmium ion in water and plant samples. This method was based on the retention of cadmium(II) ions by l-cystine adsorbed in Y-zeolite and carry out in a packed mini-column. The retained cadmium ions then were eluted and determined by flame atomic absorption spectrometry. The scanning electron microscopy (SEM), powder X-ray diffraction (XRD) and Fourier Transform Infrared (FT-IR) spectroscopy techniques were applied for the characterization of cystine modified zeolite (CMZ). Some experimental conditions affecting the analytical performance such as pH, eluent type, concentration of sample, eluent flow rate and also the presence of interfering ions were investigated. The calibration graph was linear within the range of 0.1-7.5ngmL(-1) and limit of detection was obtained 0.04ngmL(-1) with the preconcentration factor of 400. The relative standard deviation (RSD) was obtained 1.4%, indicating the excellent reproducibility of this method. The proposed method was successfully applied for the extraction and determination of cadmium(II) ion in black tea, cigarette's tobacco and also various water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Determination of activities of human carbonic anhydrase II inhibitors ...

    African Journals Online (AJOL)

    the esterase activity of CA-II using 4-NPA as a substrate in 96-well plates. Dimethyl sulfoxide was used ... intensive search for novel drugs is ongoing, through synthesis of new ..... License (http://creativecommons.org/licenses/by/. 4.0) and the ...

  3. Determination of uranium from nuclear fuel in environmental samples using inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Boulyga, S.F.; Becker, J.S.

    2000-01-01

    As a result of the accident at the Chernobyl nuclear power plant (NPP) the environment was contaminated with spent nuclear fuel. The 236 U isotope was used in this study to monitor the spent uranium from nuclear fallout in soil samples collected in the vicinity of the Chernobyl NPP. A rapid and sensitive analytical procedure was developed for uranium isotopic ratio measurement in environmental samples based on inductively coupled plasma quadrupole mass spectrometry with a hexapole collision cell (HEX-ICP-QMS). The figures of merit of the HEX-ICP-QMS were studied with a plasma-shielded torch using different nebulizers (such as an ultrasonic nebulizer (USN) and Meinhard nebulizer) for solution introduction. A 238 U + ion intensity of up to 27000 MHz/ppm in HEX-ICP-QMS with USN was observed by introducing helium into the hexapole collision cell as the collision gas at a flow rate of 10 ml min -1 . The formation rate of uranium hydride ions UH + /U + of 2 x 10 -6 was obtained by using USN with a membrane desolvator. The limit of 236 U/ 238 U ratio determination in 10 μg 1 -1 uranium solution was 3 x 10 -7 corresponding to the detection limit for 236 U of 3 pg 1 -1 . The precision of uranium isotopic ratio measurements in 10 μg 1 -1 laboratory uranium isotopic standard solution was 0.13% ( 235 U/ 238 U) and 0.33% ( 236 U/ 238 U) using a Meinhard nebulizer and 0.45% ( 235 U/ 238 U) and 0.88% ( 236 U/ 238 U) using a USN. The isotopic composition of all investigated Chernobyl soil samples differed from those of natural uranium; i.e. in these samples the 236 U/ 238 U ratio ranged from 10 -5 to 10 -3 . (orig.)

  4. Determination of aflatoxins in medicinal plants by high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Siddique, Nadeem A; Mujeeb, Mohd; Ahmad, Sayeed; Panda, Bibhu P; Makhmoor, Mohd

    2013-01-01

    The intention of the proposed work is to study the presence of the aflatoxins B1, B2, G1 and G2 in medicinal plants, namely Mucuna pruriens, Delphinium denudatum and Portulaca oleraceae. The aflatoxins were extracted, purified by immunoaffinity column chromatography and analysed by high-performance liquid chromatography-tandem quadrupole mass spectrometry with electrospray ionisation (HPLC-MS/MS). Fungal count was carried out in PDA media. A good linear relationship was found for AFB1, AFB2, AFG1 and AFG2 at 1-10 ppb (r>0.9995). The analyte accuracy under three different spiking levels was 86.7-108.1 %, with low per cent relative standard deviations in each case. The aflatoxins can be separated within 5 to7 min using an Agilent XDB C18-column. We found that AFB1 and AFB2 were in trace amounts below the detection limit in M. pruriens whilst they were not detected in D. denudatum. P. oleraceae was found to be contaminated with AFB1 and AFB2. AFG1 and AFG2 were not detected in M. pruriens, P. oleraceae and were below the detection limit in D. denudatum. This was consistent with very low numbers of fungal colonies observed after 6 hr of incubation. The analytical method developed is simple, precise, accurate, economical and can be effectively used to determine the aflatoxins in medicinal plants and therefore to control the quality of products. The aflatoxin levels in the plant extracts examined were related to the minimal fungal load in the medicinal plants examined.

  5. Determination of the serine palmitoyl transferase inhibitor myriocin by electrospray and Q-trap mass spectrometry.

    Science.gov (United States)

    Campisi, Giuseppe Matteo; Signorelli, Paola; Rizzo, Jessica; Ghilardi, Claudio; Antognetti, Jacopo; Caretti, Anna; Lazarević, Jelena S; Strettoi, Enrica; Novelli, Elena; Ghidoni, Riccardo; Rubino, Federico Maria; Paroni, Rita

    2017-12-01

    Myriocin is a potent inhibitor of serine-palmitoyl-transferase, the first and rate-determining enzyme in the sphingolipids biosynthetic pathway. This study developed, validated and applied a LC-MS/MS method to measure myriocin in minute specimens of animal tissue. The chemical analog 14-OH-myriocin was used as the internal standard. The two molecules were extracted from the tissue homogenate by solid-phase extraction, separated by gradient reversed-phase liquid chromatography and measured by negative ion electrospray mass spectrometry in the triple quadrupole. Detection was accomplished by multiple reaction monitoring, employing the most representative transitions, 400@104 and 402@104 for myriocin and 14-OH-myriocin, respectively. The typical limit of detection and lower limit of quantitation of the optimized method were 0.9 pmol/mL (~0.016 pmol injected) and 2.3 pmol/mL, respectively, and the method was linear up to 250 pmol/mL range (r 2  = 0.9996). The intra- and between-day repeatability afforded a coefficient of variation ≤7.0%. Applications included quantification of myriocin in mouse lungs after 24 h from administration of ~4 nmol by intra-tracheal delivery. Measured levels ranged from 4.11 (median; 2.3-7.4 IQR, n = 4) to 11.7 (median; 7.6-22.7 interquartile range (IQR), n = 6) pmol/lung depending on the different formulations used. Myriocin was also measured in retinas of mice treated by intravitreal injection and ranged from 0.045 (less than the limit of detection) to 0.35 pmol/retina. Copyright © 2017 John Wiley & Sons, Ltd.

  6. Multiresidue Analysis of 86 Pesticides Using Gas Chromatography Mass Spectrometry: II-Nonleafy Vegetables

    Directory of Open Access Journals (Sweden)

    M. H. EL-Saeid

    2013-01-01

    Full Text Available A total of 1057 samples of fresh vegetables from import and domestic production were analyzed (cold pepper, egg plant, carrot, cucumber, potato, hot pepper, cultivation tomato, squash, beans, okra, onions, cauliflower, and green house tomato. The aim of this study was to investigate pesticide residues in market foods in Riyadh, which have been collected from Riyadh Development Company (Al-Tamer Vegetables Market. Pesticide residues were determined by gas chromatography with mass selective detector (GC-MSD. A multiresidue method was developed and described for simultaneous determination of 86 pesticides commonly used in crop protection. This method used to determine 86 pesticide residues with a broad range of physicochemical properties in fresh vegetables related to organophosphorus (OPP, organochlorines (OCP, pyrethroids, and carbamates mainly used in agriculture. Sample extract was cleaned up by using AOAC method. Pesticide residues above the maximum residue limits (MRL were detected in 15.89% of the total samples (168 from 1057 samples, but 83.90% of the total samples (887 from 1057 samples has no residues or contained pesticide residues at or below MRL. The detected and most frequently found pesticide residues were permethrin (45 times and endosulfan (34 times followed by deltamethrin (27 times. The findings of this study pointed to the following recommendations: the need for a monitoring program for pesticide residues in imported food crops.

  7. 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...

  8. Simultaneous determination of arsenic and antimony by hydride generation atomic fluorescence spectrometry with dielectric barrier discharge atomizer

    Energy Technology Data Exchange (ETDEWEB)

    Xing Zhi [Department of Chemistry, Key Laboratory for Atomic and Molecular Nanosciences of the Education Ministry, Tsinghua University, Beijing 100084 (China); Kuermaiti, Biekesailike [Department of Chemistry, Key Laboratory for Atomic and Molecular Nanosciences of the Education Ministry, Tsinghua University, Beijing 100084 (China); Products Quality Inspection Institute, Yili, Xinjiang 835000 (China); Wang Juan; Han Guojun; Zhang Sichun [Department of Chemistry, Key Laboratory for Atomic and Molecular Nanosciences of the Education Ministry, Tsinghua University, Beijing 100084 (China); Zhang Xinrong, E-mail: xrzhang@mail.tsinghua.edu.cn [Department of Chemistry, Key Laboratory for Atomic and Molecular Nanosciences of the Education Ministry, Tsinghua University, Beijing 100084 (China)

    2010-12-15

    Simultaneous determination of As and Sb by hydride generation atomic fluorescence spectrometry was developed with the dielectric barrier discharge plasma as the hydride atomizer. The low-temperature and atmospheric-pressure micro-plasma was generated in a quartz cylindrical configuration device, which was constructed by an axial internal electrode and an outer electrode surrounding outside of the tube. The optimization of the atomizer construction and parameters for hydride generation and fluorescence detection systems were carried out. Under the optimized conditions, the detection limits for As and Sb were 0.04 and 0.05 {mu}g L{sup -1}, respectively. In addition, the applicability of the present method was confirmed by the detection of As and Sb in reference materials of quartz sandstone (GBW07106) and argillaceous limestone (GBW07108). The present work provided a new approach to exploit the miniaturized hydride generation dielectric barrier discharge atomic fluorescence spectrometry system for simultaneous multi-element determination.

  9. Matrix effect on the determination of synthetic corticosteroids and diuretics by liquid chromatography-tandem mass spectrometry

    Science.gov (United States)

    Dikunets, M. A.; Appolonova, S. A.; Rodchenkov, G. M.

    2009-04-01

    This work presents a high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) procedure for selective and reliable screening of corticosteroids and diuretics in human urine. Sample preparation included the extraction, evaporation of the organic extract under nitrogen, and solution of the dry residue. The extract was analyzed by HPLC combined with tandem mass spectrometry using electro-spraying ionization at atmospheric pressure with negative ion recording. The mass spectra of all compounds were recorded, and the characteristic ions, retention times, and detection limits were determined. The procedure was validated by evaluating the degree of the matrix suppression of ionization, extraction of analytes from human biological liquid, and the selectivity and specificity of determination.

  10. Simultaneous determination of arsenic and antimony by hydride generation atomic fluorescence spectrometry with dielectric barrier discharge atomizer

    International Nuclear Information System (INIS)

    Xing Zhi; Kuermaiti, Biekesailike; Wang Juan; Han Guojun; Zhang Sichun; Zhang Xinrong

    2010-01-01

    Simultaneous determination of As and Sb by hydride generation atomic fluorescence spectrometry was developed with the dielectric barrier discharge plasma as the hydride atomizer. The low-temperature and atmospheric-pressure micro-plasma was generated in a quartz cylindrical configuration device, which was constructed by an axial internal electrode and an outer electrode surrounding outside of the tube. The optimization of the atomizer construction and parameters for hydride generation and fluorescence detection systems were carried out. Under the optimized conditions, the detection limits for As and Sb were 0.04 and 0.05 μg L -1 , respectively. In addition, the applicability of the present method was confirmed by the detection of As and Sb in reference materials of quartz sandstone (GBW07106) and argillaceous limestone (GBW07108). The present work provided a new approach to exploit the miniaturized hydride generation dielectric barrier discharge atomic fluorescence spectrometry system for simultaneous multi-element determination.

  11. A High Sensitivity Micro Format Chemiluminescence Enzyme Inhibition Assay for Determination of Hg(II

    Directory of Open Access Journals (Sweden)

    Kanchanmala Deshpande

    2010-06-01

    Full Text Available A highly sensitive and specific enzyme inhibition assay based on alcohol oxidase (AlOx and horseradish peroxidase (HRP for determination of mercury Hg(II in water samples has been presented. This article describes the optimization and miniaturization of an enzymatic assay using a chemiluminescence reaction. The analytical performance and detection limit for determination of Hg(II was optimized in 96 well plates and further extended to 384 well plates with a 10-fold reduction in assay volume. Inhibition of the enzyme activity by dissolved Hg(II was found to be linear in the range 5–500 pg.mL−1 with 3% CVin inter-batch assay. Due to miniaturization of assay in 384 well plates, Hg(II was measurable as low as 1 pg.mL−1 within15 min. About 10-fold more specificity of the developed assay for Hg(II analysis was confirmed by challenging with interfering divalent metal ions such as cadmium Cd(II and lead Pb(II. Using the proposed assay we could successfully demonstrate that in a composite mixture of Hg(II, Cd(II and Pb(II, inhibition by each metal ion is significantly enhanced in the presence of the others. Applicability of the proposed assay for the determination of the Hg(II in spiked drinking and sea water resulted in recoveries ranging from 100–110.52%.

  12. Cu determination in crude oil distillation products by atomic absorption and inductively coupled plasma mass spectrometry after analyte transfer to aqueous solution

    International Nuclear Information System (INIS)

    Kowalewska, Zofia; Ruszczynska, Anna; Bulska, Ewa

    2005-01-01

    Cu was determined in a wide range of petroleum products from crude oil distillation using flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICP-MS). Different procedures of sample preparation were evaluated: (i) mineralization with sulfuric acid in an open system (ii) mineralization in a closed microwave system (iii) combustion in hydrogen-oxygen flame in the Wickbold's apparatus (iv) matrix evaporation followed by acid dissolution, and (v) acidic extraction. All the above procedures led to the transfer of the analyte into an aqueous solution for the analytical measurement step. It was found that application of FAAS was limited to the analysis of the heaviest petroleum products of high Cu content. In ICP-MS, the use of internal reference method (with Rh or In as internal reference element) was required to eliminate the matrix effects in the analysis of extracts and the concentrated solutions of mineralized heavy petroleum products. The detection limits (in original samples) were equal to, respectively, 10, 86, 3.3, 0.9 and 0.4 ng g -1 in procedures i-v with ETAAS detection and 10, 78, 1.1 and 0.5 ng g -1 in procedures i-iii and v with ICP-MS detection. The procedures recommended here were validated by recovery experiments, certified reference materials analysis and comparison of results, obtained for a given sample, in different ways. The Cu content in the analyzed samples was: 50-110 ng g -1 in crude oil, -1 in gasoline, -1 in atmospheric oil, -1 in heavy vacuum oil and 140-300 ng g -1 in distillation residue

  13. Cu determination in crude oil distillation products by atomic absorption and inductively coupled plasma mass spectrometry after analyte transfer to aqueous solution

    Science.gov (United States)

    Kowalewska, Zofia; Ruszczyńska, Anna; Bulska, Ewa

    2005-03-01

    Cu was determined in a wide range of petroleum products from crude oil distillation using flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICP-MS). Different procedures of sample preparation were evaluated: (i) mineralization with sulfuric acid in an open system, (ii) mineralization in a closed microwave system, (iii) combustion in hydrogen-oxygen flame in the Wickbold's apparatus, (iv) matrix evaporation followed by acid dissolution, and (v) acidic extraction. All the above procedures led to the transfer of the analyte into an aqueous solution for the analytical measurement step. It was found that application of FAAS was limited to the analysis of the heaviest petroleum products of high Cu content. In ICP-MS, the use of internal reference method (with Rh or In as internal reference element) was required to eliminate the matrix effects in the analysis of extracts and the concentrated solutions of mineralized heavy petroleum products. The detection limits (in original samples) were equal to, respectively, 10, 86, 3.3, 0.9 and 0.4 ng g - 1 in procedures i-v with ETAAS detection and 10, 78, 1.1 and 0.5 ng g - 1 in procedures i-iii and v with ICP-MS detection. The procedures recommended here were validated by recovery experiments, certified reference materials analysis and comparison of results, obtained for a given sample, in different ways. The Cu content in the analyzed samples was: 50-110 ng g - 1 in crude oil, oil, oil and 140-300 ng g - 1 in distillation residue.

  14. Determination of uranium and thorium isotopes by solid phase extraction and alpha spectrometry

    International Nuclear Information System (INIS)

    Kuruc, J.; Kovacova, M.; Strisovska, J.; Galanda, D.

    2013-01-01

    The aim of this work was to test the modified method suitable for the separation of isotopes of uranium and thorium samples of rocks, including gold ore and gold concentrate using of extraction chromatography method, after digestion of the sample, concentrating, separate the isotopes of uranium and thorium isotopes to prepare sources for the measurement of alpha spectra. Samples of rocks, gold ore and gold concentrate were digered in microwave decomposition in the environment of hydrogen peroxide and concentrated nitric acid. For the separation of uranium and thorium the vacuum box with cartridges DGA Resin and Resin(R) UTEVA (Triskem International, France) was used. Both sorbents allow separation of uranium from thorium. The results confirmed that the both sorbents give the same results within expanded uncertainty. The mass activity of monitored uranium and thorium radioisotopes was determined by alpha spectrometry method. The yields of separation were determined using uranium-232 as a tracer radionuclide; the activity of 232 U was 0.1438 Bq. Alpha spectra were measured on the Alpha spectrometer EG and G ORTEC 576A with the software MAESTRO, MCA Emulator and Gamma Vision-32 for Windows, USA. Mass activities of radionuclides were converted to mass concentration of isotopes 238 U, 234 U, 232 Th, 230 Th and 228 Th. The highest concentration of 238 U was sampled in granodiorite (Tunnel S-XIV-2, southwards, mining of Cu ore, not working there since 1990), where m( 238 U) = (0.81 ± 0.09) mg kg -1 (DGA Resin) and m( 238 U) = (0.90 ± 0.09) mg kg -1 (UTEVA(R) Resin), as well as m( 232 Th) = (18.8 ± 1.7) mg kg -1 (DGA Resin) and m( 232 Th) = (17.8 ± 1.5) mg kg -1 (UTEVA(R) Resin). In other samples of rocks, gold ore and gold concentrates have specific masses of isotopes of uranium and thorium two-to ten-folds lower. It can be concluded that the rocks, gold ores and concentrates of gold from the 'Rozalia' mine contain lower concentrations of uranium several times against

  15. Determination of Mercury in an Assortment of Dietary Supplements Using an Inexpensive Combustion Atomic Absorption Spectrometry Technique

    OpenAIRE

    Levine, Keith E.; Levine, Michael A.; Weber, Frank X.; Hu, Ye; Perlmutter, Jason; Grohse, Peter M.

    2005-01-01

    The concentrations of mercury in forty, commercially available dietary supplements, were determined using a new, inexpensive analysis technique. The method involves thermal decomposition, amalgamation, and detection of mercury by atomic absorption spectrometry with an analysis time of approximately six minutes per sample. The primary cost savings from this approach is that labor-intensive sample digestion is not required prior to analysis, further automating the analytical procedure. As a res...

  16. The measurement of abundance and content of 148Nd monitor for the determination of burnup with mass spectrometry

    International Nuclear Information System (INIS)

    Gao Shuqin; Li Silin

    1992-09-01

    The abundance and content of nuclide 148 Nd, which is used as monitor to determine reactor element burnup, were measured by mass spectrometry, and the burnup can be calculated from measured results. The distribution of 148 Nd abundance and content in the axial direction are consistent with the theoretical calculation. The burnup values agree with the data obtained from heavy isotope ratio and radiochemistry methods within the errors of 4.0% and 2.8% respectively

  17. Determination of nickel in chloralkali electrolysis brines by X-ray fluorescence spectrometry on a membrane filter

    International Nuclear Information System (INIS)

    Andrade, L.L.; Minzl, E.

    1984-01-01

    X-ray fluorescence spectrometry after ammonium pyrrolidinedithiocarbamate (APDC) preconcentration is proposed for the determination of nickel in chloralkali electrolysis brines. The optimum conditions for the precipitation target tube, peak intensity, background, analysing crystal, counters and exposure time were investigated. The method was applied to chloralkali brines of evaporite salts (halite, sylvinite, carnallite and tachhydrite), sodium, potassium and magnesium salts, explored in Sergipe (Brazil), by Petrobras-Mineracao S.A.(Author) [pt

  18. Determination of drugs and drug-like compounds in different samples with direct analysis in real time mass spectrometry.

    Science.gov (United States)

    Chernetsova, Elena S; Morlock, Gertrud E

    2011-01-01

    Direct analysis in real time (DART), a relatively new ionization source for mass spectrometry, ionizes small-molecule components from different kinds of samples without any sample preparation and chromatographic separation. The current paper reviews the published data available on the determination of drugs and drug-like compounds in different matrices with DART-MS, including identification and quantitation issues. Parameters that affect ionization efficiency and mass spectra composition are also discussed. Copyright © 2011 Wiley Periodicals, Inc.

  19. 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....

  20. Determination of trace amounts of selenium in minerals and rocks by flame less atomic-absorption spectrometry

    International Nuclear Information System (INIS)

    Alduan, F. A.; Capdevilla, C.

    1980-01-01

    The determination of trace amounts of selenium In silicate rocks and feldspar by solvent extraction and graphite furnace atomic-absorption spectrometry has been stu- died. Sodium diethyl-ditio carbamate and ammonium pyrrolidine dithiocarbamate have been tried as chelating agents. The best results are achieved when selenium is extracted Into carbon tetrachloride as the sodium diethyldithiocarbamate complex. The method allows to detect 0,75 ppm of selenium in the sample. Recoveries are about 100%. (Author) 7 refs

  1. Radon fixation for determination of 224Ra, 226Ra and 228Ra via gamma-ray spectrometry

    International Nuclear Information System (INIS)

    Herranz, M.; Idoeta, R.; Abelairas, A.; Legarda, F.

    2006-01-01

    The aim of this work is the improvement of the procedure for the determination of radium isotopes activities in water, which is done through radiochemical separation and subsequent gamma-ray spectrometry. In addition, radon gas retention is studied using different activated carbon materials. The results of the IAEA Proficiency test: 'Determination of radium and uranium radionuclides in water' of December 2002 [IAEA, 2003. Analytical quality control services: determination of radium and uranium radionuclides in water. Preliminary Report, Seibersdorf] are considered for this work

  2. Radon fixation for determination of {sup 224}Ra, {sup 226}Ra and {sup 228}Ra via gamma-ray spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Herranz, M. [Departamento Ingenieria Nuclear y Mecanica de Fluidos, E. S. Ingenieros de Bilbao - Universidad del Pais Vasco (UPV/EHU), Alda. Urquijo s/n, 48013 Bilbao (Spain)]. E-mail: inphesom@bi.ehu.es; Idoeta, R. [Departamento Ingenieria Nuclear y Mecanica de Fluidos, E. S. Ingenieros de Bilbao - Universidad del Pais Vasco (UPV/EHU), Alda. Urquijo s/n, 48013 Bilbao (Spain); Abelairas, A. [Departamento Ingenieria Nuclear y Mecanica de Fluidos, E. S. Ingenieros de Bilbao - Universidad del Pais Vasco (UPV/EHU), Alda. Urquijo s/n, 48013 Bilbao (Spain); Legarda, F. [Departamento Ingenieria Nuclear y Mecanica de Fluidos, E. S. Ingenieros de Bilbao - Universidad del Pais Vasco (UPV/EHU), Alda. Urquijo s/n, 48013 Bilbao (Spain)

    2006-04-15

    The aim of this work is the improvement of the procedure for the determination of radium isotopes activities in water, which is done through radiochemical separation and subsequent gamma-ray spectrometry. In addition, radon gas retention is studied using different activated carbon materials. The results of the IAEA Proficiency test: 'Determination of radium and uranium radionuclides in water' of December 2002 [IAEA, 2003. Analytical quality control services: determination of radium and uranium radionuclides in water. Preliminary Report, Seibersdorf] are considered for this work.

  3. Simultaneous preconcentration of cadmium and lead in water samples with silica gel and determination by flame atomic absorption spectrometry.

    Science.gov (United States)

    Xu, Hongbo; Wu, Yun; Wang, Jian; Shang, Xuewei; Jiang, Xiaojun

    2013-12-01

    A new method that utilizes pretreated silica gel as an adsorbent has been developed for simultaneous preconcentration of trace Cd(II) and Pb(II) prior to the measurement by flame atomic absorption spectrometry. The effects of pH, the shaking time, the elution condition and the coexisting ions on the separation/preconcentration conditions of analytes were investigated. Under optimized conditions, the static adsorption capacity of Cd(II) and Pb(II) were 45.5 and 27.1mg/g, the relative standard deviations were 3.2% and 1.7% (for n = 11), and the limits of detection obtained were 4.25 and 0.60 ng/mL, respectively. The method was validated by analyzing the certified reference materials GBW 07304a (stream sediment) and successfully applied to the analysis of various treated wastewater samples with satisfactory results. Copyright © 2013 The Research Centre for Eco-Environmental Sciences, Chinese Academy of Sciences. Published by Elsevier B.V. All rights reserved.

  4. Penicillamine-modified sensor for the voltammetric determination of Cd(II) and Pb(II) ions in natural samples.

    Science.gov (United States)

    Pérez-Ràfols, Clara; Serrano, Núria; Díaz-Cruz, José Manuel; Ariño, Cristina; Esteban, Miquel

    2015-11-01

    A new penicillamine-GCE was developed based on the immobilization of d-penicillamine on aryl diazonium salt monolayers anchored to the glassy carbon electrode (GCE) surface and it was applied for the first time to the simultaneous determination of Cd(II) and Pb(II) ions by stripping voltammetric techniques. The detection and quantification limits at levels of µg L(-1) suggest that the penicillamine-GCE could be fully suitable for the determination of the considered ions in natural samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Modified ionic liquid cold-induced aggregation dispersive liquid-liquid microextraction followed by atomic absorption spectrometry for trace determination of zinc in water and food samples

    International Nuclear Information System (INIS)

    Zeeb, M.; Sadeghi, M.

    2011-01-01

    We report on a new method for the microextraction and determination of zinc (II). The ion is accumulated via ionic-liquid cold-induced aggregation dispersive liquid-liquid microextraction (IL-CIA-DLLME) followed by flame atomic absorption spectrometry (FAAS). The ionic liquid (IL) 1-hexyl-3-methylimidazolium hexafluorophosphate is dispersed into a heated sample solution containing sodium hexafluorophosphate as a common ion source. The solution is then placed in an ice-water bath upon which a cloudy solution forms due to the decrease of the solubility of the IL. Zinc is complexed with 8-hydroxyquinoline and extracted into the IL. The enriched phase is dissolved in a diluting agent and introduced to the FAAS. The method is not influenced by variations in the ionic strength of the sample solution. Factors affecting the performance were evaluated and optimized. At optimum conditions, the limit of detection is 0.18 μg L -1 , and the relative standard deviation is 3.0% (at n=5). The method was validated by recovery experiments and by analyzing a certified reference material and successfully applied to the determination of Zn (II) in water and food samples. (author)

  6. One-step displacement dispersive liquid-liquid microextraction coupled with graphite furnace atomic absorption spectrometry for the selective determination of methylmercury in environmental samples.

    Science.gov (United States)

    Liang, Pei; Kang, Caiyan; Mo, Yajun

    2016-01-01

    A novel method for the selective determination of methylmercury (MeHg) was developed by one-step displacement dispersive liquid-liquid microextraction (D-DLLME) coupled with graphite furnace atomic absorption spectrometry. In the proposed method, Cu(II) reacted with diethyldithiocarbamate (DDTC) to form Cu-DDTC complex, which was used as the chelating agent instead of DDTC for the dispersive liquid-liquid microextraction (DLLME) of MeHg. Because the stability of MeHg-DDTC is higher than that of Cu-DDTC, MeHg can displace Cu from the Cu-DDTC complex and be preconcentrated in a single DLLME procedure. MeHg could be extracted into the extraction solvent phase at pH 6 while Hg(II) remained in the sample solution. Potential interference from co-existing metal ions with lower DDTC complex stability was largely eliminated without the need of any masking reagent. Under the optimal conditions, the limit of detection of this method was 13.6ngL(-1) (as Hg), and an enhancement factor of 81 was achieved with a sample volume of 5.0mL. The proposed method was successfully applied for the determination of trace MeHg in some environmental samples with satisfactory results. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Determination of Sodium, Potassium, Magnesium, and Calcium Minerals Level in Fresh and Boiled Broccoli and Cauliflower by Atomic Absorption Spectrometry

    Science.gov (United States)

    Nerdy

    2018-01-01

    Vegetables from the cabbage family vegetables consumed by many people, which is known healthful, by eaten raw, boiled, or cooked (stir fry or soup). Vegetables like broccoli and cauliflower contain vitamins, minerals, and fiber. This study aims to determine the decrease percentage of sodium, potassium, magnesium, and calcium minerals level caused by boiled broccoli and cauliflower by atomic absorption spectrometry. Boiled broccoli and cauliflower prepared by given boiled treatment in boiling water for 3 minutes. Fresh and boiled broccoli and cauliflower carried out dry destruction, followed by quantitative analysis of sodium, potassium, magnesium, and calcium minerals respectively at a wavelength of 589.0 nm; 766.5 nm; 285.2 nm; and 422.7 nm, using atomic absorption spectrometry methods. After the determination of the sodium, potassium, magnesium, and calcium minerals level followed by validation of analytical methods with accuracy, precision, linearity, range, limit of detection (LOD), and limit of quantitation (LOQ) parameters. Research results show a decrease in the sodium, potassium, magnesium, and calcium minerals level in boiled broccoli and cauliflower compared with fresh broccoli and cauliflower. Validation of analytical methods gives results that spectrometry methods used for determining sodium, potassium, magnesium, and calcium minerals level are valid. It concluded that the boiled gives the effect of decreasing the minerals level significantly in broccoli and cauliflower.

  8. Community air monitoring for pesticides-part 2: multiresidue determination of pesticides in air by gas chromatography, gas chromatography-mass spectrometry, and liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Hengel, Matt; Lee, P

    2014-03-01

    Two multiresidue methods were developed to determine pesticides in air collected in California. Pesticides were trapped using XAD-4 resin and extracted with ethyl acetate. Based on an analytical method from the University of California Davis Trace Analytical Laboratory, pesticides were detected by analyzing the extract by gas chromatography-mass spectrometry (GC-MS) to determine chlorothalonil, chlorthal-dimethyl, cycloate, dicloran, dicofol, EPTC, ethalfluralin, iprodione, mefenoxam, metolachlor, PCNB, permethrin, pronamide, simazine, trifluralin, and vinclozolin. A GC with a flame photometric detector was used to determine chlorpyrifos, chlorpyrifos oxon, diazinon, diazinon oxon, dimethoate, dimethoate oxon, fonophos, fonophos oxon, malathion, malathion oxon, naled, and oxydemeton. Trapping efficiencies ranged from 78 to 92 % for low level (0.5 μg) and 37-104 % for high level (50 and 100 μg) recoveries. Little to no degradation of compounds occurred over 31 days; recoveries ranged from 78 to 113 %. In the California Department of Food and Agriculture (CDFA) method, pesticides were detected by analyzing the extract by GC-MS to determine chlorothalonil, chlorpyrifos, cypermethrin, dichlorvos, dicofol, endosulfan 1, endosulfan sulfate, oxyfluorfen, permethrin, propargite, and trifluralin. A liquid chromatograph coupled to a MS was used to determine azinphos-methyl, chloropyrifos oxon, DEF, diazinon, diazinon oxon, dimethoate, dimethoate oxon, diuron, EPTC, malathion, malathion oxon, metolachlor, molinate, norflurazon, oryzalin, phosmet, propanil, simazine and thiobencarb. Trapping efficiencies for compounds determined by the CDFA method ranged from 10 to 113, 22 to 114, and 56 to 132 % for 10, 5, and 2 μg spikes, respectively. Storage tests yielded 70-170 % recovery for up to 28 days. These multiresidue methods represent flexible, sensitive, accurate, and cost-effective ways to determine residues of various pesticides in ambient air.

  9. Organic solvents as interferents in arsenic determination by hydride generation atomic absorption spectrometry with flame atomization

    Czech Academy of Sciences Publication Activity Database

    Karadjova, I.B.; Lampugnani, L.; Dědina, Jiří; D'Ulivo, A.; Onor, M.; Tsalev, D.L.

    2006-01-01

    Roč. 61, č. 5 (2006), s. 525-531 ISSN 0584-8547 R&D Projects: GA AV ČR IAA400310507 Institutional research plan: CEZ:AV0Z40310501 Keywords : hydride generation * atomic absorption spectrometry * interferences Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.092, year: 2006

  10. New technique for determination of long-lived radioisotopes, Iodine-129, using multiparameter coincidence spectrometry

    International Nuclear Information System (INIS)

    Hatsukawa, Yuichi; Oshima, Masumi; Toh, Yosuke; Shinohara, Nobuo; Kushita, Kosuke; Ueno, Takashi

    2003-01-01

    Multiparameter coincidence γ-ray spectrometry based on g-g coincidence is widely used in the field of nuclear structure studies, and has produced many successful results. In this study, feasibility of the method for neutron activation analysis of long lived iodine isotope, 129 I, was investigated. (author)

  11. 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, ...

  12. Determination of 239Pu/240Pu isotopic ratio by high resolution alpha-particle spectrometry

    International Nuclear Information System (INIS)

    Amoudry, F.; Burger, P.

    1983-05-01

    The development of passivated ion-implanted silicon detectors and of very thin alpha-particle sources improves the resolution of alpha-particle spectra and allows to separate energy pics up to now unseparate. The 239 Pu/ 240 Pu isotopic ratio of a mixture has been measured using the alpha spectrometry deconvolution code DEMO [fr

  13. Determination of Elizabethkingia Diversity by MALDI-TOF Mass Spectrometry and Whole-Genome Sequencing

    DEFF Research Database (Denmark)

    Eriksen, Helle Brander; Gumpert, Heidi; Faurholt, Cecilie Haase

    2017-01-01

    In a hospital-acquired infection with multidrug-resistant Elizabethkingia, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry and 16S rRNA gene analysis identified the pathogen as Elizabethkingia miricola. Whole-genome sequencing, genus-level core genome analysis, and in...

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

    Czech Academy of Sciences Publication Activity Database

    Vojtková, Blanka; Dočekal, Bohumil

    2005-01-01

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

  15. Spent fuel scanning using the gamma spectrometry bench at Osiris. Power and burnup determination

    International Nuclear Information System (INIS)

    Cerles, J.-M.; Simonet, Genevieve.

    1976-01-01

    The Saclay Nuclear Research Center is provided with an original gamma spectrometry facility located inside the pool of the Osiris reactor. It is intended for the gamma scanning of fuel elements irradiated in Osiris or elements of any other origin. The principal characteristics of this facility are given. Special emphasis is put on its [fr

  16. Novel approach to determine ghrelin analogs by liquid chromatography with mass spectrometry using a monolithic column

    Czech Academy of Sciences Publication Activity Database

    Zemenová, Jana; Sýkora, D.; Adámková, H.; Maletínská, Lenka; Elbert, Tomáš; Marek, Aleš; Blechová, Miroslava

    2017-01-01

    Roč. 40, č. 5 (2017), s. 1032-1039 ISSN 1615-9306 Institutional support: RVO:61388963 Keywords : enzyme-linked immunosorbent assay * ghrelin * lipopeptides * liquid chromatography mass spectrometry * monolithic columns Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 2.557, year: 2016

  17. PhTX-II a Basic Myotoxic Phospholipase A2 from Porthidium hyoprora Snake Venom, Pharmacological Characterization and Amino Acid Sequence by Mass Spectrometry

    Science.gov (United States)

    Huancahuire-Vega, Salomón; Ponce-Soto, Luis Alberto; Marangoni, Sergio

    2014-01-01

    A monomeric basic PLA2 (PhTX-II) of 14149.08 Da molecular weight was purified to homogeneity from Porthidium hyoprora venom. Amino acid sequence by in tandem mass spectrometry revealed that PhTX-II belongs to Asp49 PLA2 enzyme class and displays conserved domains as the catalytic network, Ca2+-binding loop and the hydrophobic channel of access to the catalytic site, reflected in the high catalytic activity displayed by the enzyme. Moreover, PhTX-II PLA2 showed an allosteric behavior and its enzymatic activity was dependent on Ca2+. Examination of PhTX-II PLA2 by CD spectroscopy indicated a high content of alpha-helical structures, similar to the known structure of secreted phospholipase IIA group suggesting a similar folding. PhTX-II PLA2 causes neuromuscular blockade in avian neuromuscular preparations with a significant direct action on skeletal muscle function, as well as, induced local edema and myotoxicity, in mice. The treatment of PhTX-II by BPB resulted in complete loss of their catalytic activity that was accompanied by loss of their edematogenic effect. On the other hand, enzymatic activity of PhTX-II contributes to this neuromuscular blockade and local myotoxicity is dependent not only on enzymatic activity. These results show that PhTX-II is a myotoxic Asp49 PLA2 that contributes with toxic actions caused by P. hyoprora venom. PMID:25365526

  18. PhTX-II a Basic Myotoxic Phospholipase A2 from Porthidium hyoprora Snake Venom, Pharmacological Characterization and Amino Acid Sequence by Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Salomón Huancahuire-Vega

    2014-10-01

    Full Text Available A monomeric basic PLA2 (PhTX-II of 14149.08 Da molecular weight was purified to homogeneity from Porthidium hyoprora venom. Amino acid sequence by in tandem mass spectrometry revealed that PhTX-II belongs to Asp49 PLA2 enzyme class and displays conserved domains as the catalytic network, Ca2+-binding loop and the hydrophobic channel of access to the catalytic site, reflected in the high catalytic activity displayed by the enzyme. Moreover, PhTX-II PLA2 showed an allosteric behavior and its enzymatic activity was dependent on Ca2+. Examination of PhTX-II PLA2 by CD spectroscopy indicated a high content of alpha-helical structures, similar to the known structure of secreted phospholipase IIA group suggesting a similar folding. PhTX-II PLA2 causes neuromuscular blockade in avian neuromuscular preparations with a significant direct action on skeletal muscle function, as well as, induced local edema and myotoxicity, in mice. The treatment of PhTX-II by BPB resulted in complete loss of their catalytic activity that was accompanied by loss of their edematogenic effect. On the other hand, enzymatic activity of PhTX-II contributes to this neuromuscular blockade and local myotoxicity is dependent not only on enzymatic activity. These results show that PhTX-II is a myotoxic Asp49 PLA2 that contributes with toxic actions caused by P. hyoprora venom.

  19. Assessment of measurement result uncertainty in determination of 210Pb with the focus on matrix composition effect in gamma-ray spectrometry

    International Nuclear Information System (INIS)

    Iurian, A.R.; Pitois, A.; Kis-Benedek, G.; Migliori, A.; Padilla-Alvarez, R.; Ceccatelli, A.

    2016-01-01

    Reference materials were used to assess measurement result uncertainty in determination of 210 Pb by gamma-ray spectrometry, liquid scintillation counting, or indirectly by alpha-particle spectrometry, using its daughter 210 Po in radioactive equilibrium. Combined standard uncertainties of 210 Pb massic activities obtained by liquid scintillation counting are in the range 2–12%, depending on matrices and massic activity values. They are in the range 1–3% for the measurement of its daughter 210 Po using alpha-particle spectrometry. Three approaches (direct computation of counting efficiency and efficiency transfer approaches based on the computation and, respectively, experimental determination of the efficiency transfer factors) were applied for the evaluation of 210 Pb using gamma-ray spectrometry. Combined standard uncertainties of gamma-ray spectrometry results were found in the range 2–17%. The effect of matrix composition on self-attenuation was investigated and a detailed assessment of uncertainty components was performed. - Highlights: • Confirmed 210 Pb certified values by LSC and alpha-particle spectrometry ( 210 Po). • Assessed 210 Po measurement result uncertainty by alpha-particle spectrometry. • Matrix composition effect on gamma-ray spectrometry measurement result uncertainty. • Assessment of 210 Pb measurement result uncertainty by gamma-ray spectrometry. • Comparison of techniques and approaches: ‘fit-for-purpose’ considerations.

  20. Determination of uranium from nuclear fuel in environmental samples using inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Boulyga, S.F. [Forschungszentrum Juelich GmbH (Germany). Zentralabteilung fuer Chemische Analysen]|[Radiation Physics and Chemistry Problems Inst., Minsk (Belarus); Becker, J.S. [Forschungszentrum Juelich GmbH (Germany). Zentralabteilung fuer Chemische Analysen

    2000-11-01

    As a result of the accident at the Chernobyl nuclear power plant (NPP) the environment was contaminated with spent nuclear fuel. The {sup 236}U isotope was used in this study to monitor the spent uranium from nuclear fallout in soil samples collected in the vicinity of the Chernobyl NPP. A rapid and sensitive analytical procedure was developed for uranium isotopic ratio measurement in environmental samples based on inductively coupled plasma quadrupole mass spectrometry with a hexapole collision cell (HEX-ICP-QMS). The figures of merit of the HEX-ICP-QMS were studied with a plasma-shielded torch using different nebulizers (such as an ultrasonic nebulizer (USN) and Meinhard nebulizer) for solution introduction. A {sup 238}U{sup +} ion intensity of up to 27000 MHz/ppm in HEX-ICP-QMS with USN was observed by introducing helium into the hexapole collision cell as the collision gas at a flow rate of 10 ml min{sup -1}. The formation rate of uranium hydride ions UH{sup +}/U{sup +} of 2 x 10{sup -6} was obtained by using USN with a membrane desolvator. The limit of {sup 236}U/{sup 238}U ratio determination in 10 {mu}g 1{sup -1} uranium solution was 3 x 10{sup -7} corresponding to the detection limit for {sup 236}U of 3 pg 1{sup -1}. The precision of uranium isotopic ratio measurements in 10 {mu}g 1{sup -1} laboratory uranium isotopic standard solution was 0.13% ({sup 235}U/{sup 238}U) and 0.33% ({sup 236}U/{sup 238}U) using a Meinhard nebulizer and 0.45% ({sup 235}U/{sup 238}U) and 0.88% ({sup 236}U/{sup 238}U) using a USN. The isotopic composition of all investigated Chernobyl soil samples differed from those of natural uranium; i.e. in these samples the {sup 236}U/{sup 238}U ratio ranged from 10{sup -5} to 10{sup -3}. (orig.)

  1. Advanced hyphenated chromatographic-mass spectrometry in mycotoxin determination: current status and prospects.

    Science.gov (United States)

    Li, Peiwu; Zhang, Zhaowei; Hu, Xiaofeng; Zhang, Qi

    2013-01-01

    Mass spectrometric techniques are essential for advanced research in food safety and environmental monitoring. These fields are important for securing the health of humans and animals, and for ensuring environmental security. Mycotoxins, toxic secondary metabolites of filamentous fungi, are major contaminants of agricultural products, food and feed, biological samples, and the environment as a whole. Mycotoxins can cause cancers, nephritic and hepatic diseases, various hemorrhagic syndromes, and immune and neurological disorders. Mycotoxin-contaminated food and feed can provoke trade conflicts, resulting in massive economic losses. Risk assessment of mycotoxin contamination for humans and animals generally depends on clear identification and reliable quantitation in diversified matrices. Pioneering work on mycotoxin quantitation using mass spectrometry (MS) was performed in the early 1970s. Now, unambiguous confirmation and quantitation of mycotoxins can be readily achieved with a variety hyphenated techniques that combine chromatographic separation with MS, including liquid chromatography (LC) or gas chromatography (GC). With the advent of atmospheric pressure ionization, LC-MS has become a routine technique. Recently, the co-occurrence of multiple mycotoxins in the same sample has drawn an increasing amount of attention. Thus, modern analyses must be able to detect and quantitate multiple mycotoxins in a single run. Improvements in tandem MS techniques have been made to achieve this purpose. This review describes the advanced research that has been done regarding mycotoxin determination using hyphenated chromatographic-MS techniques, but is not a full-circle survey of all the literature published on this topic. The present work provides an overview of the various hyphenated chromatographic-MS-based strategies that have been applied to mycotoxin analysis, with a focus on recent developments. The use of chromatographic-MS to measure levels of mycotoxins, including

  2. Functional group composition of ambient and source organic aerosols determined by tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Dron, J.; El Haddad, I.; Temime-Roussel, B.; Wortham, H.; Marchand, N. [Univ Aix Marseille, CNRS, Lab Chim Provence, Equipe Instrumentat and React Atmospher, UMR 6264, F-13331 Marseille 3 (France); Jaffrezo, J.L. [Univ Grenoble 1, CNRS, UMR 5183, Lab Glaciol and Geophys Environm, F-38402 St Martin Dheres (France)

    2010-07-01

    The functional group composition of various organic aerosols (OA) is investigated using a recently developed analytical approach based on atmospheric pressure chemical ionisation-tandem mass spectrometry (APCIMS/MS). The determinations of three functional groups contents are performed quantitatively by neutral loss (carboxylic and carbonyl groups, R-COOH and R-CO-R' respectively) and precursor ion (nitro groups, R-NO{sub 2}) scanning modes of a tandem mass spectrometer. Major organic aerosol sources are studied: vehicular emission and wood combustion for primary aerosol sources; and a secondary organic aerosol (SOA) produced through photooxidation of o-xylene. The results reveal significant differences in the functional group contents of these source aerosols. The laboratory generated SOA is dominated by carbonyls while carboxylics are preponderate in the wood combustion particles. On the other hand, vehicular emissions are characterised by a strong nitro content. The total amount of the three functional groups accounts for 1.7% (vehicular) to 13.5% (o-xylene photooxidation) of the organic carbon. Diagnostic functional group ratios are then used to tentatively discriminate sources of particles collected in an urban background environment located in an Alpine valley (Chamonix, France) during a strong winter pollution event. The three functional groups under study account for a total functionalization rate of 2.2 to 3.8% of the organic carbon in this ambient aerosol, which is also dominated by carboxylic moieties. In this particular case study of a deep alpine valley during winter, we show that the nitro- and carbonyl-to-carboxylic diagnostic ratios can be a useful tool to discriminate sources. In these conditions, the total OA concentrations are highly dominated by wood combustion OA. This result is confirmed by an organic markers source apportionment approach which assess a wood burning organic carbon contribution of about 60%. Finally, examples of functional

  3. Functional group composition of ambient and source organic aerosols determined by tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    J. Dron

    2010-08-01

    Full Text Available The functional group composition of various organic aerosols (OA is investigated using a recently developed analytical approach based on atmospheric pressure chemical ionisation-tandem mass spectrometry (APCI-MS/MS. The determinations of three functional groups contents are performed quantitatively by neutral loss (carboxylic and carbonyl groups, R-COOH and R-CO-R´ respectively and precursor ion (nitro groups, R-NO2 scanning modes of a tandem mass spectrometer. Major organic aerosol sources are studied: vehicular emission and wood combustion for primary aerosol sources; and a secondary organic aerosol (SOA produced through photooxidation of o-xylene. The results reveal significant differences in the functional group contents of these source aerosols. The laboratory generated SOA is dominated by carbonyls while carboxylics are preponderate in the wood combustion particles. On the other hand, vehicular emissions are characterised by a strong nitro content. The total amount of the three functional groups accounts for 1.7% (vehicular to 13.5% (o-xylene photooxidation of the organic carbon. Diagnostic functional group ratios are then used to tentatively discriminate sources of particles collected in an urban background environment located in an Alpine valley (Chamonix, France during a strong winter pollution event. The three functional groups under study account for a total functionalisation rate of 2.2 to 3.8% of the organic carbon in this ambient aerosol, which is also dominated by carboxylic moieties. In this particular case study of a deep alpine valley during winter, we show that the nitro- and carbonyl-to-carboxylic diagnostic ratios can be a useful tool to discriminate sources. In these conditions, the total OA concentrations are highly dominated by wood combustion OA. This result is confirmed by an organic markers source apportionment approach which assess a wood burning organic carbon contribution of about 60

  4. 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)

  5. Determination of arsenic and cadmium in shellfish samples by graphite furnace atomic absorption spectrometry using matrix modifier

    International Nuclear Information System (INIS)

    Cortez Diaz, Mirella del Carmen

    2002-01-01

    Heavy metals are a big source of environmental contamination and are also highly toxic to humans. Since shellfish are bio-accumulators of these metals, proper techniques for quantifying them should be available. This work aims to develop an analytical method for the quantitative determination of heavy metals in biological materials (shellfish), specifically arsenic and cadmium at the trace level, using graphite furnace atomic absorption spectrometry, for which nickel and phosphate solutions were used to modify the modifiers. Prior to the analysis, the sample was diluted with nitric acid in a DAB II pressure digestion system order to destroy the organic matter. The instrument conditions were initially set (wavelength, slit, integration peaks, graphite tube, etc.), then the work range was defined for each element and the most appropriate operational parameters were studied, such as: temperature, ramp times, hold times and internal gas flow, in the different stage of the electrothermal treatment (drying, calcination, atomization) for the furnace program. Once the above mentioned conditions were set and since this was a biological sample, a matrix chemical modifier had to be used, in order to make the elements that accompany the element being studied more volatile. In this way the chemical and spectral interferences decrease together with the high background absorption of the matrix. Therefore, different matrix modifiers were studied for the definition of each analyte. The method validation was done using Certified Oyster Tissue Reference Material N o 1566a from the National Institute of Standards and Technology applying different tests in order to eliminate outliers. Repeatability, uncertainty, sensitivity, lineal range, working range, detection limit and quantification limit were evaluated for each element, and the results were compared with the values for the certified material. The Fisher and Student tests were the statistical tools used. The experimental values

  6. Photon spectrometry for the determination of the dose-rate constant of low-energy photon-emitting brachytherapy sources

    International Nuclear Information System (INIS)

    Chen, Zhe Jay; Nath, Ravinder

    2007-01-01

    Accurate determination of dose-rate constant (Λ) for interstitial brachytherapy sources emitting low-energy photons (<50 keV) has remained a challenge in radiation dosimetry because of the lack of a suitable absolute dosimeter for accurate measurement of the dose rates near these sources. Indeed, a consensus value of Λ taken as the arithmetic mean of the dose-rate constants determined by different research groups and dosimetry techniques has to be used at present for each source model in order to minimize the uncertainties associated with individual determinations of Λ. Because the dosimetric properties of a source are fundamentally determined by the characteristics of the photons emitted by the source, a new technique based on photon spectrometry was developed in this work for the determination of dose-rate constant. The photon spectrometry technique utilized a high-resolution gamma-ray spectrometer to measure source-specific photon characteristics emitted by the low-energy sources and determine their dose-rate constants based on the measured photon-energy spectra and known dose-deposition properties of mono-energetic photons in water. This technique eliminates many of the difficulties arising from detector size, the energy dependence of detector sensitivity, and the use of non-water-equivalent solid phantoms in absolute dose rate measurements. It also circumvents the uncertainties that might be associated with the source modeling in Monte Carlo simulation techniques. It was shown that the estimated overall uncertainty of the photon spectrometry technique was less than 4%, which is significantly smaller than the reported 8-10% uncertainty associated with the current thermo-luminescent dosimetry technique. In addition, the photon spectrometry technique was found to be stable and quick in Λ determination after initial setup and calibration. A dose-rate constant can be determined in less than two hours for each source. These features make it ideal to determine

  7. A novel liquid chromatography/mass spectrometry method for determination of neurotransmitters in brain tissue: Application to human tauopathies.

    Science.gov (United States)

    Forgacsova, Andrea; Galba, Jaroslav; Garruto, Ralph M; Majerova, Petra; Katina, Stanislav; Kovac, Andrej

    2018-01-15

    Neurotransmitters, small molecules widely distributed in the central nervous system are essential in transmitting electrical signals across neurons via chemical communication. Dysregulation of these chemical signaling molecules is linked to numerous neurological diseases including tauopathies. In this study, a precise and reliable liquid chromatography method was established with tandem mass spectrometry detection for the simultaneous determination of aspartic acid, asparagine, glutamic acid, glutamine, γ-aminobutyric acid, N-acetyl-l-aspartic acid, pyroglutamic acid, acetylcholine and choline in human brain tissue. The method was successfully applied to the analysis of human brain tissues from three different tauopathies; corticobasal degeneration, progressive supranuclear palsy and parkinsonism-dementia complex of Guam. Neurotransmitters were analyzed on ultra-high performance chromatography (UHPLC) using an ethylene bridged hybrid amide column coupled with tandem mass spectrometry (MS/MS). Identification and quantification of neurotransmitters was carried out by ESI+ mass spectrometry detection. We optimized sample preparation to achieve simple and fast extraction of all nine analytes. Our method exhibited an excellent linearity for all analytes (all coefficients of determination >0.99), with inter-day and intra-day precision yielding relative standard deviations 3.2%-11.2% and an accuracy was in range of 92.6%-104.3%. The present study, using the above method, is the first to demonstrate significant alterations of brain neurotransmitters caused by pathological processes in the brain tissues of patient with three different tauopathies. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. [Simultaneous determination of 16 flavonoids in the ginkgo dietary supplement tea by high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Jiang, Yalan; Huang, Fang; Wu, Fuhai; Wu, Huiqin; Huang, Xiaolan; Deng, Xin

    2015-10-01

    A method for the determination of 16 functional components of ginkgo dietary supplement tea such as catechin, vitexin, puerarin, isoflavoues aglycone, silymarin, quercetin, luteolin, apigenin, naringenin, hesperitin dihydrochalcone, kaempferol, hesperitin, isorhamnetin, baicalein, nobiletin and tangeretin by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was proposed. The conditions of chromatography and mass spectrometry were optimized. The 16 flavonoids were separated on a C18 chromatographic column with acetonitrile and water (additional 0.1% formic acid) as mobile phases under gradient elution at a flow rate of 0.25 mL/min. The determination was conducted by tandem mass spectrometry in positive ESI mode under multiple reaction monitoring (MRM) mode. Good linearities for all the compounds, with correlation coefficients over 0.996, were acquired. The recoveries were in the range of 70.9% to 100.0% (n = 6), while the relative standard deviations (RSDs) were less than 10%. The results showed that the nine flavonoids, which were kaempferol, quercetin, hesperitin, vitexin, luteolin, catechin, apigenin, naringenin and isorhamnetin, were higher in contents among the 16 flavonoids in real samples, and they constituted up to 99.6% of the total flavonoids. The contents of these nine flavonoids can be considered as the quality control index of the ginkgo dietary supplement tea. The method proved to be rapid, selective, sensitive and stable, and it can be applied to control the quality of the ginkgo dietary supplement tea.

  9. Determination of silver in fresh water by atomic absorption spectrometry following flotation preconcentration by iron(III) collectors

    Energy Technology Data Exchange (ETDEWEB)

    Cundeva, K.; Stafilov, T. [Institute of Chemistry, Faculty of Science, St. Cyril and Methodius University, Skopje (Yugoslavia)

    1997-08-01

    Colloid precipitate flotation of silver from fresh water is applied for preconcentration and separation. Optimal conditions using hydrated iron(III) oxide and iron(III) tetramethylenedithiocarbamate as collectors were investigated. Various factors affecting the silver recovery, including collector mass, nature of the supporting electrolyte, pH of the working medium, electrokinetic potential of the collector particle surfaces, type of surfactant, induction time etc., were checked. Within the optimal pH range (5.5-6.5) silver was separated quantitatively (94.9- 100.0%) with 30 mg Fe(III) as collector. The content of silver was determined by electrothermal atomic absorption spectrometry and compared to that from inductively coupled plasma-atomic emission spectrometry. The detection limit of silver by the method described is 0.01 {mu}g/L. (orig.) With 2 figs., 3 tabs.

  10. Determination of Endocrine Disrupting Compounds in surface waters by means of chromatographic techniques coupled to mass spectrometry

    Directory of Open Access Journals (Sweden)

    M. Di Carro

    2011-01-01

    Full Text Available Two analytical methods were developed to study five endocrine disrupting compounds (4-n-nonylphenol, bisphenol A, estrone, 17β-estradiol and 17α-ethinylestradiol in waters. One method includes a fast liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS-MS analysis, while the second comprise a Stir Bar Sorptive Extraction (SBSE followed by a headspace derivatization and gaschromatography-mass spectrometry (GC-MS analysis. Passive samplers POCIS (Polar Organic Chemical Integrative Samplers were used as sampling and preconcentration steps in order to reach the very low levels of the analytes in environmental waters. Both methods were then applied to the determination of the analytes in different water samples.

  11. Comparison of direct alpha spectrometry and neutron activation analysis of aerosol filters for determination of workplace thorium air concentrations

    Energy Technology Data Exchange (ETDEWEB)

    Hoetzl, H.; Winkler, R. [Institut fuer Strahlenschutz, Oberschleibheim (Germany); Riedmann, W.; Weinmueller, K. [Strahlenschutz und Isotopentechnik, Muenchen (Germany)

    1996-05-01

    Direct alpha spectrometry with three different filter types was investigated for the determination of thorium air concentrations at workplaces in the manufacturing process of discharge lamps containing thoriated tungsten electrodes. The method was compared with neutron activation analysis over an activity range of five orders of magnitude. Within the experimental limits of error, both methods were found to be comparable with respect to sensitivity and accuracy. The advantage of direct alpha spectrometry, however, is that it is less laborious than neutron activation analysis and that it supplies information on the degree of radioactive equilibrium of the thorium series, which is important with regard to the estimation of dose. 20 refs., 2 figs., 1 tab.

  12. Determination of rare earth elements in seawater by inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Moeller, P.; Dulski, P.; Luck, J.

    1992-01-01

    Shortly after sampling, rare earth elements (REEs) from 11.5 l of seawater were concentrated in 35 ml solutions by ion exchange chromatography on board the German research vessel ''Sonne'' using Chelex 100 chelating resin for preconcentration. Two millilitres of a 0.2 μg g -1 Lu spike was added to the seawater samples (i) for monitoring the chemical yield which was always found to vary between 85 and 112% (mean: 100±6) and (ii) as an internal standard. Rare earth elements have been determined by ICP-MS, with REE concentrations ranging from 100 (La) to 1 (Eu) pmol kg -1 . La in blanks can be as high as 30 pmol kg -1 , but blank concentrations for other REEs range between 0.5 and 0.01 pmol kg -1 . The trend of the precision of relative response factors varies between 12% (La) and 4% (Yb). The accuracy is estimated to be about 10% with the exception of La and Ce. Methodology improvements are suggested. (author)

  13. Determination of Fe in blood using portable X-ray fluorescence spectrometry: an alternative for sports medicine

    International Nuclear Information System (INIS)

    Zamboni, C.B.; Metairon, S.; Kovacs, L.; Macedo, D.V.; Rizzutto, M.A.

    2016-01-01

    An alternate methodology based on a portable X-ray fluorescence spectrometry (PXRFS) for determination of Fe in blood was evaluated. The iron concentrations was determined in whole blood of 18 male amateur athletes (runners) using this portable XRF spectrometer and compared with a control group (54 male donors at the same age but not involved with physical activities) obtained by XRF and NAA techniques. The Fe concentration in the blood of runners is an important factor in sports medicine contributing to the performance of endurance athletes as well as for proposing new protocols of clinical evaluation. (author)

  14. Determination of salbutamol and salbutamol glucuronide in human urine by means of liquid chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Mareck, Ute; Guddat, Sven; Schwenke, Anne

    2012-01-01

    The determination of salbutamol and its glucuronide in human urine following the inhalative and oral administration of therapeutic doses of salbutamol preparations was performed by means of direct urine injection utilizing liquid chromatography-tandem mass spectrometry (LC-MS/MS) and employing d(3...... glucuronide values between 8 and 15 ng/ml. The approach enabled the rapid determination of salbutamol and its glucuronic acid conjugate in human urine and represents an alternative to existing procedures since time-consuming hydrolysis or derivatization steps were omitted. Moreover, the excretion...

  15. 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

  16. A sequential extraction procedure to determine Ra and U isotopes by alpha-particle spectrometry in selective leachates

    International Nuclear Information System (INIS)

    Aguado, J.L.; Bolivar, J.P.; San-Miguel, E.G.; Garcia-Tenorio, R.

    2003-01-01

    A radiochemical sequential extraction procedure has been developed in our laboratory to determine 226 Ra and 234,238 U by alpha spectrometry in environmental samples. This method has been validated for both radionuclides by comparing in selected samples the values obtained through its application with the results obtained by applying alternative procedures. Recoveries obtained, counting periods applied and background levels found in the alpha spectra give suitable detection limits to allow the Ra and U determination in operational forms defined in riverbed contaminated sediments. Results obtained in these speciation studies show that 226 Ra and 234,238 U contamination tend to be associated to precipitated forms of the sediments. (author)

  17. Sensitivity of DF-ICP-MS, PERALS and alpha-spectrometry for the determination of actinides. A comparison

    International Nuclear Information System (INIS)

    Ayranov, M.; Kraehenbuehl, U.

    2009-01-01

    We applied three techniques (DF-ICP-MS, PERALS and alpha-spectrometry) for the determination of minor actinides at environmental levels. For each method the limit of detection and the resolution were estimated in order to study the content and isotopic composition of the actinides. Two international reference materials, IAEA-135 (Irish Sea Sediment) and IAEA-300 (Baltic Sea sediment) were analyzed for activity concentrations of 238 Pu, 239 Pu, 240 Pu, 241 Pu and 241 Am. The sensitivities of the three determination techniques were compared. (author)

  18. 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.

  19. Determination of gold in copper-bearing sulphide ores and metallurgical flotation products by atomic-absorption spectrometry.

    Science.gov (United States)

    Strong, B; Murray-Smith, R

    1974-12-01

    A method is described which is specific for the determination of gold in sulphide copper ores and concentrates. Direct decomposition with aqua regia was found to be incomplete. A carefully controlled roasting stage followed by treatment with hydrochloric acid and then aqua regia was effective for dissolving all the gold. The gold is extracted into 4-methylpentan-2-one (methyli-sobutylketone) then aspirated into a very lean air-acetylene flame and the gold determined by atomic-absorption spectrometry. No interferences were observed from large concentrations of copper, iron or nickel.

  20. Selective separation, preconcentration and determination of Pd(II ions in environmental samples by coprecipitation with a 1,2,4-triazole derivative

    Directory of Open Access Journals (Sweden)

    D. Ozdes

    2015-01-01

    Full Text Available A simple, sensitive, facile and low cost methodology, combined with flame atomic absorption spectrometry (FAAS, was employed to evaluate the selective separation and preconcentration of Pd(II ions in environmental samples by using a triazole derivative as an organic coprecipitating agent without a carrier element. The developed method was systematically investigated in different set of experimental parameters that influence the quantitative recovery of Pd(II ions. The accuracy of the method was tested by analyzing certified reference material and spike tests. The developed coprecipitation procedure has been applied to road dust, anodic slime, industrial electronic waste materials and water samples to determine their Pd(II levels. DOI: http://dx.doi.org/10.4314/bcse.v29i1.1

  1. Combination of flame atomic absorption spectrometry with ligandless-dispersive liquid- liquid microextraction for preconcentration and determination of trace amount of lead in water samples

    Directory of Open Access Journals (Sweden)

    Y.M. Baghelani

    2013-05-01

    Full Text Available A new ligandless-dispersive liquid–liquid microextraction method has been developed for the separation and flame atomic absorption spectrometry determination of trace amount of lead(II ion. In the proposed approach 1,2-dicholorobenzene and ethanol were used as extraction and dispersive solvents. Factors influencing the extraction efficiency of lead, including the extraction and dispersive solvent type and volume, pH of sample solution, concentration of chloride and extraction time were studied. Under the optimal conditions, the calibration curve was linear in the range of 7.0–6000 ng mL−1 of lead with R2 = 0.9992 (n = 10 and detection limit based on three times the standard deviation of the blank (3Sb was 0.5 ng mL−1 in original solution. The relative standard deviation for eight replicate determinations of 1.0 mg mL-1 lead was ±1.6%. The high efficiency of dispersive liquid-liquid microextraction to carry out the determination of trace amounts of lead in complex matrices was demonstrated. The proposed method has been applied for determination of trace amounts of lead in water samples and satisfactory results were obtained. The accuracy was checked by analyzing a certified reference material from the National Institute of Standard and Technology, Trace elements in water (NIST CRM 1643e.

  2. Determining the Amount of Copper(II) Ions in a Solution Using a Smartphone

    Science.gov (United States)

    Montangero, Marc

    2015-01-01

    When dissolving copper in nitric acid, copper(II) ions produce a blue-colored solution. It is possible to determine the concentration of copper(II) ions, focusing on the hue of the color, using a smartphone camera. A free app can be used to measure the hue of the solution, and with the help of standard copper(II) solutions, one can graph a…

  3. Determination of "1"3"5Cs by accelerator mass spectrometry

    International Nuclear Information System (INIS)

    MacDonald, C.M.; Charles, C.R.J.; Zhao, X.-L.; Kieser, W.E.; Cornett, R.J.; Litherland, A.E.

    2015-01-01

    The ratio of anthropogenic "1"3"5Cs and "1"3"7Cs isotopes is characteristic of a uranium fission source. This research evaluates the technique of isotope dilution (yield tracing) for the purpose of quantifying "1"3"5Cs by accelerator mass spectrometry with on-line isobar separation. Interferences from Ba, Zn_2, and isotopes of equal mass to charge ratios were successfully suppressed. However, some sample crosstalk from source contamination remains. The transmission and di-fluoride ionization efficiencies of Cs isotopes were found to be 8 × 10"−"3 and 1.7 × 10"−"7 respectively. This quantification of "1"3"5Cs using yield tracing by accelerator mass spectrometry shows promise for future environmental sample analysis once the issues of sample crosstalk and low efficiency can be resolved.

  4. Determination of hydroxylated polycyclic aromatic hydrocarbons by HPLC-photoionization tandem mass spectrometry in wood smoke particles and soil samples.

    Science.gov (United States)

    Avagyan, Rozanna; Nyström, Robin; Boman, Christoffer; Westerholm, Roger

    2015-06-01

    A simple and fast method for analysis of hydroxylated polycyclic aromatic hydrocarbons using pressurized liquid extraction and high performance liquid chromatography utilizing photoionization tandem mass spectrometry was developed. Simultaneous separation and determination of nine hydroxylated polycyclic aromatic hydrocarbons and two hydroxy biphenyls could be performed in negative mode with a run time of 12 min, including equilibration in 5 min. The calibration curves were in two concentration ranges; 1-50 ng/mL and 0.01-50 μg/mL, with coefficients of correlation R (2) > 0.997. The limits of detection and method quantification limits were in the range of 9-56 pg and 5-38 ng/g, respectively. A two-level full factorial experimental design was used for screening of conditions with the highest impact on the extraction. The extraction procedure was automated and suitable for a large number of samples. The extraction recoveries ranged from 70 to 102 % and the matrix effects were between 92 and 104 %. The overall method was demonstrated on wood smoke particles and soil samples with good analytical performance, and five OH-PAHs were determined in the concentration range of 0.19-210 μg/g. As far as we know, hydroxylated polycyclic aromatic hydrocarbons were determined in wood smoke and soil samples using photoionization mass spectrometry for the first time in this present study. Accordingly, this study shows that high performance liquid chromatography photoionization tandem mass spectrometry can be a good option for the determination of hydroxylated polycyclic aromatic hydrocarbons in complex environmental samples. Graphical Abstract The method developed in this study was used to determine hydroxylated polycyclic aromatic hydrocarbons in wood smoke and soil.

  5. Uranium Enrichment Determination of the InSTEC Sub Critical Ensemble Fuel by Gamma Spectrometry

    International Nuclear Information System (INIS)

    Borrell Munnoz, Jose L.; LopezPino, Neivy; Diaz Rizo, Oscar; D'Alessandro Rodriguez, Katia; Padilla Cabal, Fatima; Arbelo Penna, Yunieski; Garcia Rios, Aczel R.; Quintas Munn, Ernesto L.; Casanova Diaz, Amaya O.

    2009-01-01

    Low background gamma spectrometry was applied to analyze the uranium enrichment of the nuclear fuel used in the InSTEC Sub Critical ensemble. The enrichment was calculated by two variants: an absolute method using the Monte Carlo method to simulated detector volumetric efficiency, and an iterative procedure without using standard sources. The results confirm that the nuclear fuel of the ensemble is natural uranium without any additional degree of enrichment. (author)

  6. Comparison of in-situ gamma ray spectrometry measurements with conventional methods in determination natural and artificial nuclides in soil

    International Nuclear Information System (INIS)

    Al-Masri, M. S.; Doubal, A. W.

    2010-12-01

    Two nuclear analytical techniques (In-Situ Gamma ray spectrometry and laboratory gamma ray spectrometry) for determination of natural and artificial radionuclides in soil have been validated. The first technique depends on determination of radioactivity content of representative samples of the studied soil after laboratory preparation, while the second technique is based on direct determination of radioactivity content of soil using in-situ gamma-ray spectrometer. Analytical validation parameter such as detection limits, repeatability, reproducibility in addition to measurement uncertainties were estimated and compared for both techniques. Comparison results have shown that the determination of radioactivity in soil should apply the two techniques together where each of techniques is characterized by its low detection limit and uncertainty suitable for defined application of measurement. Radioactive isotopes in various locations were determined using the two methods by measuring 40 k, 238 U,and 137 Cs. The results showed that there are differences in attenuation factors due to soil moisture content differences; wet weight corrections should be applied when the two techniques are compared. (author)

  7. [Evaluation of uncertainty for determination of tin and its compounds in air of workplace by flame atomic absorption spectrometry].

    Science.gov (United States)

    Wei, Qiuning; Wei, Yuan; Liu, Fangfang; Ding, Yalei

    2015-10-01

    To investigate the method for uncertainty evaluation of determination of tin and its compounds in the air of workplace by flame atomic absorption spectrometry. The national occupational health standards, GBZ/T160.28-2004 and JJF1059-1999, were used to build a mathematical model of determination of tin and its compounds in the air of workplace and to calculate the components of uncertainty. In determination of tin and its compounds in the air of workplace using flame atomic absorption spectrometry, the uncertainty for the concentration of the standard solution, atomic absorption spectrophotometer, sample digestion, parallel determination, least square fitting of the calibration curve, and sample collection was 0.436%, 0.13%, 1.07%, 1.65%, 3.05%, and 2.89%, respectively. The combined uncertainty was 9.3%.The concentration of tin in the test sample was 0.132 mg/m³, and the expanded uncertainty for the measurement was 0.012 mg/m³ (K=2). The dominant uncertainty for determination of tin and its compounds in the air of workplace comes from least squares fitting of the calibration curve and sample collection. Quality control should be improved in the process of calibration curve fitting and sample collection.

  8. Preconcentration, speciation and determination of ultra trace amounts of mercury by modified octadecyl silica membrane disk/electron beam irradiation and cold vapor atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ashkenani, Hamid [Department of Chemistry, Yazd University, Yazd (Iran, Islamic Republic of); Dadfarnia, Shayessteh [Department of Chemistry, Yazd University, Yazd (Iran, Islamic Republic of)], E-mail: sdadfarnia@yazduni.ac.ir; Shabani, Ali Mohammad Haji; Jaffari, Abbas Ali [Department of Chemistry, Yazd University, Yazd (Iran, Islamic Republic of); Behjat, Abbas [Department of physics, Yazd University, Yazd (Iran, Islamic Republic of)

    2009-01-15

    Mercury (II) and methyl mercury cations at the Sub-ppb level were adsorbed quantitatively from aqueous solution onto an octadecyl-bonded silica membrane disk modified by 2-[(2-mercaptophyenylimino)methyl] phenol (MPMP). The trapped mercury was then eluted with 3 ml ethanol and Hg{sup 2+} ion was directly measured by cold vapor atomic absorption spectrometry, utilizing tin (II) chloride. Total mercury (Hgt) was determined after conversion of MeHg{sup +} into Hg{sup 2+} ion by electron beam irradiation. A sample volume of 1500 ml resulted in a preconcentration factor of 500 and the precision for a sampling volume of 500 ml at a concentration of 2.5 {mu}g l{sup -1} (n = 7) was 3.1%. The limit of detection of the proposed method is 3.8 ng l{sup -1}. The method was successfully applied to analysis of water samples, and the accuracy was assessed via recovery experiment.

  9. Photoassisted vapor generation in the presence of organic acids for ultrasensitive determination of Se by electrothermal-atomic absorption spectrometry following headspace single-drop microextraction

    International Nuclear Information System (INIS)

    Figueroa, Raul; Garcia, Monica; Lavilla, Isela; Bendicho, Carlos

    2005-01-01

    A method is described for the determination of selenium at the pg/mL level by electrothermal-atomic absorption spectrometry using in situ photogeneration of Se vapors, headspace sequestration onto an aqueous microdrop containing Pd(II) and subsequent injection in a graphite tube. Several organic acids (formic, oxalic, acetic, citric and ethylenediaminetetraacetic) have been tried for photoreduction of Se(IV) into volatile Se compounds under UV irradiation. Experimental variables such as UV irradiation time, organic acid concentration, Pd(II) concentration in the drop, sample and drop volumes, extraction time and pH were fully optimized. Low-molecular weight acids such as formic and acetic provided optimal photogeneration of volatile Se species at a 0.6 mol/L concentration. Citric and ethylenediaminetetraacetic acid allowed to use a concentration as low as 1 mmol/L, but extraction times were longer than for formic and acetic acids. Photogeneration of (CH 3 ) 2 Se from Se(IV) in the presence of acetic acid provided a detection limit of 20 pg/mL, a preconcentration factor of nearly 285 and a precision, expressed as relative standard deviation, of 4%. Analytical performance seemed to depend not only on the photogeneration efficiency obtained with each acid but also on the stability of the vapors in the headspace. The method showed a high freedom from interferences caused by saline matrices, but interferences were observed for transition metals at a relatively low concentration

  10. Towards automated diffraction tomography. Part II-Cell parameter determination

    International Nuclear Information System (INIS)

    Kolb, U.; Gorelik, T.; Otten, M.T.

    2008-01-01

    Automated diffraction tomography (ADT) allows the collection of three-dimensional (3d) diffraction data sets from crystals down to a size of only few nanometres. Imaging is done in STEM mode, and diffraction data are collected with quasi-parallel beam nanoelectron diffraction (NED). Here, we present a set of developed processing steps necessary for automatic unit-cell parameter determination from the collected 3d diffraction data. Cell parameter determination is done via extraction of peak positions from a recorded data set (called the data reduction path) followed by subsequent cluster analysis of difference vectors. The procedure of lattice parameter determination is presented in detail for a beam-sensitive organic material. Independently, we demonstrate a potential (called the full integration path) based on 3d reconstruction of the reciprocal space visualising special structural features of materials such as partial disorder. Furthermore, we describe new features implemented into the acquisition part

  11. Applicability of cloud point extraction for the separation trace amount of lead ion in environmental and biological samples prior to determination by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Sayed Zia Mohammadi

    2016-09-01

    Full Text Available A sensitive cloud point extraction procedure(CPE for the preconcentration of trace lead prior to its determination by flame atomic absorption spectrometry (FAAS has been developed. The CPE method is based on the complex of Pb(II ion with 1-(2-pyridylazo-2-naphthol (PAN, and then entrapped in the non-ionic surfactant Triton X-114. The main factors affecting CPE efficiency, such as pH of sample solution, concentration of PAN and Triton X-114, equilibration temperature and time, were investigated in detail. A preconcentration factor of 30 was obtained for the preconcentration of Pb(II ion with 15.0 mL solution. Under the optimal conditions, the calibration curve was linear in the range of 7.5 ng mL−1–3.5 μg mL−1 of lead with R2 = 0.9998 (n = 10. Detection limit based on three times the standard deviation of the blank (3Sb was 5.27 ng mL−1. Eight replicate determinations of 1.0 μg mL−1 lead gave a mean absorbance of 0.275 with a relative standard deviation of 1.6%. The high efficiency of cloud point extraction to carry out the determination of analytes in complex matrices was demonstrated. The proposed method has been applied for determination of trace amounts of lead in biological and water samples with satisfactory results.

  12. Application of cotton as a solid phase extraction sorbent for on-line preconcentration of copper in water samples prior to inductively coupled plasma optical emission spectrometry determination.

    Science.gov (United States)

    Faraji, Mohammad; Yamini, Yadollah; Shariati, Shahab

    2009-07-30

    Copper, as a heavy metal, is toxic for many biological systems. Thus, the determination of trace amounts of copper in environmental samples is of great importance. In the present work, a new method was developed for the determination of trace amounts of copper in water samples. The method is based on the formation of ternary Cu(II)-CAS-CTAB ion-pair and adsorption of it into a mini-column packed with cotton prior applying inductively coupled plasma optical emission spectrometry (ICP-OES). The experimental parameters that affected the extraction efficiency of the method such as pH, flow rate and volume of the sample solution, concentration of chromazurol S (CAS) and cethyltrimethylammonium bromide (CTAB) as well as type and concentration of eluent were investigated and optimized. The ion-pair (Cu(II)-CAS-CTAB) was quantitatively retained on the cotton under the optimum conditions, then eluted completely using a solution of 25% (v/v) 1-propanol in 0.5 mol L(-1) HNO(3) and directly introduced into the nebulizer of the ICP-OES. The detection limit (DL) of the method for copper was 40 ng L(-1) (V(sample)=100mL) and the relative standard deviation (R.S.D.) for the determination of copper at 10 microg L(-1) level was found to be 1.3%. The method was successfully applied to determine the trace amounts of copper in tap water, deep well water, seawater and two different mineral waters, and suitable recoveries were obtained (92-106%).

  13. Proceedings of the relevance of mass spectrometry to DNA sequence determination: Research needs for the Human Genome Program

    Energy Technology Data Exchange (ETDEWEB)

    Edmonds, C.G.; Smith, R.D. (Pacific Northwest Lab., Richland, WA (USA)); Smith, L.M. (Wisconsin Univ., Madison, WI (USA))

    1990-11-01

    A workshop was sponsored for the US Department of Energy (DOE), Office of Health and Environmental Research by Pacific Northwest Laboratory, April 4--5, 1990, in Seattle, Washington, to examine the potential role of mass spectrometry in the joint DOE/National Institutes of Health (NIH) Human Genome Program. The workshop was occasioned by recent developments in mass spectrometry that are providing new levels for selectivity, sensitivity, and, in particular, new methods of ionization appropriate for large biopolymers such as DNA. During discussions, three general mass spectrometric approaches to the determination of DNA sequence were considered: (1) the mass spectrometric detection of isotopic labels from DNA sequencing mixtures separated using gel electrophoresis, (2) the direct mass spectrometric analysis from direct ionization of unfractionated sequencing mixtures where the measured mass of the constituents functions to identify and order the base sequence (replacing separation by gel electrophoresis), and (3) an approach in which a single highly charged molecular ion of a large DNA segment produced is rapidly sequenced in an ion cyclotron resonance ion trap. The consensus of the workshop was that, on the basis of the new developments, mass spectrometry has the potential to provide the substantial increases in sequencing speed required for the Human Genome Program. 66 refs., 3 tabs.

  14. Accurate determination of 41Ca concentrations in spent resins from the nuclear industry by Accelerator Mass Spectrometry

    International Nuclear Information System (INIS)

    Nottoli, Emmanuelle; Bourlès, Didier; Bienvenu, Philippe; Labet, Alexandre; Arnold, Maurice; Bertaux, Maité

    2013-01-01

    The radiological characterisation of nuclear waste is essential for managing storage sites. Determining the concentration of Long‐Lived RadioNuclides (LLRN) is fundamental for their long-term management. This paper focuses on the measurement of low 41 Ca concentrations in ions exchange resins used for primary fluid purification in Pressurised Water Reactors (PWR). 41 Ca concentrations were successfully measured by Accelerator Mass Spectrometry (AMS) after the acid digestion of resin samples, followed by radioactive decontamination and isobaric suppression through successive hydroxide, carbonate, nitrate and final CaF 2 precipitations. Measured 41 Ca concentrations ranged from 0.02 to 0.03 ng/g, i.e. from 0.06 to 0.09 Bq/g. The 41 Ca/ 60 Co activity ratios obtained were remarkably reproducible and in good agreement with the current ratio used for resins management. - Highlights: • In the context of radioactive waste management, this study aimed at measuring 41 Ca in spent resins using Accelerator Mass Spectrometry. • A chemical treatment procedure was developed to quantitatively recover calcium in solution and selectively extract it. • Developed firstly on synthetic matrices, the chemical treatment procedure was then successfully applied to real resin samples. • Accelerator mass spectrometry allowed measuring concentrations of 41 Ca in spent resins as low as 0.02 ng/g of dry resin. • Final results are in agreement with current data used for spent resins management

  15. Burn-up determination of irradiated uranium oxide by means of direct gama spectrometry and by radiochemical method

    International Nuclear Information System (INIS)

    Cunha, I.I.L.; Nastasi, M.J.C.; Lima, F.W.

    1981-09-01

    The burn-up of thermal neutrons irradiated U 3 O 8 (natural uranium) samples has been determined by using both direct gamma spectrometry and radiochemical methods and the results obtained were compared. The fission products 144 Ce, 103 Ru, 106 Ru, 137 Cs and 95 Zr were chosen as burn-up monitors. In order to isolate the radioisotopes chosen as monitors, a radiochemical separation procedure has been established, in which the solvent extraction technique was used to separate cerium, cesium and ruthenium one from the other and all of them from uranium. The separation between zirconium and niobium and of both elements from the other radioisotopes and uranium was accomplished by means of adsorption on a silica-gel column, followed by selective elution of zirconium and of niobium. When use was made of the direct gamma-ray spectrometry method, the radioactivity of each nuclide of interest was measured in presence of all others. For this purpose use was made of gamma-ray spectrometry and of a Ge-Li detector. Comparison of burn-up values obtained by both methods was made by means of Student's 't' test, and this showed that results obtained in each case are statistically equal. (Author) [pt

  16. Determination of 4-Methylimidazole in Ammonia Caramel Using Gas Chromatography–Tandem Mass Spectrometry (GC-MS/MS

    Directory of Open Access Journals (Sweden)

    Martyna N. Wieczorek

    2018-01-01

    Full Text Available One of Maillard reaction products formed in the production of ammonia caramel is 4(5-methylimidazole (4-MeI classified as carcinogen. A method of 4-MeI determination based on ion-pair extraction and derivatisation with isobutyl chloroformate with subsequent gas chromatography-tandem mass spectrometry analysis was proposed. Tandem mass spectrometry was applied to reduce the influence of matrix and increase the selectivity and sensitivity of the method. Triple quadrupole GC-MS system was used for this study. The collision energies were optimized for MRM mode. The detection (LOD and quantification limits (LOQ of the elaborated method were 17 and 37.8 μg kg−1, respectively, repeatability was <15% RSD for analyzed caramel samples, and the recovery for 4-MeI was 101%. Comparison of MS/MS with SIM detection on the same instrument proved almost 30 times lower LODs achieved by tandem mass spectrometry compared to SIM. Described method can be routinely used for monitoring 4-MeI as a quality and safety marker in the production of ammonia caramel.

  17. Quantitative determination of total cesium in highly active liquid waste by using liquid electrode plasma optical emission spectrometry.

    Science.gov (United States)

    Do, Van-Khoai; Yamamoto, Masahiko; Taguchi, Shigeo; Takamura, Yuzuru; Surugaya, Naoki; Kuno, Takehiko

    2018-06-01

    A sensitive analytical method for determination of total cesium (Cs) in highly active liquid waste (HALW) by using modified liquid electrode plasma optical emission spectrometry (LEP-OES) is developed in this study. The instrument is modified to measure radioactive samples in a glove box. The effects of important factors, including pulsed voltage sequence and nitric acid concentration, on the emission of Cs are investigated. The limit of detection (LOD) and limit of quantification (LOQ) are 0.005 mg/L and 0.02 mg/L, respectively. The achieved LOD is one order lower than that of recently developed spectroscopic methods using liquid discharge plasma. The developed method is validated by subjecting a simulated HALW sample to inductively coupled plasma mass spectrometry (ICP-MS). The recoveries obtained from a spike-and-recovery test are 96-102%, implying good accuracy. The method is successfully applied to the quantification of Cs in a real HALW sample at the Tokai reprocessing plant in Japan. Apart from dilution and filtration of the HALW sample, no other pre-treatment process is required. The results agree well with the values obtained using gamma spectrometry. The developed method offers a reliable technique for rapid analysis of total Cs in HALW samples. Copyright © 2018 Elsevier B.V. All rights reserved.

  18. Ligandless surfactant mediated solid phase extraction combined with Fe₃O₄ nano-particle for the preconcentration and determination of cadmium and lead in water and soil samples followed by flame atomic absorption spectrometry: multivariate strategy.

    Science.gov (United States)

    Jalbani, N; Soylak, M

    2014-04-01

    In the present study, a microextraction technique combining Fe3O4 nano-particle with surfactant mediated solid phase extraction ((SM-SPE)) was successfully developed for the preconcentration/separation of Cd(II) and Pb(II) in water and soil samples. The analytes were determined by flame atomic absorption spectrometry (FAAS). The effective variables such as the amount of adsorbent (NPs), the pH, concentration of non-ionic (TX-114) and centrifugation time (min) were investigated by Plackett-Burman (PBD) design. The important variables were further optimized by central composite design (CCD). Under the optimized conditions, the detection limits (LODs) of Cd(II) and Pb(II) were 0.15 and 0.74 µg/L, respectively. The validation of the proposed procedure was checked by the analysis of certified reference materials of TMDA 53.3 fortified water and GBW07425 soil. The method was successfully applied for the determination of Cd(II) and Pb(II) in water and soil samples. Copyright © 2014 Elsevier Inc. All rights reserved.

  19. Determination of 210Pb by direct gamma-ray spectrometry, beta counting via 210Bi and alpha-particle spectrometry via 210Po in coal, slag and ash samples from thermal power plant

    International Nuclear Information System (INIS)

    Seslak, Bojan; Vukanac, Ivana; Kandic, Aleksandar; Durasevic, Mirjana; Eric, Milic; Jevremovic, Aleksandar

    2017-01-01

    In order to compare three different techniques and estimate radiological impact, activity concentration of 210 Pb in coal, slag and ash samples from thermal power plant 'Nikola Tesla', Serbia, were measured, and results are presented in this study. Determination of 210 Pb was carried out in three ways: using HPGe gamma spectrometer and via in-growth of 210 Po and 210 Bi by alpha-particle spectrometry and proportional counting, respectively. The results obtained for three different techniques were compared. Statistical analysis and comparison of methods were carried out by combination of Z score and χ 2 statistical tests. Tests results, as well as values of measured activities concentrations obtained by alpha and gamma spectrometry, showed that gamma spectrometry is a valid alternative to time-consuming alpha spectrometry for low level activity measurements of 210 Pb. This remark is also valid even for gamma spectrometers with poor efficiency in low energy region. (author)

  20. 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%

  1. 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.

  2. On-line preconcentration system using a minicolumn of polyurethane foam loaded with Me-BTABr for zinc determination by Flame Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    Azevedo Lemos, Valfredo; Nei Lopes dos Santos, Walter; Silva Santos, Juracir; Bezerra de Carvalho, Marcilio

    2003-01-01

    In the present paper, an on-line system for preconcentration and determination of zinc by Flame Atomic Absorption Spectrometry (FAAS) is proposed. It is based in the sorption of zinc(II) ions on a minicolumn packed with polyurethane foam loaded with 2-[2'-(6-methyl-benzothiazolylazo)]-4-bromophenol (Me-BTABr) reagent. Chemical and flow variables as pH effect, sample flow rate and eluent concentration were optimized using univariate methodology. The results demonstrated that zinc can determinate using the sample pH in the range of 6.5-9.2, sample flow rate of 6.0 ml min -1 , and the elution step using 0.10 mol l -1 hydrochloric acid solution at flow rate of 5.5 ml min -1 . In these conditions, an enrichment factor of 23 and a sampling rate of 48 samples per hour were achieved. The detection limit (DL, 3σ) as IUPAC recommendation was 0.37 μg l -1 and the precision (assessed as the relative standard deviation, R.S.D.) reached values of 5.9-1.8% in zinc solutions of 1.0-10.0 μg l -1 concentration, respectively. The method was successfully applied to the determination of trace amounts of zinc in natural water samples from Salvador (Brazil)

  3. Flotation separation of Cd, Co, Cr, Cu, Ni and Tl from calcium minerals and their determination by inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    Zajkova-Paneva, Vesna; Stafilov, Trajche; Boev, Blazho

    2003-01-01

    The method of inductively coupled plasma-atomic spectrometry (ICP-AES), is developed for determination of Cd, Co, Cr, Cu, Ni and Tl in traces in calcite and gypsum. The interferences of Ca as matrix element on Co, Cr, Cu, Ni and Tl intensities during their ICP-AES determination are investigated. The results reveal that Ca does not interfere on intensities of Cr, but tends to decrease the intensity of the other elements. To eliminate those matrix interferences of Ca on trace elements intensities a flotation separation method is proposed. Lead(II) hexamethylenedithiocarbamate, Pb(HMDTC) 2 , is applied as a collector for flotation of trace elements from acidic solutions of mineral samples. The most suitable concentrations of calcite and gypsum solutions for flotation are ascertained. The detection limits of ICP-AES method following flotation of elements present in calcite and gypsum as impurities are determined: 0.022 and 0.061 μg·g -1 for Cd, 0.071 and 0.042 μg·g -1 for Co, 0.026 and 0.132 μg·g -1 for Cr, 0.164 and 0.149 μg·g -1 for Cu, 0.289 and 0.095 μg·g -1 for Ni and 0.645 and 0.7666 μg·g -1 for Tl, respectively. (Original)

  4. Optimisation and application of ICP-MS and alpha-spectrometry for determination of isotopic ratios of depleted uranium and plutonium in samples collected in Kosovo

    OpenAIRE

    Boulyga, S. F.; Testa, C.; Desideri, D.; Becker, J. S.

    2001-01-01

    The determination of environmental contamination with natural and artificial actinide isotopes and evaluation of their source requires precise isotopic determination of actinides, above all uranium and plutonium. This can be achieved by alpha spectrometry or by inductively coupled plasma mass spectrometry (ICP-MS) after chemical separation of actinides. The performance of a sector-field ICP-MS (ICP-SFMS) coupled to a low-flow micronebulizer with a membrane desolvation unit, "Aridus'', was stu...

  5. Determination of As, Cd, Cu, Hg and Pb in biological samples by modern electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Sardans, Jordi; Montes, Fernando; Penuelas, Josep

    2010-01-01

    Pollution from heavy metals has increased in recent decades and has become an important concern for environmental agencies. Arsenic, cadmium, copper, mercury and lead are among the trace elements that have the greatest impact and carry the highest risk to human health. Electrothermal atomic absorption spectrometry (ETAAS) has long been used for trace element analyses and over the past few years, the main constraints of atomic absorption spectrometry (AAS) methods, namely matrix interferences that provoked high background absorption and interferences, have been reduced. The use of new, more efficient modifiers and in situ trapping methods for stabilization and pre-concentration of these analytes, progress in control of atomization temperatures, new designs of atomizers and advances in methods to correct background spectral interferences have permitted an improvement in sensitivity, an increase in detection power, reduction in sample manipulation, and increase in the reproducibility of the results. These advances have enhanced the utility of Electrothermal atomic absorption spectrometry (ETAAS) for trace element determination at μg L -1 levels, especially in difficult matrices, giving rise to greater reproducibility, lower economic cost and ease of sample pre-treatment compared to other methods. Moreover, the recent introduction of high resolution continuum source Electrothermal atomic absorption spectrometry (HR-CS-ETAAS) has facilitated direct solid sampling, reducing background noise and opening the possibility of achieving even more rapid quantitation of some elements. The incorporation of flow injection analysis (FIA) systems for automation of sample pre-treatment, as well as chemical vapor generation renders (ETAAS) into a feasible option for detection of As and Hg in environmental and food control studies wherein large numbers of samples can be rapidly analyzed. A relatively inexpensive approach with low sample consumption provide additional advantages of

  6. Determination of As, Cd, Cu, Hg and Pb in biological samples by modern electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sardans, Jordi, E-mail: j.sardans@creaf.uab.ca [Ecophysiological and Global Change Unit CSIC-CREAF, Edifici C, Universitat Autonoma de Barcelona, Bellaterra 08193, Barcelona (Spain); Montes, Fernando [Departamento de Ciencias Analiticas, Facultad de Ciencias, Universidad Nacional de Educacion a Distancia (UNED), C/ Senda del Rey 9. 28040 Madrid (Spain); Penuelas, Josep [Ecophysiological and Global Change Unit CSIC-CREAF, Edifici C, Universitat Autonoma de Barcelona, Bellaterra 08193, Barcelona (Spain)

    2010-02-15

    Pollution from heavy metals has increased in recent decades and has become an important concern for environmental agencies. Arsenic, cadmium, copper, mercury and lead are among the trace elements that have the greatest impact and carry the highest risk to human health. Electrothermal atomic absorption spectrometry (ETAAS) has long been used for trace element analyses and over the past few years, the main constraints of atomic absorption spectrometry (AAS) methods, namely matrix interferences that provoked high background absorption and interferences, have been reduced. The use of new, more efficient modifiers and in situ trapping methods for stabilization and pre-concentration of these analytes, progress in control of atomization temperatures, new designs of atomizers and advances in methods to correct background spectral interferences have permitted an improvement in sensitivity, an increase in detection power, reduction in sample manipulation, and increase in the reproducibility of the results. These advances have enhanced the utility of Electrothermal atomic absorption spectrometry (ETAAS) for trace element determination at mug L{sup -1} levels, especially in difficult matrices, giving rise to greater reproducibility, lower economic cost and ease of sample pre-treatment compared to other methods. Moreover, the recent introduction of high resolution continuum source Electrothermal atomic absorption spectrometry (HR-CS-ETAAS) has facilitated direct solid sampling, reducing background noise and opening the possibility of achieving even more rapid quantitation of some elements. The incorporation of flow injection analysis (FIA) systems for automation of sample pre-treatment, as well as chemical vapor generation renders (ETAAS) into a feasible option for detection of As and Hg in environmental and food control studies wherein large numbers of samples can be rapidly analyzed. A relatively inexpensive approach with low sample consumption provide additional advantages

  7. Determinants of exercise among children. II. A longitudinal analysis.

    Science.gov (United States)

    DiLorenzo, T M; Stucky-Ropp, R C; Vander Wal, J S; Gotham, H J

    1998-01-01

    Research has demonstrated that physical activity serves an important preventive function against the development of cardiovascular disease. The recognition that U.S. children are often sedentary, coupled with the observation that physical activity habits tend to persist into adulthood, has prompted the investigation of exercise determinants consistent with social learning theory. The purposes of the present study were to identify social learning variables relevant to children's exercise and to explore the longitudinal predictive value of the determinants. Data were collected from 111 families (N = 54 girls, N = 57 boys) who were interviewed in both Phase 1 (fifth and sixth grades) and Phase 2 (eight and ninth grades) of this study. Data from mothers (N = 111) were collected during both phases; data from 80 fathers were collected at Phase 2 only. The results of simultaneous stepwise regression analyses indicated that child's enjoyment of physical activity was the only consistent predictor of physical activity during Phase 1. At Phase 2, child's exercise knowledge, mother's physical activity, and child's and mother's friend modeling/support emerged as predictors for girls. For boys, child's self-efficacy for physical activity, exercise knowledge, parental modeling, and interest in sports media were important. Longitudinally, mother's self-efficacy, barriers to exercise, enjoyment of physical activity, and child's self-efficacy for physical activity were important for girls. Only child's exercise knowledge predicted boys' physical activity. The addition of information from fathers nearly doubled the explanatory power of the predictors for both genders. Socialization in the family unit exerts a tremendous influence on health-related behaviors such as exercise. The relative importance of determinants seems to differ for girls and boys and the pattern of these determinants appears to change over time.

  8. Simultaneous determination of Hg(II)-Ag(I)-Cd(II) by conductometric titration using the formation of ternary complex

    International Nuclear Information System (INIS)

    Hayashida, Ichiro; Yoshida, Hitoshi; Taga, Mitsuhiko; Hikime, Seiichiro

    1979-01-01

    A conductometric determination of Hg(II), Ag(I) and Cd(II) was carried out by using the insoluble ternary complex formation of the metal ions with iodide ion in the presence of 1,10-phenanthroline (phen). Recommended procedure is as follows; An aliquot of sample solution containing (14 -- 29) mg of Hg(II), (8 -- 16) mg of Ag(I), and (9 -- 17) mg of Cd(II) transfered into a 100 ml beaker. Add to acetate buffer and stoichiometric amounts of phen (40% ethanol-water solution). Amounts of nitrate ion which was estimated separately by other titration with 0.1 M Ag(phen) 2 complex (40% ethanol-water solution) are adjusted in the range of (4.0 -- 6.0) mM. The sample solution is titrated with 0.1 M KI standard solution at the rate of 0.20 ml/min or less. The titration curve showed three end-points corresponding to the formation of (1) Hg(phen) 2 I 2 , (2) Ag(phen)I, and (3) Cd(phen) 2 I 2 . The relative standard deviation was less than 0.8%, when the pH value was controlled at 4.0 -- 4.5 (acetate buffer) and the nitrate concentration was adjusted in the range of (4.0 -- 6.0)mM. The effect of diverse ions on the determination was also investigated in detail. (author)

  9. High-sensitivity determination of Zn(II) and Cu(II) in vitro by fluorescence polarization

    Science.gov (United States)

    Thompson, Richard B.; Maliwal, Badri P.; Feliccia, Vincent; Fierke, Carol A.

    1998-04-01

    Recent work has suggested that free Cu(II) may play a role in syndromes such as Crohn's and Wilson's diseases, as well as being a pollutant toxic at low levels to shellfish and sheep. Similarly, Zn(II) has been implicated in some neural damage in the brain resulting from epilepsy and ischemia. Several high sensitivity methods exist for determining these ions in solution, including GFAAS, ICP-MS, ICP-ES, and electrochemical techniques. However, these techniques are generally slow and costly, require pretreatment of the sample, require complex instruments and skilled personnel, and are incapable of imaging at the cellular and subcellular level. To address these shortcomings we developed fluorescence polarization (anisotropy) biosensing methods for these ions which are very sensitivity, highly selective, require simple instrumentation and little pretreatment, and are inexpensive. Thus free Cu(II) or Zn(II) can be determined at picomolar levels by changes in fluorescence polarization, lifetime, or wavelength ratio using these methods; these techniques may be adapted to microscopy.

  10. Potentiometric determination of the tungsten content of tantalum-tungsten alloys with chromium II

    International Nuclear Information System (INIS)

    Gavra, Z.; Ronen, S.; Levin, R.

    1977-05-01

    A method was developed for the potentiometric determination of the tungsten content of tantalum-tungsten alloys of different compositions. These were dissolved under conditions that enabled the tungsten content to be determined with chromium (II). Phosphoric acid was selected as a suitable complexing agent for the prevention of the precipitation of tungsten and tantalum compounds. The use of chromium (II) required an oxygen-tight system and therefore the work was carried out in suitable vessels for storage and tritation

  11. On line determination of deuterium in hydrogen water exchange reaction by mass spectrometry. IRP-10

    International Nuclear Information System (INIS)

    Sharma, J.D.; Alphonse, K.P.; Mishra, Sushama; Prabhu, S.A.; Mohan, Sadhana; Tangri, V.K.

    2007-01-01

    The Deuterium (D)/Hydrogen (H) analysis at low Concentration is generally carried out by Mass Spectrometry. Mass Spectrometer is specially designed for the measurement of Mass 2 and 3 ratio. The Deuterium analysis of water and hydrogen in concentration range of a few ppm to about 1% plays an important role in the Heavy Water Production Plants. For the enrichment of the Deuterium concentration in H 2 O by H 2 - H 2 O exchange a catalyst is essential as reaction is relatively slow. Heavy Water Division has developed in house Platinum based catalyst for the isotopic exchange of Hydrogen and Water

  12. 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...

  13. A simple theoretical approach to determine relative ion yield (RIY) in glow discharge mass spectrometry (GDMS)

    Energy Technology Data Exchange (ETDEWEB)

    Born, Sabine [Degussa AG, Hanau (Germany); Matsunami, Noriaki [Nagoya Univ. (Japan). Faculty of Engineering; Tawara, Hiroyuki [National Inst. for Fusion Science, Toki, Gifu (Japan)

    2000-01-01

    Direct current glow discharge mass spectrometry (dc-GDMS) has been applied to detect impurities in metals. The aim of this study is to understand quantitatively the processes taking place in GDMS and establish a model to calculate the relative ion yield (RIY), which is inversely proportional to the relative sensitivity factor (RSF), in order to achieve better agreement between the calculated and the experimental RIYs. A comparison is made between the calculated RIY of the present model and the experimental RIY, and also with other models. (author)

  14. Determination of cocaine in brazilian paper currency by capillary gas chromatography/mass spectrometry

    Directory of Open Access Journals (Sweden)

    Enrico Di Donato

    2007-01-01

    Full Text Available The presence of illicit drugs such as cocaine and marijuana in US paper currency is very well demonstrated. However, there is no published study describing the presence of cocaine and/or other illicit drugs in Brazilian paper currency. In this study, Brazilian banknotes were collected from nine cities, extracted and analyzed by capillary gas chromatography/mass spectrometry, in order to investigate the presence of cocaine. Bills were extracted with deionized water followed by ethyl acetate. Results showed that 93% of the bills presented cocaine in a concentration range of 2.38-275.10 µg/bill.

  15. Determination of vanadium in titanate-based ferroelectrics by INAA with discriminating gamma-ray spectrometry

    Czech Academy of Sciences Publication Activity Database

    Kameník, Jan; Dragounová, K.; Kučera, Jan; Bryknar, Z.; Trepakov, Vladimír; Strunga, Vladimír

    2017-01-01

    Roč. 311, č. 2 (2017), s. 1333-1338 ISSN 0236-5731. [1st International Conference on Radioanalytical and Nuclear chemistry (RANC). Budapest, 10.04.2016-15.04.2016] R&D Projects: GA ČR(CZ) GBP108/12/G108; GA MŠk LM2015056 Institutional support: RVO:68378271 ; RVO:61389005 Keywords : Titanate-based ferroelectrics * Vanadium * INAA * discriminating gamma-ray spectrometry Subject RIV: CB - Analytical Chemistry, Separation; BM - Solid Matter Physics ; Magnetism (FZU-D) OBOR OECD: Analytical chemistry; Condensed matter physics (including formerly solid state physics, supercond.) (FZU-D) Impact factor: 1.282, year: 2016

  16. Hyphenation of supercritical fluid chromatography with tandem mass spectrometry for fast determination of four aflatoxins in edible oil.

    Science.gov (United States)

    Lei, Fang; Li, Chenglong; Zhou, Shuang; Wang, Dan; Zhao, Yunfeng; Wu, Yongning

    2016-08-01

    Aflatoxins (AFTs) are of great concern all over the world. Supercritical fluid chromatography (SFC) has the advantage of fast, high resolution and excellent compatibility with a broad range of organic solvents and samples, thus hyphenating SFC with tandem mass spectrometry (MS/MS) can be used for the easy and fast determination of AFTs in edible oils. Edible oil was spiked with isotope-labeled aflatoxin standards, diluted with hexane and extracted with acetonitrile. The extraction was directly loaded to an SFC apparatus and separated on a UPC(2) 2-EP column with CO2 -methanol gradient elution. A post-column make-up flow was introduced to facilitate mass spectrometry performance, and the mixture was analyzed by MS/MS with an electrospray ionization (ESI) source. The SFC conditions including separation column, modifier and sample solvent were optimized, and the four target aflatoxins were baseline separated. The ESI interface parameters were also investigated, implicating the make-up flow as a critical factor for sensitive determination by SFC-MS/MS. The LOQs for the AFTs were 0.05-0.12 μg L(-1) , while the RSDs were lower than 8.5%. Supercritical fluid chromatography was successfully coupled to tandem mass spectrometry to establish a simple, fast and sensitive method for the analysis of four aflatoxins in edible oil. This shows the combination of SFC-MS/MS has great potential in determination of trace contaminants in food. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  17. Determination of low specific activity iodine-129 off-gas concentrations by GC separation and negative ionization mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Fernandez, S.J.; Rankin, R.A.; McManus, G.J.; Nielsen, R.A.; Delmore, J.E.; Hohorst, F.A.; Murphy, L.P.

    1983-09-01

    This document is the final report of the laboratory development of a method for determining the specific activity of the /sup 129/I emitted from a nuclear fuel reprocessing plant. The technique includes cryogenic sample collection, chemical form separation, quantitation by gas chromatography, and specific activity measurement of each chemical species by negative ionization mass spectrometry. The major conclusions were that both organic and elemental iodine can be quantitatively collected without fractionation and that specific activity measurements as low as one atom of /sup 129/I per 10/sup 5/ atoms of /sup 127/I are possible.

  18. Opticofiber photoacoustic spectrometry in single-ray two-cell grouping for analytical determination of actinoids in solutions of reprocessing

    International Nuclear Information System (INIS)

    Yin'kov, S.I.; Myasoedov, B.F.; Kikhara, T.; Fuine, S.; Maeda, M.

    1996-01-01

    Single-ray two-cell version of photoacoustic spectrometry with laser excitation (Laser Induced Photoacoustic Spectroscopy, LIPAS) for remote determination of actinoids ions in solutions is developed. The spectrometer characteristics were specified by means of uranium-containing solutions, including a great number of non-radioactive ions, the absorption bonds where of imitated the absorption of Pu(3) and Pu(4). The possibilities of the LIPAS technique were studied by analysis of ions, imitating plutonium within the range of 650-724 nm on synthetic solutions with high uranium(6) content and a great number of nonradioactive isotopes of fragmentation-type elements. 8 refs., 9 figs., 1 tab

  19. Determination of Cu, Cr, and As in preserved wood (Eucalyptus sp.) using x-ray fluorescent spectrometry techniques

    International Nuclear Information System (INIS)

    Sergio Matias Pereira Junior; Vera Akiko Maihara; Edson Goncalves Moreira; Vera Lucia Ribeiro Salvador; Ivone Mulako Sato

    2016-01-01

    Energy dispersive (EDXRF) and Portable (PXRF) X-ray fluorescence techniques are proposed for wood treatment control process and wood waste assortment. In this study, different retentions of chromated copper arsenate preservative were applied to Eucalyptus sp. sapwood samples. Cu, Cr and As were determined by XRF techniques in treated sapwood massive blocks and treated sapwood sawdust samples were analyzed by FAAS spectrometry (Flame Atomic Absorption) and INAA (Instrumental Neutron Activation Analysis). Cu, Cr and As mean values, obtained by FAASS and INAA, showed to be statically equal; however, XRF analysis showed considerable deviations, presenting the absorption and the enhancement effects in analytical lines. (author)

  20. Determination of low specific activity iodine-129 off-gas concentrations by GC separation and negative ionization mass spectrometry

    International Nuclear Information System (INIS)

    Fernandez, S.J.; Rankin, R.A.; McManus, G.J.; Nielsen, R.A.; Delmore, J.E.; Hohorst, F.A.; Murphy, L.P.

    1983-09-01

    This document is the final report of the laboratory development of a method for determining the specific activity of the 129 I emitted from a nuclear fuel reprocessing plant. The technique includes cryogenic sample collection, chemical form separation, quantitation by gas chromatography, and specific activity measurement of each chemical species by negative ionization mass spectrometry. The major conclusions were that both organic and elemental iodine can be quantitatively collected without fractionation and that specific activity measurements as low as one atom of 129 I per 10 5 atoms of 127 I are possible