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Sample records for chromatography inductively coupled

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

    International Nuclear Information System (INIS)

    Highlights: · We determine methylmercury in serum and plasma using isotope dilution calibration. · Separation by gas chromatography and detection by inductively coupled plasma mass spectrometry. · Data for 50 specimens provides first reference range for methylmercury in serum. · 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 198Hg-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) μg L-1 could be performed with uncertainty amplification factors -1 was estimated at 10 times the standard deviation of concentrations measured in preparation blanks. Within- and between-run relative standard deviations were -1, 0.35 μg L-1 and 2.8 μg L-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; -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.

  2. Novel applications of high performance ion chromatography - inductively coupled plasma mass spectrometry (HPIC-ICP-MS)

    International Nuclear Information System (INIS)

    This work demonstrates the development of highly sensitive and selective analytical methods, which make use of the hyphenation of high performance ion chromatography (HPIC) to inductively coupled plasma sector field mass spectrometry (ICP-SFMS). On-line coupling a chromatographic separation method with an elemental detection method provides two advantages: (1) The components of a possibly interfering matrix can be separated allowing accurate and precise ultra trace analysis of the element of interest and (2) elemental species of an element can be separated and quantified. In this work, matrix separation methods for interference free determination of 232Th, 234U, 235U and 238U in geological matrices were developed and employed. Furthermore HPIC-ICP-SFMS was applied for ultra trace analysis of Pd in environmental and geological matrices. The usefulness of HPIC-ICP-SFMS for speciation studies was demonstrated by investigating the interaction of an anti-cancer drug (cisplatin) with guanosine monophosphates. (author)

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

    OpenAIRE

    Kretschy, Daniela; Koellensperger, Gunda; Hann, Stephan

    2012-01-01

    This article reviews novel quantification concepts where elemental labelling is combined with flow injection inductively coupled plasma mass spectrometry (FI-ICP-MS) or liquid chromatography inductively coupled plasma mass spectrometry (LC–ICP-MS), and employed for quantification of biomolecules such as proteins, peptides and related molecules in challenging sample matrices. In the first sections an overview on general aspects of biomolecule quantification, as well as of labelling will be pre...

  4. Speciation of metals in soil extracts by size exclusion chromatography/inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Metal ion speciation influences the mobility of metals in the environment and their bioavailability. Dissolved humic substances (HS) and low molecular weight organic acids greatly influence the speciation of metals in soil and other natural environment. This study was conducted to identify HS bound metal in citric acid extracts from soil by size exclusion chromatography/inductively coupled plasma mass spectrometry (SEC/ICP-MS). The size exclusion column, which has optimal separation range from 3000-7000, was used. Absorption was monitored at 280 nm using an UV/VIS absorption detector. The eluate from the detector was directly introduced to the ICP-MS through a nebulizer. The size exclusion chromatography could separate HS and citric acid used for extraction. This was confirmed by the results obtained using a multi-channel diode array detector. HS was evidenced by broad absorption from UV to VIS range while organic acid was by narrow UV absorption. Analysis showed that most of iron was bound to HS, while part of aluminium was bound HS. Other metals were not bound to HS and some transitional metals except manganese made complex with citric acid. Most of silicon was not bound to HS and probably existed in the form of silicic acid. (author)

  5. Arsenic speciation in soil using high performance liquid chromatography/inductively coupled plasma/mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bass, D.A.; Yaeger, J.S.; Parish, K.J.; Crain, J.S.; Kiely, J.T.; Gowdy, M.J. [Argonne National Lab., IL (United States); Mohrman, G.B.; Besmer, M.G. [Rocky Mountain Arsenal, Commerce City, CO (United States)

    1996-08-01

    A method has been developed to identify and quantify As(III), As(V), and organoarsenic compounds in soil samples from the Rocky Mountain Arsenal (RMA) by high performance liquid chromatography/inductively coupled plasma/mass spectrometry (HPLC/ICP/MS). The soils were extracted using tetrabutylammonium hydroxide (TBAH) and sonication. The percentages of As(III), As(V), and organoarsenic species extracted from soil samples were 30, 50, and 100 respectively. The arsenic species were not altered during the extraction process. They were separated by reversed-phase, ion-pairing, HPLC using a microbore Inertsil-ODS{trademark} column. The HPLC column effluent was introduced into an ICP/MS system using a direct injection nebulizer (DIN). Detection limits of less than 1 pg were readily obtained for each arsenic species. Internal standards are recommended to increase accuracy and precision. Soil samples spiked with arsenic oxide, sodium arsenate, dimethylarsinic acid (DMAA), and chlorovinyl arsenious acid (CVAA) were extracted, identified and quantified with the HPLC/ICP/MS system. The soil samples were analyzed in support of the analytical needs of a thermal desorption treatability study being conducted at the RMA.

  6. Direct Determination of Total Arsenic and Arsenic Species by Ion Chromatography Coupled with Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    The simultaneous determination of As(III), As(V), and DMA has been performed by ion chromatography (IC) coupled with inductively coupled plasma-mass spectrometry (ICP-MS). The separation of the three arsenic species was achieved by an anionic separator column (AS 7) with an isocratic elution system. The separated species were directly detected by ICP-MS as an element-selective detection method. The IC-ICP-MS technique was applied for the determination of arsenic species in a NIST SRM 1643d water sample. An As(III) only was detected in the sample. The detection limits of As(III), As(V) and DMA were 0.31, 0.45, and 2.09 ng/mL, respectively. It was also applied for the determination of arsenic species in a human urine obtained by a volunteer, and three arsenic species were identified. The determination of total As in human urines that were obtained from 25 volunteers at the different age was also carried out by ICP-MS

  7. Determination of multiple human arsenic metabolites employing high performance liquid chromatography inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Stice, Szabina; Liu, Guangliang; Matulis, Shannon; Boise, Lawrence H; Cai, Yong

    2016-01-15

    During the metabolism of different arsenic-containing compounds in human, a variety of metabolites are produced with significantly varying toxicities. Currently available analytical methods can only detect a limited number of human metabolites in biological samples during one run due to their diverse characteristics. In addition, co-elution of species is often unnoticeable with most detection techniques leading to inaccurate metabolic profiles and assessment of toxicity. A high performance liquid chromatography inductively coupled mass spectrometry (HPLC-ICP-MS) method was developed that can identify thirteen common arsenic metabolites possibly present in human with special attention dedicated to thiolated or thiol conjugated arsenicals. The thirteen species included in this study are arsenite (As(III)), arsino-glutathione (As(GS)3), arsenate (As(V)), monomethylarsonous acid (MMA(III)), monomethylarsino-glutathione (MMA(III)(GS) 2), monomethylarsonic acid (MMA(V)), dimethylarsinous acid (DMA(III) (from DMA(III)I)), S-(dimethylarsinic)cysteine (DMA(III) (Cys)), dimethylarsino-glutathione (DMA(III)(GS)), dimethylarsinic acid (DMA(V)), dimethylmonothioarsinic acid (DMMTA(V)), dimethyldithioarsinic acid (DMDTA(V)), dimethylarsinothioyl glutathione (DMMTA(V)(GS)). The developed method was applied for the analysis of cancer cells that were incubated with darinaparsin (DMA(III)(GS)), a novel chemotherapeutic agent for refractory malignancies, and the arsenic metabolic profile obtained was compared to results using a previously developed method. This method provides a useful analytical tool which is much needed in unequivocally identifying the arsenicals formed during the metabolism of environmental arsenic exposure or therapeutic arsenic administration. PMID:26708625

  8. Gas and liquid chromatography with inductively coupled plasma mass spectrometry detection for environmental speciation analysis — advances and limitations

    Science.gov (United States)

    Szpunar, Joanna; McSheehy, Shona; Połeć, Kasia; Vacchina, Véronique; Mounicou, Sandra; Rodriguez, Isaac; Łobiński, Ryszard

    2000-07-01

    Recent advances in the coupling of gas chromatography (GC) and high performance liquid chromatography (HPLC) with inductively coupled plasma mass spectrometry (ICP MS) and their role in trace element speciation analysis of environmental materials are presented. The discussion is illustrated with three research examples concerning the following topics: (i) development and coupling of multicapillary microcolumn GC with ICP MS for speciation of organotin in sediment and biological tissue samples; (ii) speciation of arsenic in marine algae by size-exclusion-anion-exchange HPLC-ICP MS; and (iii) speciation of cadmium in plant cell cultures by size-exclusion HPLC-ICP MS. Particular attention is paid to the problem of signal identification in ICP MS chromatograms; the potential of electrospray MS/MS for this purpose is highlighted.

  9. Multicapillary gas chromatography coupled to inductively coupled plasma-time-of-flight mass spectrometry for rapid mercury speciation analysis

    International Nuclear Information System (INIS)

    A simple, rapid and accurate method on the basis of multicapillary gas chromatography (MCGC) combined with inductively coupled plasma-time-of-flight mass spectrometry (ICP-TOFMS) was developed for speciation analysis of methylmercury (MeHg+) and inorganic mercury (Hg2+). The potential of the ICP-TOFMS for transient multi-isotope detection of very short signals (peak width of 0.4 s at half peak height) was evaluated. Two injection systems (purge-and-trap (PTI) and split (SI) injections) were compared in terms of species separation resolution and transient signal profile. Using purge-and-trap injection, after in situ derivatization of the ionic mercury species with sodium tetraethylborate, a baseline separation of MeHg+ and Hg2+ was achieved within a chromatographic run of +) was used as internal standard. Detection limits of 16 and 257 fg g-1 for MeHg+ (as Hg) and Hg2+, respectively, were achieved. The analytical precision (R.S.D. (%)) for 10 successive injections of a standard mixture containing 10 pg MeHg+ (as Hg) and Hg2+ was 1.2% for MeHg+ and 4.1% for Hg2+. The method was validated by analysis of two biological certified reference materials (CRM): a dogfish muscle (DORM-2) and a freeze-dried tuna fish (CRM 464)

  10. Determination of trimethylselenonium ion in urine by ion chromatography and inductively coupled plasma mass spectrometry detection

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Jessen, K.D.; Kristensen, F.H.;

    2000-01-01

    H 3. The Se-78 and Se-82 isotopes were used for the inductively coupled plasma mass spectrometry (ICP-MS) detection. Using the chromatographic system on urine diluted 1 + 1, a large shift in retention times was observed. TMSe+ could be separated from the other species, but the signal from SeMet co...

  11. Determination of technetium-99 in soil samples by high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Muto, Toshio; Shimokawa, Toshinari [Tokyo Metropolitan Isotope Research Center (Japan)

    1997-03-01

    A new powerful analytical technique viz. high performance liquid chromatography(HPLC) coupled to inductively coupled plasma mass spectrometry(HPLC/ICP-MS) has been applied to the determination of technetium-99({sup 99}Tc) in soils as a typical environmental sample. Technetium was enriched in a solution from incinerated soil samples by leaching in HNO{sub 3} and passed through `TEVA resin` column. The solution was injected into HPLC/ICP-MS system to eliminate the interfering elements (i.e. Ru and Mo) and to determine the {sup 99}Tc concentration at the same time. The concentrations of {sup 99}Tc in the incinerated soils were found to be 0.49Bq/kg(0.77ng/kg)-1.4Bq/kg(2.2ng/kg) with the determination limit of 0.02Bq/kg(0.03ng/kg(0.03ppt)). The results indicate the following findings; 1) the determination of {sup 99}Tc by ICP-MS after strict elimination of the interfering elements by HPLC brings about the improvement in their reliability; 2) the detection limits identified are much lower compared with those by conventional ICP-MS methods because of the concentration of {sup 99}Tc to smaller volume, which is due to only 100{mu}l of samples could be measured by HPLC/ICP-MS system; 3) sample preparation could be simplified because of strict elimination of the interfering elements by HPLC. This research showed that HPLC/ICP-MS system is very effective to determine {sup 99}Tc in environmental samples. (author)

  12. Determination of technetium-99 in soil samples by high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    A new powerful analytical technique viz. high performance liquid chromatography(HPLC) coupled to inductively coupled plasma mass spectrometry(HPLC/ICP-MS) has been applied to the determination of technetium-99(99Tc) in soils as a typical environmental sample. Technetium was enriched in a solution from incinerated soil samples by leaching in HNO3 and passed through 'TEVA resin' column. The solution was injected into HPLC/ICP-MS system to eliminate the interfering elements (i.e. Ru and Mo) and to determine the 99Tc concentration at the same time. The concentrations of 99Tc in the incinerated soils were found to be 0.49Bq/kg(0.77ng/kg)-1.4Bq/kg(2.2ng/kg) with the determination limit of 0.02Bq/kg(0.03ng/kg(0.03ppt)). The results indicate the following findings; 1) the determination of 99Tc by ICP-MS after strict elimination of the interfering elements by HPLC brings about the improvement in their reliability; 2) the detection limits identified are much lower compared with those by conventional ICP-MS methods because of the concentration of 99Tc to smaller volume, which is due to only 100μl of samples could be measured by HPLC/ICP-MS system; 3) sample preparation could be simplified because of strict elimination of the interfering elements by HPLC. This research showed that HPLC/ICP-MS system is very effective to determine 99Tc in environmental samples. (author)

  13. Determination of selenite and selenate in human urine by ion chromatography and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Jons, O.

    2000-01-01

    The selenium species selenite, selenate and selenomethionine were separated in aqueous solution by ion chromatography. The separation was performed on an IonPac AG11 in series with an AS11 anion exchange column by elution with 25 mM sodium hydroxide in 2% methanol. The Se-78 and Se-82 isotopes were...... monitored in the inductively coupled plasma mass spectrometry (ICP-MS) detector. When the chromatographic system was applied to analysis of urine samples diluted 1 + 1, the selenomethionine signal appeared in the front together with other unresolved selenium species, while the selenite and selenate signals...

  14. Cobalamin speciation using reversed-phase micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry was optimized for the determination and separation of a mixture of cobalt containing species. Four cobalamin species (cyanocobalamin, hydroxocobalamin, methylcobalamin, and 5'-deoxyadenosylcobalamin) representing the various forms of vitamin B12 as well as the harmful corrinoid analogue cobinamide dicyanide were separated using reversed-phase microcapillary chromatography with columns containing C18 packing material with a 2-μm particle size. Selection of organic solvents for the separation took into consideration compatibility with the inductively coupled plasma mass spectrometer being used for element specific detection. Optimized method conditions included use of a methanol gradient and make-up solution for the nebulizer. Some issues associated with dead volume were overcome by the extension of the gradient program. The total analysis time was 52 min. The column-to-column variability was evaluated and was found to be very reasonable (9% RSD on average), confirming that this method is rugged and that the technology should be easily transferred to other laboratories

  15. Cobalamin speciation using reversed-phase micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Yanes, Enrique G. E-mail: yanes@bhnrc.usda.gov; Miller-Ihli, Nancy J. E-mail: miller-ihli@bhnrc.usda.gov

    2004-06-18

    Micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry was optimized for the determination and separation of a mixture of cobalt containing species. Four cobalamin species (cyanocobalamin, hydroxocobalamin, methylcobalamin, and 5'-deoxyadenosylcobalamin) representing the various forms of vitamin B12 as well as the harmful corrinoid analogue cobinamide dicyanide were separated using reversed-phase microcapillary chromatography with columns containing C18 packing material with a 2-{mu}m particle size. Selection of organic solvents for the separation took into consideration compatibility with the inductively coupled plasma mass spectrometer being used for element specific detection. Optimized method conditions included use of a methanol gradient and make-up solution for the nebulizer. Some issues associated with dead volume were overcome by the extension of the gradient program. The total analysis time was 52 min. The column-to-column variability was evaluated and was found to be very reasonable (9% RSD on average), confirming that this method is rugged and that the technology should be easily transferred to other laboratories.

  16. Cobalamin speciation using reversed-phase micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Yanes, Enrique G.; Miller-Ihli, Nancy J.

    2004-06-01

    Micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry was optimized for the determination and separation of a mixture of cobalt containing species. Four cobalamin species (cyanocobalamin, hydroxocobalamin, methylcobalamin, and 5'-deoxyadenosylcobalamin) representing the various forms of vitamin B12 as well as the harmful corrinoid analogue cobinamide dicyanide were separated using reversed-phase microcapillary chromatography with columns containing C18 packing material with a 2-μm particle size. Selection of organic solvents for the separation took into consideration compatibility with the inductively coupled plasma mass spectrometer being used for element specific detection. Optimized method conditions included use of a methanol gradient and make-up solution for the nebulizer. Some issues associated with dead volume were overcome by the extension of the gradient program. The total analysis time was 52 min. The column-to-column variability was evaluated and was found to be very reasonable (9% RSD on average), confirming that this method is rugged and that the technology should be easily transferred to other laboratories.

  17. Analysis of potassium iodate reduction in tissue homogenates using high performance liquid chromatography-inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Cao, Xiaoxiao; Ma, Wei; Liu, Liejun; Xu, Jing; Wang, Haiyan; Li, Xiuwei; Wang, Jiangqing; Zhang, Jianhua; Wang, Zexi; Gu, Yunyou

    2015-10-01

    Potassium iodate (KIO3) and potassium iodide (KI) are the major salt iodization agents used worldwide. Unlike iodide (I(-)), iodate (IO3(-)) should be reduced to I(-) before it can be effectively used by the thyroid. In this study, we developed a new method for analyzing IO3(-) and I(-) in tissue homogenates using high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry (HPLC-ICP-MS). We further applied the method to demonstrate the KIO3 reduction process by tissues in vitro. The effects of KIO3 on the total antioxidative activity (TAA) and reduced nicotinamide adenine dinucleotide phosphate (NADPH) were also investigated here. Finally, we found that IO3(-) can be reduced to I(-) by tissue homogenates and IO3(-) irreversibly decreases the antioxidant capability of tissues. Our studies suggest that KIO3 might have a big effect on the redox balance of tissue and would further result in oxidative stress of organisms. PMID:26302905

  18. Novel applications of high performance ion chromatography-inductively coupled plasma mass spectrometry (HPIC-ICP-MS)

    CERN Document Server

    Hann, S

    2001-01-01

    This work demonstrates the development of highly sensitive and selective analytical methods, which make use of the hyphenation of high performance ion chromatography (HPIC) to inductively coupled plasma sector field mass spectrometry (ICP-SFMS). On-line coupling a chromatographic separation method with an elemental detection method provides two advantages: (1) the components of a possibly interfering matrix can be separated allowing accurate and precise ultra trace analysis of the element of interest and (2) elemental species of an element can be separated and quantified. In this work, matrix separation methods for interference free determination of 232Th, 234U, 235U and 238U in geological matrices were developed and employed. Furthermore HPIC-ICP-SFMS was applied for ultra trace analysis of Pd in environmental and geological matrices. The usefulness of HPIC-ICP-SFMS for speciation studies was demonstrated by investigating the interaction of an anti-cancer drug (cisplatin) with guanosine monophosphates.

  19. Novel applications of high performance ion chromatography-inductively coupled plasma mass spectrometry (HPIC-ICP-MS)

    International Nuclear Information System (INIS)

    This work demonstrates the development of highly sensitive and selective analytical methods, which make use of the hyphenation of high performance ion chromatography (HPIC) to inductively coupled plasma sector field mass spectrometry (ICP-SFMS). On-line coupling a chromatographic separation method with an elemental detection method provides two advantages: (1) the components of a possibly interfering matrix can be separated allowing accurate and precise ultra trace analysis of the element of interest and (2) elemental species of an element can be separated and quantified. In this work, matrix separation methods for interference free determination of 232Th, 234U, 235U and 238U in geological matrices were developed and employed. Furthermore HPIC-ICP-SFMS was applied for ultra trace analysis of Pd in environmental and geological matrices. The usefulness of HPIC-ICP-SFMS for speciation studies was demonstrated by investigating the interaction of an anti-cancer drug (cisplatin) with guanosine monophosphates. (author)

  20. Lead speciation in rainwater by isotope dilution-high performance liquid chromatography-inductively coupled plasma-mass spectrometry

    Science.gov (United States)

    Ebdon, Les; Hill, Steve J.; Rivas, Cristina

    1998-02-01

    A new method for lead speciation in rainwater by isotope dilution analysis (IDA) using directly coupled high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) is described and demonstrated. Samples containing trimethyllead (TML) chloride and triethyllead (TEL) chloride in the presence of large amounts of inorganic lead have been analysed by HPLC-ICP-MS using reverse phase ion-pairing chromatography. The detection limit for the procedure is 3 ng g -1 for TML as Pb and 14 ng g -1 for TEL as Pb, with a linear range exceeding 1000 ng g -1 and a relative standard deviation of 4% for TML in the range 50-1000 ng g -1. TML chloride isotopically enriched in the stable 206 isotope was prepared and used to enhance the accuracy of the method by isotope dilution analysis. The IDA-HPLC-ICP-MS method was successfully applied to the analysis of a sample of artificial rainwater used in a collaborative study.

  1. Selenium speciation analysis in a sediment using strong anion exchange and reversed phase chromatography coupled with inductively coupled plasma-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ochsenkuehn-Petropoulou, M.; Michalke, B.; Kavouras, D.; Schramel, P

    2003-02-22

    An analytical procedure for selenium speciation of analysis of selenourea (SeU), selenoethionine (SeE), selenomethionine (SeM), Se(VI), Se(IV), dimethylselenide (dMeSe) and dimethyldiselenide (dMedSe) was developed, based on two complementary liquid chromatography (LC) techniques coupled with inductively coupled plasma-mass spectrometry (ICP-MS). Specifically, strong anion exchange (SAX) chromatography coupled with ICP-MS was used for the separation and quantification of all the earlier mentioned Se compounds, except for the two methyl selenides, which could be separated and determined by reversed phase chromatography coupled with ICP-MS. This procedure was applied to a soil sample from the warm springs area of Thermopyles (Greece). For leaching the Se species from the soil sample, four extraction methods, using water at ambient temperature, hot water, methanol and 0.5 M HCl, were tested for their efficiency of extracting the different Se species. The speciation results obtained by the LC-ICP-MS methods were compared with those obtained by voltammetric techniques. The determination of total selenium in the sample was achieved by graphite furnace atomic absorption spectrometry, as well as by ICP-atomic emission spectrometry, after suitable digestion of the sediment sample.

  2. Hydride generation, electrothermal vaporization and liquid chromatography as sample introduction techniques for inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Olson, Lisa K.; Vela, Nohora P.; Caruso, Joseph A.

    1995-06-01

    Although the most common method of sample introduction for inductively coupled plasma-mass spectrometry (ICP-MS) used is pneumatic nebulization, it suffers from limitations particularly with respect to the transport efficiency. In an effort to improve the analyte transport to the plasma, many alternative techniques have been studied, including electrothermal vaporization (ETV) and hydride generation, among others. Flow injection and liquid chromatography, although they employ pneumatic nebulization, have also been studied as sample introduction techniques due to the ability to analyze small volume samples and obtain speciation information. Here, some advances in sample introduction for ICP-MS will be discussed including hydride generation and ETV techniques. In addition, recent studies in HPLC-ICP-MS will also be described. Advantages and disadvantages of each method will be reviewed together with the application to some representative samples.

  3. Estimation of the quantification uncertainty from flow injection and liquid chromatography transient signals in inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    The quality of the quantitative results obtained from transient signals in high-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICPMS) and flow injection-inductively coupled plasma mass spectrometry (FI-ICPMS) was investigated under multielement conditions. Quantification methods were based on multiple-point calibration by simple and weighted linear regression, and double-point calibration (measurement of the baseline and one standard). An uncertainty model, which includes the main sources of uncertainty from FI-ICPMS and HPLC-ICPMS (signal measurement, sample flow rate and injection volume), was developed to estimate peak area uncertainties and statistical weights used in weighted linear regression. The behaviour of the ICPMS instrument was characterized in order to be considered in the model, concluding that the instrument works as a concentration detector when it is used to monitorize transient signals from flow injection or chromatographic separations. Proper quantification by the three calibration methods was achieved when compared to reference materials, although the double-point calibration allowed to obtain results of the same quality as the multiple-point calibration, shortening the calibration time. Relative expanded uncertainties ranged from 10-20% for concentrations around the LOQ to 5% for concentrations higher than 100 times the LOQ

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

    International Nuclear Information System (INIS)

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

  5. Simplified sample preparation procedure for measuring isotope-enriched methylmercury by gas chromatography and inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Avramescu, Mary-Luyza; Zhu, Joy; Yumvihoze, Emmanuel; Hintelmann, Holger; Fortin, Danielle; Lean, David R S

    2010-06-01

    Many procedures have been developed to measure the concentration of monomethylmercury (MeHg) from different sample matrices, and the use of stable isotopes of mercury now provides opportunities to determine its formation and degradation rates. Here, a modified procedure for measuring mercury isotopes in sediment samples that uses acid leaching-ion exchange-thiosulfate extraction (TSE) to isolate and purify the methylated mercury from the matrix is proposed. The latter is followed by aqueous-phase ethylation, purge and trap on Tenax, gas chromatography separation of ethylated mercury compounds, and inductively coupled plasma mass spectrometry detection. The new TSE procedure bridges together two well-known methods, the acid-leaching and distillation-derivatization procedures, offering the advantages of artifact-free formation of the first, and low detection limits and the possibility of quantification of individual isotopes of mercury of the second. The modified procedure retains the derivatization, purge and trap, and gas chromatography and inductively coupled plasma mass spectrometry (GC-ICP-MS) detection steps from the distillation-derivatization procedure, and eliminates the distillation step, which is not only laborious but also expensive, due to the high cost of installation and time-consuming cleaning process. Major advantages of the TSE procedure proposed include the extraction and analysis of a large number of samples in a short time, excellent analyte recoveries, and the lack of artifact formation. Sediment certified reference materials (CRMs), BCR 580 and IAEA 405, were used to test the TSE procedure accuracy. Recoveries between 94 to 106% and 95 to 96% were obtained for CRMs and spiked samples (Milli-Q(R) water), respectively. Comparisons among thiosulfate extraction, distillation, and acid-leaching procedures have shown good agreement of methylmercury values. PMID:20821567

  6. Methyl mercury in nail clippings in relation to fish consumption analysis with gas chromatography coupled to inductively coupled plasma mass spectrometry: a first orientation.

    Science.gov (United States)

    Krystek, Petra; Favaro, Paulo; Bode, Peter; Ritsema, Rob

    2012-08-15

    For the identification of human exposure to one of the most toxic compounds, which is methyl mercury (MeHg(+)), fingernail clippings were selected as the matrix of interest. Within this pilot study, six samples from different origins and from people with different food consumption patterns were chosen. Species-analysis of MeHg(+) was performed according to the following procedure: dissolution of the sample material in tetramethylammonium hydroxide (TMAH), derivatisation of MeHg(+) with sodium tetraethylborate (NaBEt(4)), extraction into iso-octane and measurement with gas chromatography hyphenated to inductively coupled plasma mass spectrometry (GC-ICPMS) for the quantification MeHg(+). PMID:22841050

  7. Characterization of Arsenic Biotransformation Products from an Open Anaerobic Degradation of Fucus distichus by Hydride Generation Gas Chromatography Atomic Absorption Spectrometry and High Performance Liquid Chromatography Inductively Coupled Plasma Mass Spectrometry

    OpenAIRE

    Abiodun A. Ojo; Onasanya, Amos

    2013-01-01

    This work reports on the isolation and determination of biotransformation products obtained from the organoarsenic compounds that are present in Fucus distichus when it was subjected to an open anaerobic decomposition by using the Hydride Generation Gas Chromatography Atomic Absorption Spectrometry (HG-GC-AAS) and High Performance Liquid Chromatography Inductively Coupled Plasma Mass Spectrometry (HPLC-ICP-MS). The seaweed and filtrate residues obtained from the open anaerobic degradation pro...

  8. High performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry for V and Ni quantification as tetrapyrroles

    Science.gov (United States)

    Duyck, Christiane Béatrice; Saint'Pierre, Tatiana Dillenburg; Miekeley, Norbert; da Fonseca, Teresa Cristina Oliveira; Szatmari, Peter

    2011-05-01

    A method was developed for the determination of V and Ni as tetrapyrroles by High Performance Liquid Chromatography hyphenated to Inductively Coupled Plasma Mass Spectrometry (HPLC-ICP-MS) using reversed phase and elution gradient. Chlorinated solvents and tetrahydrofuran were investigated as regard to separation time and ICP-MS detection efficiencies. The final elution gradient program started from pure methanol to a mixture of 20:80 (v/v) chloroform:methanol. External quantification of V and Ni with inorganic standards by flow injection ICP-MS, used online with HPLC, resulted in 95% of recoveries. The Limits of Detection for V during methanol elution and for Ni during the 20% chloroform gradient elution were evaluated by their minimum detectable concentrations, which were, respectively, 5 μg L - 1 and 8 μg L - 1 . The methodology was applied to polar and resin fractions separated from a Brazilian crude oil and a sediment extract from an oil-polluted area in the Guanabara Bay, Rio de Janeiro, Brazil. Vanadium as tetrapyrroles represented the totality of V content in the polar fraction, whereas Ni was in different polar forms in the resin and sediment extract.

  9. Fingerprinting of complex mixtures with the use of high performance liquid chromatography, inductively coupled plasma atomic emission spectroscopy and chemometrics

    International Nuclear Information System (INIS)

    The molecular and metal profile fingerprints were obtained from a complex substance, Atractylis chinensis DC-a traditional Chinese medicine (TCM), with the use of the high performance liquid chromatography (HPLC) and inductively coupled plasma atomic emission spectroscopy (ICP-AES) techniques. This substance was used in this work as an example of a complex biological material, which has found application as a TCM. Such TCM samples are traditionally processed by the Bran, Cut, Fried and Swill methods, and were collected from five provinces in China. The data matrices obtained from the two types of analysis produced two principal component biplots, which showed that the HPLC fingerprint data were discriminated on the basis of the methods for processing the raw TCM, while the metal analysis grouped according to the geographical origin. When the two data matrices were combined into a one two-way matrix, the resulting biplot showed a clear separation on the basis of the HPLC fingerprints. Importantly, within each different grouping the objects separated according to their geographical origin, and they ranked approximately in the same order in each group. This result suggested that by using such an approach, it is possible to derive improved characterisation of the complex TCM materials on the basis of the two kinds of analytical data. In addition, two supervised pattern recognition methods, K-nearest neighbors (KNNs) method, and linear discriminant analysis (LDA), were successfully applied to the individual data matrices-thus, supporting the PCA approach

  10. High performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry for V and Ni quantification as tetrapyrroles

    International Nuclear Information System (INIS)

    A method was developed for the determination of V and Ni as tetrapyrroles by High Performance Liquid Chromatography hyphenated to Inductively Coupled Plasma Mass Spectrometry (HPLC-ICP-MS) using reversed phase and elution gradient. Chlorinated solvents and tetrahydrofuran were investigated as regard to separation time and ICP-MS detection efficiencies. The final elution gradient program started from pure methanol to a mixture of 20:80 (v/v) chloroform:methanol. External quantification of V and Ni with inorganic standards by flow injection ICP-MS, used online with HPLC, resulted in 95% of recoveries. The Limits of Detection for V during methanol elution and for Ni during the 20% chloroform gradient elution were evaluated by their minimum detectable concentrations, which were, respectively, 5 μg L-1 and 8 μg L-1. The methodology was applied to polar and resin fractions separated from a Brazilian crude oil and a sediment extract from an oil-polluted area in the Guanabara Bay, Rio de Janeiro, Brazil. Vanadium as tetrapyrroles represented the totality of V content in the polar fraction, whereas Ni was in different polar forms in the resin and sediment extract.

  11. High performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry for V and Ni quantification as tetrapyrroles

    Energy Technology Data Exchange (ETDEWEB)

    Duyck, Christiane Beatrice, E-mail: cbduyck@vm.uff.br [Pontificia Universidade Catolica do Rio de Janeiro (PUC-Rio), R. Marques de Sao Vicente, 225, Gavea, Rio de Janeiro, RJ, 22451-900 (Brazil); Universidade Federal Fluminense (UFF), Campus do Valonguinho, Outeiro de Sao Joao Batista, s/no, 24020-150, Niteroi, RJ (Brazil); Saint' Pierre, Tatiana Dillenburg; Miekeley, Norbert [Pontificia Universidade Catolica do Rio de Janeiro (PUC-Rio), R. Marques de Sao Vicente, 225, Gavea, Rio de Janeiro, RJ, 22451-900 (Brazil); Oliveira da Fonseca, Teresa Cristina; Szatmari, Peter [Centro de Pesquisas Leopoldo A. Miguez de Mello da Petrobras (CENPES), Av. Horacio Macedo, 950, Cidade Universitaria, Rio de Janeiro, RJ, 21941-915 (Brazil)

    2011-05-15

    A method was developed for the determination of V and Ni as tetrapyrroles by High Performance Liquid Chromatography hyphenated to Inductively Coupled Plasma Mass Spectrometry (HPLC-ICP-MS) using reversed phase and elution gradient. Chlorinated solvents and tetrahydrofuran were investigated as regard to separation time and ICP-MS detection efficiencies. The final elution gradient program started from pure methanol to a mixture of 20:80 (v/v) chloroform:methanol. External quantification of V and Ni with inorganic standards by flow injection ICP-MS, used online with HPLC, resulted in 95% of recoveries. The Limits of Detection for V during methanol elution and for Ni during the 20% chloroform gradient elution were evaluated by their minimum detectable concentrations, which were, respectively, 5 {mu}g L{sup -1} and 8 {mu}g L{sup -1}. The methodology was applied to polar and resin fractions separated from a Brazilian crude oil and a sediment extract from an oil-polluted area in the Guanabara Bay, Rio de Janeiro, Brazil. Vanadium as tetrapyrroles represented the totality of V content in the polar fraction, whereas Ni was in different polar forms in the resin and sediment extract.

  12. Fingerprinting of complex mixtures with the use of high performance liquid chromatography, inductively coupled plasma atomic emission spectroscopy and chemometrics

    Energy Technology Data Exchange (ETDEWEB)

    Ni Yongnian [Department of Chemistry, Nanchang University, Nanchang, Jiangxi 330047 (China)], E-mail: ynni@ncu.edu.cn; Peng Yunyan [Department of Chemistry, Nanchang University, Nanchang, Jiangxi 330047 (China); Kokot, Serge [Inorganic Materials Program, School of Physical and Chemical Sciences, Queensland University of Technology, Brisbane, Queensland 4001 (Australia)

    2008-05-26

    The molecular and metal profile fingerprints were obtained from a complex substance, Atractylis chinensis DC-a traditional Chinese medicine (TCM), with the use of the high performance liquid chromatography (HPLC) and inductively coupled plasma atomic emission spectroscopy (ICP-AES) techniques. This substance was used in this work as an example of a complex biological material, which has found application as a TCM. Such TCM samples are traditionally processed by the Bran, Cut, Fried and Swill methods, and were collected from five provinces in China. The data matrices obtained from the two types of analysis produced two principal component biplots, which showed that the HPLC fingerprint data were discriminated on the basis of the methods for processing the raw TCM, while the metal analysis grouped according to the geographical origin. When the two data matrices were combined into a one two-way matrix, the resulting biplot showed a clear separation on the basis of the HPLC fingerprints. Importantly, within each different grouping the objects separated according to their geographical origin, and they ranked approximately in the same order in each group. This result suggested that by using such an approach, it is possible to derive improved characterisation of the complex TCM materials on the basis of the two kinds of analytical data. In addition, two supervised pattern recognition methods, K-nearest neighbors (KNNs) method, and linear discriminant analysis (LDA), were successfully applied to the individual data matrices-thus, supporting the PCA approach.

  13. Determination of hexavalent chromium in sludge incinerator emissions using ion chromatography and inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Arar, E.J.; Long, S.E. (Technology Applications, Inc., Cincinnati, OH (United States)); Martin, T.D.; Gold, S. (Environmental Monitoring Systems Lab., Cincinnati, OH (United States))

    1992-10-01

    A unique approach is described using ion chromatography (IC) and inductively coupled plasma mass spectrometry (ICP-MS) for the determination of hexavalent chromium [Cr(VI)] in wastewater sludge incinerator emissions. Quartz fiber filters, spiked with an isotopically enriched ([sup 50]Cr or [sup 53]Cr) chromate salt, were used to collect emission particulates. The enriched Cr(VI) isotope was used to monitor the reduction of Cr(IV) during sample collection using a pseudo-first-order reaction model and to calculate the rate of deposition of native Cr(VI) on the filters. At the end of the sampling period, the Cr(VI) was extracted from the filters with 0.1 N sodium hydroxide and determined by IC using postcolumn derivatization with 1,5-diphenylcarbohydrazide. To determine the ratio of enriched Cr(VI) to the native Cr(VI) emitted from the incinerator, an additional aliquot of the sample extract was preconcentrated by IC and the isotopic composition of the Cr(VI) fraction determined by ICP-MS. 21 refs., 4 figs., 3 figs.

  14. Speciation of vanadium in oilsand coke and bacterial culture by high performance liquid chromatography inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Li, X Sherry; Glasauer, Susan; Le, X Chris

    2007-10-17

    A simple and sensitive method for the speciation of vanadium(III), (IV), and (V) was developed by using high performance liquid chromatography and inductively coupled plasma mass spectrometry (HPLC-ICPMS). The EDTA-complexed vanadium species were separated on a strong anion exchange column with an eluent containing 2 mM EDTA, 3% acetonitrile, and 80 mM ammonium bicarbonate at pH 6. Each analysis was complete in 5 min. The detection limits were 0.6, 0.7 and 1.0 microg L(-1) for V(III), V(IV), and V(V), respectively. The method was applied to coke pore water samples from an oilsand processing/upgrading site in Fort McMurray, Alberta, Canada and to Shewanella putrefaciens CN32 bacterial cultures incubated with V(V). In the coke pore water samples, V(IV) and V(V) were found to be the major species. For the first time, V(III) was detected in the bacterial cultures incubated with V(V). PMID:17936102

  15. Speciation of vanadium in oilsand coke and bacterial culture by high performance liquid chromatography inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Li, X. Sherry [Department of Chemistry, University of Alberta, Edmonton, Alberta T6G 2G2 (Canada); Le, X. Chris [Department of Chemistry, University of Alberta, Edmonton, Alberta T6G 2G2 (Canada); Analytical and Environmental Toxicology, Department of Laboratory Medicine and Pathology, University of Alberta, Edmonton, Alberta T6G 2G3 (Canada)], E-mail: xc.le@ualberta.ca

    2007-10-17

    A simple and sensitive method for the speciation of vanadium(III), (IV), and (V) was developed by using high performance liquid chromatography and inductively coupled plasma mass spectrometry (HPLC-ICPMS). The EDTA-complexed vanadium species were separated on a strong anion exchange column with an eluent containing 2 mM EDTA, 3% acetonitrile, and 80 mM ammonium bicarbonate at pH 6. Each analysis was complete in 5 min. The detection limits were 0.6, 0.7 and 1.0 {mu}g L{sup -1} for V(III), V(IV), and V(V), respectively. The method was applied to coke pore water samples from an oilsand processing/upgrading site in Fort McMurray, Alberta, Canada and to Shewanella putrefaciens CN32 bacterial cultures incubated with V(V). In the coke pore water samples, V(IV) and V(V) were found to be the major species. For the first time, V(III) was detected in the bacterial cultures incubated with V(V)

  16. Speciation of vanadium in oilsand coke and bacterial culture by high performance liquid chromatography inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    A simple and sensitive method for the speciation of vanadium(III), (IV), and (V) was developed by using high performance liquid chromatography and inductively coupled plasma mass spectrometry (HPLC-ICPMS). The EDTA-complexed vanadium species were separated on a strong anion exchange column with an eluent containing 2 mM EDTA, 3% acetonitrile, and 80 mM ammonium bicarbonate at pH 6. Each analysis was complete in 5 min. The detection limits were 0.6, 0.7 and 1.0 μg L-1 for V(III), V(IV), and V(V), respectively. The method was applied to coke pore water samples from an oilsand processing/upgrading site in Fort McMurray, Alberta, Canada and to Shewanella putrefaciens CN32 bacterial cultures incubated with V(V). In the coke pore water samples, V(IV) and V(V) were found to be the major species. For the first time, V(III) was detected in the bacterial cultures incubated with V(V)

  17. Survey of inorganic arsenic in marine animals and marine certified reference materials by anion exchange high-performance liquid chromatography-inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Sloth, Jens Jørgen; Larsen, Erik Huusfeldt; Julshamn, Kåre

    2005-01-01

    A method for the determination of inorganic arsenic in seafood samples using high-performance liquid chromatography-inductively coupled plasma mass spectrometry is described. The principle of the method relied on microwave-assisted alkaline dissolution of the sample, which at the same time oxidized...... arsenite [As(Ill)] to arsenate [As(V)], whereby inorganic arsenic could be determined as the single species As(V). Anion exchange chromatography using isocratic elution with aqueous ammonium carbonate as the mobile phase was used for the separation of As(V) from other coextracted organoarsenic compounds...

  18. Speciation of eight arsenic compounds in human urine by high performance liquid chromatography with inductively coupled plasma mass spectrometric detection using antimonate for internal chromatographic standardization

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Pritzl, G.; Hansen, S. H.

    1993-01-01

    Four anionic and four cationic arsenic compounds in urine were separated by anion- and cation-exchange high-performance liquid chromatography and detected by inductively coupled plasma mass spectrometry (ICP-MS) at m/z 75. The species were the anions arsenite, arsenate, monomethylarsonate and...... arsenate in urine but was stable after at least 4-fold dilution of the urine with water. Arsenite was unstable in both urine samples and standard mixtures when diluted with the basic (pH 10.3) mobile phase used for anion chromatography. This could not be prevented by adding ascorbic acid as antioxidant...

  19. Separation of selenium, zinc, and copper compounds in bovine whey using size exclusion chromatography linked to inductively coupled plasma mass spectrometry.

    OpenAIRE

    Hoac, Tien; Lundh, Thomas; Purup, Stig; Onning, Gunilla; Sejrsen, Kristen; Akesson, Bjorn

    2007-01-01

    To study the role of trace elements for the quality and nutritional value of bovine milk, the distribution of selenium, zinc, and copper in whey was investigated using a method linking size exclusion chromatography to inductively coupled plasma mass spectrometry (SEC-ICP-MS). Three major peaks were detected for selenium, two peaks for zinc, and five peaks for copper. More than 65% of the selenium was found in protein fractions, mainly in fractions coinciding with the major whey proteins beta-...

  20. Arsenic Species in Edible Seaweeds Using In Vitro Biomimetic Digestion Determined by High-Performance Liquid Chromatography Inductively Coupled Plasma Mass Spectrometry

    OpenAIRE

    Yan-Fang Zhao; Ji-Fa Wu; De-Rong Shang; Jin-Song Ning; Hai-Yan Ding; Yu-Xiu Zhai

    2014-01-01

    Arsenite [As (III)], arsenate [As (V)], methylarsonate (MMA), and dimethylarsinate (DMA) in five edible seaweeds (the brown algae Laminaria japonica, red algae Porphyra yezoensis, brown algae Undaria pinnatifida, brown algae Hizikia fusiformis, and green algae Enteromorpha prolifera) were analyzed using in vitro digestion method determined by high-performance liquid chromatography inductively coupled plasma mass spectrometry. The results showed that DMA was found in the water extracts of all ...

  1. Quantitation of motexafin lutetium in human plasma by liquid chromatography-tandem mass spectrometry and inductively coupled plasma-atomic emission spectroscopy

    OpenAIRE

    Miles, Dale; Mody, Tarak D.; Hatcher, Lori I.; Fiene, John; Stiles, Mark; Patrick P. Lin; Lee, J.W.

    2003-01-01

    Liquid chromatography-tandem mass spectrometry (LC-MS/MS) and inductively coupled plasma-atomic emission spectroscopy (ICP-AES) methods were developed and validated for the evaluation of motexafin lutetium (MLu, lutetium texaphyrin, PCI-0123) pharmacokinetics in human plasma. The LC-MS/MS method was specific for MLu, whereas the ICP-AES method measured total elemental lutetium. Both methods were fast, simple, precise, and accurate. For the LC-MS/MS method, a closely related analogue (PCI-0353...

  2. High temperature liquid chromatography-inductively coupled plasma mass spectrometry for the determination of arsenosugars in biological samples.

    Science.gov (United States)

    Terol, Amanda; Ardini, Francisco; Grotti, Marco; Todolí, José Luis

    2012-11-01

    The potential of high temperature liquid chromatography (HTLC) with detection by inductively coupled plasma mass spectrometry (ICP-MS) for the determination of arsenosugars in marine organisms was examined for the first time. The retention behavior of four naturally occurring dimethylarsinoylribosides was studied on a graphite column using plain water as mobile phase. An aqueous solution of pH 8, ionic strength 13.8mM and containing 2% (v/v) of methanol, along with a column temperature of 120°C and a liquid flow rate of 1.0 mL/min, were selected as the optimal conditions, as they allowed the separation of the four arsenosugars in less than 18 min, without any interferences due to other common arsenic species (arsenite, arsenate, dimethylarsinate, methylarsonate and arsenobetaine). The run time could be further decreased to 12 min by working at 1.5 mL/min, although with a 3-4 times loss of sensitivity. The procedural limits of detection were 0.03-0.04 μg As/g dry mass, and the precision of the procedure ranged from 4% for arsenosugar glycerol to 18% for arsenosugar sulfate (RSD%, n=5). The developed method was applied to a number of representative biological samples, such as algae and crustaceans, providing results consistent with previous studies. In the red algae samples, the most of extracted arsenic was as arsenosugars (81-97%), mainly arsenosugar phosphate (56-94%). On the other hand, lower concentrations of these compounds were found in the crustacean, accounting for about 15% of the extracted arsenic. PMID:22995196

  3. Determination of phosphoric acid triesters in human plasma using solid-phase microextraction and gas chromatography coupled to inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Shah, Monika; Meija, Juris; Cabovska, Baiba; Caruso, Joseph A

    2006-01-27

    A simple and sensitive method for determination of phosphoric acid triesters at trace levels in human plasma sample is described. In this work, solid-phase microextraction (SPME) is employed as a sample preparation procedure for extraction and pre-concentration of alkyl and aryl phosphates followed by gas chromatography coupled to inductively coupled plasma mass spectrometry (GC-ICP-MS) for phosphorus-specific and very sensitive determination of these compounds in human plasma. The detection limits from blood plasma were 50 ngL(-1) (tripropyl phosphate), 17 ngL(-1) (tributyl phosphate), 240 ngL(-1) (tris(2-chloroethyl) phosphate) and 24 ngL(-1) (triphenyl phosphate). Sample preparation involves plasma deproteinization followed by direct immersion SPME with 65 microm poly(dimethylsiloxane/divinylbenzene) fiber. Extraction was performed at 40 degrees C for 30 min and at pH 7.0 in 10 mM sodium carbonate buffer. The reported method, to our knowledge, describes the first application of SPME with element-specific detection for analysis of phosphoric acid esters. Application of the method to the plasma samples, previously stored in poly(vinyl chloride) plasma bags revealed the presence of triphenyl phosphate, which was further confirmed by SPME GC time-of-flight high-resolution mass spectrometry. PMID:16337211

  4. Determination of actinides in environmental and biological samples using high-performance chelation ion chromatography coupled to sector-field inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Truscott, J B; Jones, P; Fairman, B E; Evans, E H

    2001-08-31

    High-performance chelation ion chromatography, using a neutral polystyrene substrate dynamically loaded with 0.1 mM dipicolinic acid, coupled with sector-field inductively coupled plasma mass spectrometry has been successfully used for the separation of the actinides thorium, uranium, americium, neptunium and plutonium. Using this column it was possible to separate the various actinides from each other and from a complex sample matrix. In particular, it was possible to separate plutonium and uranium to facilitate the detection of the former free of spectral interference. The column also exhibited some selectivity for different oxidation states of Np, Pu and U. Two oxidation states each for plutonium and neptunium were found, tentatively identified as Np(V) and Pu(III) eluting at the solvent front, and Np(IV) and Pu(IV) eluting much later. Detection limits were 12, 8, and 4 fg for 237Np, 239Pu, and 241Am, respectively, for a 0.5 ml injection. The system was successfully used for the determination of 239Pu in NIST 4251 Human Lung and 4353 Rocky Flats Soil, with results of 570+/-29 and 2939+/-226 fg g(-1), respectively, compared with a certified range of 227-951 fg g(-1) for the former and a value of 3307+/-248 fg g(-1) for the latter. PMID:11589474

  5. Alcohol and metal determination in alcoholic beverages through high-temperature liquid-chromatography coupled to an inductively coupled plasma atomic emission spectrometer.

    Science.gov (United States)

    Terol, Amanda; Paredes, Eduardo; Maestre, Salvador E; Prats, Soledad; Todolí, José L

    2011-06-01

    In the present work, an inductively coupled plasma atomic emission spectrometry (ICP-AES) system was used as a high temperature liquid chromatography (HTLC) detector for the determination of alcohols and metals in beverages. For the sake of comparison, a refractive index (RI) detector was also employed for the first time to detect alcohols with HTLC. The organic compounds studied were methanol, ethanol, propan-1-ol and butan-1-ol (in the 10-125 mg/L concentration range) and the elements tested were magnesium, aluminum, copper, manganese and barium at concentrations included between roughly 0.01 and 80 mg/L. Column heating temperatures ranged from 80 to 175 °C and the optimum ones in terms of peak resolution, sensitivity and column lifetime were 125 and 100 °C for the HTLC-RI and HTLC-ICP-AES couplings, respectively. The HTLC-ICP-AES interface design (i.e., spray chamber design and nebulizer type used) was studied and it was found that a single pass spray chamber provided about 2 times higher sensitivities than a cyclonic conventional design. Comparatively speaking, limits of detection for alcohols were of the same order for the two evaluated detection systems (from 5 to 25 mg/L). In contrast, unlike RI, ICP-AES provided information about the content of both organic and inorganic species. Furthermore, temperature programming was applied to shorten the analysis time and it was verified that ICP-AES was less sensitive to temperature changes and modifications in the analyte chemical nature than the RI detector. Both detectors were successfully applied to the determination of short chain alcohols in several beverages such as muscatel, pacharan, punch, vermouth and two different brands of whiskeys (from 10 to 40 g of ethanol/100 g of sample). The results of the inorganic elements studied by HTLC-ICP-AES were compared with those obtained using inductively coupled plasma mass spectrometry (ICP-MS) obtaining good agreement between them. Recoveries found for spiked samples

  6. Capabilities of mixed-mode liquid chromatography coupled to inductively coupled plasma mass spectrometry for the simultaneous speciation analysis of inorganic and organically-bound selenium.

    Science.gov (United States)

    Peachey, Emma; Cook, Ken; Castles, Adrian; Hopley, Christopher; Goenaga-Infante, Heidi

    2009-10-16

    This work investigates for the first time the potential of mixed-mode (anion-exchange with reversed-phase) high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry (ICP-MS) for the simultaneous retention and selective separation of a range of inorganic and organically-bound selenium (Se) species. Baseline separation and detection of selenocystine (SeCys(2)), Se-methyl-selenocysteine (SeMC), selenomethionine (SeMet), methylseleninic acid (MSA), selenite, gamma-glutamyl-methyl-selenocysteine (gamma-glutamyl-SeMC), and selenate in a Se standard mixture by mixed-mode HPLC-ICP-MS was achieved by switching between two citrate mobile phases of different pH and ionic strength within a single chromatographic run of 20 min. Limits of detection obtained for these Se species ranged from 80 ng kg(-1) (for SeMC) to 123 ng kg(-1) (for selenate). Using this approach as developed for selenium speciation, an adequate separation of inorganic and organic As compounds was also achieved. These include arsenite, arsenate, arsenobetaine (AsB) and dimethylarsenic acid (DMA), which may coexist with Se species in biological samples. Application of the newly proposed methodology to the investigation of the elemental species distribution in watercress (used as the model sample) after enzymatic hydrolysis or leaching in water by accelerated solvent extraction (ASE) was addressed. Only SeMet, SeMC and selenate could be tentatively identified in watercress extracts by mixed-mode HPLC-ICP-MS and retention time matching with standards. Recoveries (n=3) of these Se species from samples spiked with standards averaged 102% (for SeMC), 94.9% (for SeMet) and 98.3% (for selenate). Verification of the presence of SeMet and SeMC in an enzymatic watercress extract was achieved by on-line HPLC-ESI MS/MS in selected reaction monitoring (SRM) mode. PMID:19758595

  7. Towards silicon speciation in light petroleum products using gas chromatography coupled to inductively coupled plasma mass spectrometry equipped with a dynamic reaction cell

    Science.gov (United States)

    Chainet, Fabien; Lienemann, Charles-Philippe; Ponthus, Jeremie; Pécheyran, Christophe; Castro, Joaudimir; Tessier, Emmanuel; Donard, Olivier François Xavier

    2014-07-01

    Silicon speciation has recently gained interest in the oil and gas industry due to the significant poisoning problems caused by silicon on hydrotreatment catalysts. The poisoning effect clearly depends on the structure of the silicon species which must be determined and quantified. The hyphenation of gas chromatography (GC) coupled to inductively coupled plasma mass spectrometry (ICP-MS) allows a specific detection to determine the retention times of all silicon species. The aim of this work is to determine the retention indices of unknown silicon species to allow their characterization by a multi-technical approach in order to access to their chemical structure. The optimization of the dynamic reaction cell (DRC) of the ICP-MS using hydrogen as reactant gas successfully demonstrated the resolution of the interferences (14N14N+ and 12C16O+) initially present on 28Si. The linearity was excellent for silicon compounds and instrumental detection limits ranged from 20 to 140 μg of Si/kg depending on the response of the silicon compounds. A continuous release of silicon in the torch was observed most likely due to the use of a torch and an injector which was made of quartz. A non-universal response for silicon was observed and it was clearly necessary to use response coefficients to quantify silicon compounds. Known silicon compounds such as cyclic siloxanes (D3-D16) coming from PDMS degradation were confirmed. Furthermore, more than 10 new silicon species never characterized before in petroleum products were highlighted in polydimethylsiloxane (PDMS) degradation samples produced under thermal cracking of hydrocarbons. These silicon species mainly consisted of linear and cyclic structures containing reactive functions such as ethoxy, peroxide and hydroxy groups which can be able to react with the alumina surface and hence, poison the catalyst. This characterization will further allow the development of innovative solutions such as trapping silicon compounds or

  8. Determination of rare-earth elements in geological materials by ion-exchange chromatography separation and induction coupled plasma emission spectroscopy

    International Nuclear Information System (INIS)

    A methodology for the analysis of Rare-Earth elements in geological samples has been developed. Ion exchange chromatography for the separation and induction coupled plasma emission spectroscopy for the analysis have been used. The columns with cationic resin were calibrated with radioactive elements. With complexes matrices, the instrument's data must be corrected for the presence of majors elements (CEM) and for the interferences of the Rare-earth elements (CETR). The accuracy and precision are evaluated critically with respect to the convenience and efficiency of this methodology in the analysis of rare-Earth elements i geological samples. (author)

  9. Comparative oxidation state specific analysis of arsenic species by high-performance liquid chromatography- inductively coupled plasma-mass spectrometry and hydride generation-cryotrapping-atomic absorption spectrometry

    OpenAIRE

    Currier, J. M.; Saunders, R J; Ding, L.; Bodnar, W.; Cable, P.; Matoušek, T. (Tomáš); Creed, J. T.; Stýblo, M.

    2013-01-01

    The formation of methylarsonous acid (MAsIII) and dimethylarsinous acid (DMAsIII) in the course of inorganic arsenic (iAs) metabolism plays an important role in the adverse effects of chronic exposure to iAs. High-performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) and hydride generation-cryotrapping-atomic absorption spectrometry (HG-CT-AAS) have been frequently used for the analysis of MAsIII and DMAsIII in biological samples. While HG-CT-AAS has con...

  10. Determination of 20 trace elements and arsenic species for a realgar-containing traditional Chinese medicine Niuhuang Jiedu tablets by direct inductively coupled plasma-mass spectrometry and high performance liquid chromatography-inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Jin, Pengfei; Liang, Xiaoli; Xia, Lufeng; Jahouh, Farid; Wang, Rong; Kuang, Yongmei; Hu, Xin

    2016-01-01

    Niuhuang Jiedu tablet (NHJDT) is a realgar-containing traditional Chinese medicine. A direct inductively coupled plasma-mass spectrometry (ICP-MS) method for the simultaneous determination of 20 trace elements (Mg, K, Ca, Na, Fe, As, Zn, Sr, Ba, Cu, Mn, Ni, Pb, V, Cr, Se, Co, Mo, Cd, Hg) in NHJDT, as well as in water, gastric fluid and intestinal fluid was established. Meanwhile, a high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) method was developed for the determination of arsenite (As(III)), arsenate (As(V)), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA) and for the identification of arsenobetaine (AsB) and arsenocholine (AsC) in these extracts. Both methods were fully validated in the respect of linearity, sensitivity, precision, stability and accuracy. The reliability of the ICP-MS method was further evaluated using a certified standard reference material prepared from dried tomato leaves (NIST, SRM 1572a). The analysis showed that some manufacturers formulated lower amount of realgar than required in the Chinese Pharmacopoeia (ChP) in their preparations. In addition, almost same extraction profiles for total As and inorganic As were found in water and in gastrointestinal fluids, while higher extraction rates for other 19 elements were observed in gastrointestinal fluids. Our findings show that the toxicities of Hg, Cu, Cd and Pb in NHJDP are low, while the real As toxicity in NHJDT should be deeply investigated. PMID:26653746

  11. Speciation of arsenic animal feed additives by microbore high-performance liquid chromatography with inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Pergantis, S A; Heithmar, E M; Hinners, T A

    1997-10-01

    Phenylarsonic compounds have been used as poultry and swine feed additives for the purpose of growth promotion and disease prevention. Owing to the lack of suitable analytical methods, however, knowledge of their metabolism, environmental fate and impact remains incomplete. In order to compensate for this, analytical procedures were developed that allow the speciation of arsenic animal feed additives by using microbore high-performance liquid chromatography (microHPLC) coupled on-line with ICP-MS. More specifically, reversed-phase (RP) chromatographic methods were optimised to achieve the separation of various phenylarsonic acids from each other and from the more toxic inorganic arsenic compounds. This mode of chromatography, however, exhibits limitations, especially in the presence of naturally occurring organoarsenic compounds. The application of RP ion-pairing chromatography eliminates such shortcomings by minimising the co-elution of arsenic species. In general, the microHPLC-ICP-MS methods developed in this study provide high selectivity, extremely good sensitivity, low limits of detection (low-ppb or sub-pg amounts of As), require small sample volumes (< 1 microliter), minimise waste and operate most efficiently under low mobile-phase flow rates (15-40 microliters min-1), which are compatible for use with other types of mass spectrometers, e.g., electrospray. Reference materials containing naturally occurring arsenic compounds were spiked with phenylarsonic compounds and then analysed by using the procedures developed in this study. PMID:9463956

  12. Separation of silver ions and starch modified silver nanoparticles using high performance liquid chromatography with ultraviolet and inductively coupled mass spectrometric detection

    Science.gov (United States)

    Hanley, Traci A.; Saadawi, Ryan; Zhang, Peng; Caruso, Joseph A.; Landero-Figueroa, Julio

    2014-10-01

    The production of commercially available products marketed to contain silver nanoparticles is rapidly increasing. Species-specific toxicity is a phenomenon associated with many elements, including silver, making it imperative to develop a method to identify and quantify the various forms of silver (namely, silver ions vs. silver nanoparticles) possibly present in these products. In this study a method was developed using high performance liquid chromatography (HPLC) with ultraviolet (UV-VIS) and inductively coupled mass spectrometric (ICP-MS) detection to separate starch stabilized silver nanoparticles (AgNPs) and silver ions (Ag+) by cation exchange chromatography with 0.5 M nitric acid mobile phase. The silver nanoparticles and ions were baseline resolved with an ICP-MS response linear over four orders of magnitude, 0.04 mg kg- 1 detection limit, and 90% chromatographic recovery for silver solutions containing ions and starch stabilized silver nanoparticles smaller than 100 nm.

  13. Separation of silver ions and starch modified silver nanoparticles using high performance liquid chromatography with ultraviolet and inductively coupled mass spectrometric detection

    International Nuclear Information System (INIS)

    The production of commercially available products marketed to contain silver nanoparticles is rapidly increasing. Species-specific toxicity is a phenomenon associated with many elements, including silver, making it imperative to develop a method to identify and quantify the various forms of silver (namely, silver ions vs. silver nanoparticles) possibly present in these products. In this study a method was developed using high performance liquid chromatography (HPLC) with ultraviolet (UV–VIS) and inductively coupled mass spectrometric (ICP-MS) detection to separate starch stabilized silver nanoparticles (AgNPs) and silver ions (Ag+) by cation exchange chromatography with 0.5 M nitric acid mobile phase. The silver nanoparticles and ions were baseline resolved with an ICP-MS response linear over four orders of magnitude, 0.04 mg kg−1 detection limit, and 90% chromatographic recovery for silver solutions containing ions and starch stabilized silver nanoparticles smaller than 100 nm

  14. Towards silicon speciation in light petroleum products using gas chromatography coupled to inductively coupled plasma mass spectrometry equipped with a dynamic reaction cell

    Energy Technology Data Exchange (ETDEWEB)

    Chainet, Fabien, E-mail: fabien.chainet@ifpen.fr [IFP Energies nouvelles, Rond-point de l' échangeur de Solaize, BP 3, 69360 Solaize (France); Lienemann, Charles-Philippe; Ponthus, Jeremie [IFP Energies nouvelles, Rond-point de l' échangeur de Solaize, BP 3, 69360 Solaize (France); Pécheyran, Christophe; Castro, Joaudimir; Tessier, Emmanuel; Donard, Olivier François Xavier [LCABIE-IPREM, UMR 5254, CNRS-UPPA, Helioparc, 2 av. Pr. Angot, 64053 Pau (France)

    2014-07-01

    Silicon speciation has recently gained interest in the oil and gas industry due to the significant poisoning problems caused by silicon on hydrotreatment catalysts. The poisoning effect clearly depends on the structure of the silicon species which must be determined and quantified. The hyphenation of gas chromatography (GC) coupled to inductively coupled plasma mass spectrometry (ICP-MS) allows a specific detection to determine the retention times of all silicon species. The aim of this work is to determine the retention indices of unknown silicon species to allow their characterization by a multi-technical approach in order to access to their chemical structure. The optimization of the dynamic reaction cell (DRC) of the ICP-MS using hydrogen as reactant gas successfully demonstrated the resolution of the interferences ({sup 14}N{sup 14}N{sup +} and {sup 12}C{sup 16}O{sup +}) initially present on {sup 28}Si. The linearity was excellent for silicon compounds and instrumental detection limits ranged from 20 to 140 μg of Si/kg depending on the response of the silicon compounds. A continuous release of silicon in the torch was observed most likely due to the use of a torch and an injector which was made of quartz. A non-universal response for silicon was observed and it was clearly necessary to use response coefficients to quantify silicon compounds. Known silicon compounds such as cyclic siloxanes (D{sub 3}–D{sub 16}) coming from PDMS degradation were confirmed. Furthermore, more than 10 new silicon species never characterized before in petroleum products were highlighted in polydimethylsiloxane (PDMS) degradation samples produced under thermal cracking of hydrocarbons. These silicon species mainly consisted of linear and cyclic structures containing reactive functions such as ethoxy, peroxide and hydroxy groups which can be able to react with the alumina surface and hence, poison the catalyst. This characterization will further allow the development of innovative

  15. Development of an analytical method for the determination of polybrominated diphenyl ethers in sewage sludge by the use of gas chromatography coupled to inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Novak, Petra; Zuliani, Tea; Milačič, Radmila; Ščančar, Janez

    2016-04-01

    Polybrominated diphenyl ethers (PBDEs) are flame retardants. As a consequence of their widespread use, they have been released into the environment. PBDEs are lipophilic organic contaminants that enter wastewater treatment plants (WWTPs) from urban, agricultural and industrial discharges. Because of their low aqueous solubility and resistance to biodegradation, up to 90% of the PBDEs are accumulated in the sewage sludge during the wastewater treatment. To assess the possibilities for sludge re-use, a reliable determination of the concentrations of these PBDEs is of crucial importance. Six PBDE congeners (BDE 28, BDE 47, BDE 99, BDE 100, BDE 153 and BDE 154) are listed as priority substances under the EU Water Framework Directive. In the present work a simple analytical method with minimal sample-preparation steps was developed for a sensitive and reliable determination of the six PBDEs in sewage sludge by the use of gas chromatography coupled to inductively coupled plasma mass spectrometry (GC-ICP-MS). For this purpose an extraction procedure was optimised. Different extracting agents (methanol (MeOH), acetic acid (AcOH)/MeOH mixture (3:1) and 0.1 mol L(-1) hydrochloric acid (HCl) in MeOH) followed by the addition of a Tris-citrate buffer (co-extracting agent) and iso-octane were applied under different modes of extraction (mechanical shaking, microwave- and ultrasound-assisted extraction). Mechanical shaking or the microwave-assisted extraction of sewage sludge with 0.1 mol L(-1) HCl in MeOH and the subsequent addition of the Tris-citrate buffer and the iso-octane extracted the PBDEs from the complex sludge matrix most effectively. However, due to easier sample manipulation during the extraction step, mechanical shaking was used. The PBDEs in the organic phase were quantified with GC-ICP-MS by applying a standard addition calibration method. The spike recovery test (recoveries between 95 and 104%) and comparative analyses with the species-specific isotope

  16. Towards silicon speciation in light petroleum products using gas chromatography coupled to inductively coupled plasma mass spectrometry equipped with a dynamic reaction cell

    International Nuclear Information System (INIS)

    Silicon speciation has recently gained interest in the oil and gas industry due to the significant poisoning problems caused by silicon on hydrotreatment catalysts. The poisoning effect clearly depends on the structure of the silicon species which must be determined and quantified. The hyphenation of gas chromatography (GC) coupled to inductively coupled plasma mass spectrometry (ICP-MS) allows a specific detection to determine the retention times of all silicon species. The aim of this work is to determine the retention indices of unknown silicon species to allow their characterization by a multi-technical approach in order to access to their chemical structure. The optimization of the dynamic reaction cell (DRC) of the ICP-MS using hydrogen as reactant gas successfully demonstrated the resolution of the interferences (14N14N+ and 12C16O+) initially present on 28Si. The linearity was excellent for silicon compounds and instrumental detection limits ranged from 20 to 140 μg of Si/kg depending on the response of the silicon compounds. A continuous release of silicon in the torch was observed most likely due to the use of a torch and an injector which was made of quartz. A non-universal response for silicon was observed and it was clearly necessary to use response coefficients to quantify silicon compounds. Known silicon compounds such as cyclic siloxanes (D3–D16) coming from PDMS degradation were confirmed. Furthermore, more than 10 new silicon species never characterized before in petroleum products were highlighted in polydimethylsiloxane (PDMS) degradation samples produced under thermal cracking of hydrocarbons. These silicon species mainly consisted of linear and cyclic structures containing reactive functions such as ethoxy, peroxide and hydroxy groups which can be able to react with the alumina surface and hence, poison the catalyst. This characterization will further allow the development of innovative solutions such as trapping silicon compounds or

  17. Speciation of butyltin compounds in environmental and biological samples using headspace single drop microextraction coupled with gas chromatography-inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Xiao, Qin; Hu, Bin; He, Man

    2008-11-21

    A method based on headspace single drop microextraction (HS-SDME) in combination with gas chromatography-inductively coupled plasma mass spectrometry (GC-ICP-MS) was proposed for the speciation analysis of butyltin compounds in environmental and biological samples. The sodium tetraethylborate (NaBEt4) and sodium tetrahydroborate (NaBH4) were used as the derivatizing reagent for in situ derivatization of the butyltins. For the two derivatizations, the HS-SDME parameters such as organic solvent, drop volume, sample pH, stirring rate, temperature, extraction time and the ionic strength were examined systematically. The analytical performance including the linearity ranges, limits of detection (LODs) and reproducibilities of the two derivatizations were compared under the respective optimized conditions. Derivatization with NaBEt(4) proved to be more sensitive and robust than that with NaBH4, leading to the LODs of 1.4 ng/L for MBT, 1.8 ng/L for DBT and 0.8 ng/L for TBT. The reproducibilities, expressed as relative standard deviations (RSDs), were in the range of 1.1-5.3% (c=1 microg/L, n=3). With tripropyltin (TPrT) as internal standard, HS-SDME-GC-ICP-MS with NaBEt(4) derivatization was applied for the speciation analysis of butyltins in real seawater and shellfish samples. The butyltins found in the real-world samples are 31ng/L MBT, 79 ng/L DBT and 32 ng/L TBT for seawater, and 11.6-30.4 ng/g MBT, 11.8-8.9 ng/g DBT and 12.8-52.6 ng/g TBT for different shellfish samples. For validation, the developed method was also employed for the speciation analysis of butyltins in certified reference material (CRM) of PACS-2 sediment, and the determined values are in a good agreement with the certified values. The developed method is simple, rapid, sensitive, and cost-effective and provides an attractive alternative for butyltins speciation in biological and environmental samples with complex matrix. PMID:18922539

  18. Investigation of mercury-containing proteins by enriched stable isotopic tracer and size-exclusion chromatography hyphenated to inductively coupled plasma-isotope dilution mass spectrometry

    International Nuclear Information System (INIS)

    In order to investigate trace mercury-containing proteins in maternal rat and their offspring, a method of enriched stable isotopic tracer (196Hg and 198Hg) combined with size-exclusion chromatography (SEC) coupled to inductively coupled plasma-isotope dilution mass spectrometry (ICP-IDMS) was developed. Prior to the analysis, 196Hg- and 198Hg-enriched methylmercury was administrated to the pregnant rats. Then the mercury-containing proteins in serum and brain cytosol of the dam and pup rats were separated by size-exclusion columns and the mercury was detected by ICP-MS. The ICP-MS spectrogram of the tracing samples showed significantly elevated 196Hg and 198Hg isotopic signals compared with the natural ones, indicating that the detection sensitivity could be increased by the tracer method. The contents of mercury in chromatographic fractions of the dam and pup rat brain cytosol were quantitatively estimated by post-column reverse ID-ICP-MS. The quantitative speciation differences of mercury in brain cytosol between the dam and pup rats were observed, indicating that such studies could be useful for toxicological estimation. Additionally, the isotopic ratio measurement of 198Hg/202Hg in the tracing samples could be used to identify the artifact mercury species caused in the analytical procedure. The study demonstrates that the tracer method combined with high-performance liquid chromatography (HPLC)-ICP-IDMS could provide reliably qualitative and quantitative information on mercury-containing proteins in organisms

  19. Environmental application of elemental speciation analysis based on liquid or gas chromatography hyphenated to inductively coupled plasma mass spectrometry-A review

    International Nuclear Information System (INIS)

    In recent years the number of environmental applications of elemental speciation analysis using inductively coupled plasma mass spectrometry (ICP-MS) as detector has increased significantly. The analytical characteristics, such as extremely low detection limits (LOD) for almost all elements, the wide linear range, the possibility for multi-elemental analysis and the possibility to apply isotope dilution mass spectrometry (IDMS) make ICP-MS an attractive tool for elemental speciation analysis. Two methodological approaches, i.e. the combination of ICP-MS with high performance liquid chromatography (HPLC) and gas chromatography (GC), dominate the field. Besides the investigation of metals and metalloids and their species (e.g. Sn, Hg, As), representing 'classic' elements in environmental science, more recently other elements (e.g. P, S, Br, I) amenable to ICP-MS determination were addressed. In addition, the introduction of isotope dilution analysis and the development of isotopically labeled species-specific standards have contributed to the success of ICP-MS in the field. The aim of this review is to summarize these developments and to highlight recent trends in the environmental application of ICP-MS coupled to GC and HPLC.

  20. Ultra-Sensitive Elemental Analysis Using Plasmas 5.Speciation of Arsenic Compounds in Biological Samples by High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry System

    Science.gov (United States)

    Kaise, Toshikazu

    Arsenic originating from the lithosphere is widely distributed in the environment. Many arsenicals in the environment are in organic and methylated species. These arsenic compounds in drinking water or food products of marine origin are absorbed in human digestive tracts, metabolized in the human body, and excreted viatheurine. Because arsenic shows varying biological a spects depending on its chemical species, the biological characteristics of arsenic must be determined. It is thought that some metabolic pathways for arsenic and some arsenic circulation exist in aqueous ecosystems. In this paper, the current status of the speciation analysis of arsenic by HPLC/ICP-MS (High Performance Liquid Chromatography-Inductively Coupled Plasma Mass spectrometry) in environmental and biological samples is summarized using recent data.

  1. Determination of trace zirconium and hafnium in high-purity scandium oxide by inductively coupled plasma atomic emission spectrometry and extraction chromatography

    International Nuclear Information System (INIS)

    Inductively coupled plasma atomic emission spectrometry in combination with extraction chromatography was applied to the determination of trace amounts of zirconium and hafnium in high-purity scandium oxide. The chromatographic column separation procedure was carried out with 1-phenyl-3-methyl-4-benzoylpyrazol-5-one as the stationary phase and hydrochloride acid as the mobile phase. Optimum column operating conditions were established. The enrichment factor based on 0.1 g of scandium oxide was over 2000. The results obtained agreed well with those obtained by spark-source mass spectrometry without the separation of scandium. For a sample mass of 0.3 g, the detection limits for zirconium and hafnium were 0.14 and 0.17 μg g-1, respectively. The proposed method could be applied to the analysis of scandium oxide of laser grade and 99.9995% purity

  2. Inductively coupled plasma mass spectrometry in comparison with neutron activation and ion chromatography with UV/VIS detection for the determination of lanthanides in plant materials.

    Science.gov (United States)

    Bulska, Ewa; Danko, Bożena; Dybczyński, Rajmund S; Krata, Agnieszka; Kulisa, Krzysztof; Samczyński, Zbigniew; Wojciechowski, Marcin

    2012-08-15

    Analytical performance of inductively coupled plasma mass spectrometry (ICP-MS) for determination of lanthanides in plant materials was investigated and compared with neutron activation analysis (NAA) as well as ion chromatography (IC) with UV-VIS detection. Two sample preparation protocols were tested: (i) microwave assisted digestion by concentrated nitric acid; (ii) microwave digestion involving silica and fluoride removal, followed by the selective and quantitative lanthanides group separation from the plant matrix. Several Certified Reference Materials (CRM) of plant origin were used for the evaluation of the accuracy of the applied analytical procedures. The consistency of results, obtained by various methods, enabled to establish the tentative recommended values (TRV) for several missing elements in one of CRMs. The ICP-MS, due to its very high sensitivity, has the potential to contribute to this aim. The discrepancy of the results obtained by various methods was discussed in a view of possible matrix effects related to the composition of investigated materials. PMID:22841084

  3. Development of cadmium/silver/palladium separation by ion chromatography with quadrupole inductively coupled plasma mass spectrometry detection for off-line cadmium isotopic measurements

    International Nuclear Information System (INIS)

    A separation method was investigated to perform off-line cadmium isotopic measurements on a 109Ag transmutation target. Ion chromatography (IC) with Q ICPMS detection (quadrupole inductively coupled plasma mass spectrometry detection) was chosen to separate cadmium from the isobarically interfering elements, silver and palladium, present in the sample. The optimization of chromatographic conditions was particularly studied. Several anion and cation columns (Dionex AG11 (R), CS10 (R) and CS12 (R)) were compared with different mobile phases (HNO3, HCl). The separation procedure was achieved with a carboxylate-functionalized cation exchange CS12 column using 0.5 M HNO3 as eluent. The developed technique yielded satisfactory results in terms of separation factors (greater than 5) and provides an efficient solution to obtain rapidly purified cadmium fractions (decontamination factors higher 100,000 for silver and palladium) which can directly be analyzed by multi collection inductively coupled plasma mass spectrometry (MC ICPMS). By applying the proposed procedure, accurate and precise cadmium isotope ratios were determined for the irradiated 109Ag transmutation target. (authors)

  4. Precise determination of dissolved silica in seawater by ion-exclusion chromatography isotope dilution inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Highlights: • One mg kg−1 level of dissolved silica in seawater was determined precisely (0.5 %). • Silicon background problem was minimized to yield a BEC value of 3 ng g−1. • Good precision of isotope ratio measurement was achieved in m/Δm = 4000 of ICP–MS. • Developed method has been applied to production of three levels of seawater CRMs. - Abstract: Ion exclusion chromatograph (IEC) isotope dilution (ID) inductively coupled plasma mass spectrometry (ICP–MS) (IEC–ID–ICP–MS) was developed for measurement of dissolved silica in seawater, which was applied to production of certified reference materials (CRMs) of three concentration levels of nutrients (high, medium and low levels). IEC–ICP–MS has been employed to separate dissolved silica from seawater matrix. In the present study, in order to solve substantial problems due to spectral interference in ICP–MS and to improve the accuracy of IEC–ICP–MS beyond standard addition or conventional calibration methods, ID method was coupled with ICP-sector field mass spectrometry (operated under medium resolution,i.e., m/Δm = 4000). In addition, effects of various operating parameters in ICP–MS on a silicon background level were also investigated to obtain lower background equivalent concentration (BEC). As a result, 3 ng g−1 of the BEC and 0.5 % of relative standard uncertainties were achieved in the analyses of dissolved silica in seawater samples at concentration levels from 4.0 mg kg -1 to 0.8 mg kg−1 as silicon. The developed method was successfully validated by analyses of an artificial seawater containing a known amount of silicate and the seawater certified reference material MOOS-2 produced by the National Research Council Canada

  5. Application of high performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS) for determination of chromium compounds in the air at the workplace.

    Science.gov (United States)

    Stanislawska, Magdalena; Janasik, Beata; Wasowicz, Wojciech

    2013-12-15

    The toxicity and bioavailability of chromium species are highly dependable on the form or species, therefore determination of total chromium is insufficient for a complete toxicological evaluation and risk assessment. An analytical method for determination of soluble and insoluble Cr (III) and Cr (VI) compounds in welding fume at workplace air has been developed. The total chromium (Cr) was determined by using quadruple inductively coupled plasma mass spectrometry (ICP-MS) equipped with a dynamic reaction cell (DRC(®)). Soluble trivalent and hexavalent chromium compounds were determined by high performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS). A high-speed, reversed-phase CR C8 column (PerkinElmer, Inc., Shelton, CT, USA) was used for the speciation of soluble Cr (III) and soluble Cr (VI). The separation was accomplished by interaction of the chromium species with the different components of the mobile phase. Cr (III) formed a complex with EDTA, i.e. retained on the column, while Cr (VI) existed in the solutions as dichromate. Alkaline extraction (2% KOH and 3% Na2CO3) and anion exchange column (PRP-X100, PEEK, Hamilton) were used for the separation of the total Cr (VI). The results of the determination of Cr (VI) were confirmed by the analysis of the certified reference material BCR CRM 545 (Cr (VI) in welding dust). The results obtained for the certified material (40.2±0.6 g kg(-1)) and the values recorded in the examined samples (40.7±0.6 g kg(-1)) were highly consistent. This analytical method was applied for the determination of chromium in the samples in the workplace air collected onto glass (Whatman, Ø 37 mm) and membrane filters (Sartorius, 0.8 μm, Ø 37 mm). High performance liquid chromatography with inductively coupled plasma mass spectrometry is a remarkably powerful and versatile technique for determination of chromium species in welding fume at workplace air. PMID:24209303

  6. Method for the quantification of vanadyl porphyrins in fractions of crude oils by High Performance Liquid Chromatography-Flow Injection-Inductively Coupled Plasma Mass Spectrometry

    Science.gov (United States)

    Wandekoken, Flávia G.; Duyck, Christiane B.; Fonseca, Teresa C. O.; Saint'Pierre, Tatiana D.

    2016-05-01

    High performance liquid chromatography hyphenated by flow injection to inductively coupled plasma mass spectrometry (HPLC-FI-ICP-MS) was used to investigate V linked to porphyrins present in fractions of crude oil. First, the crude oil sample was submitted to fractionation by preparative liquid chromatography with UV detection, at the porphyrin Soret band wavelength (400 nm). The obtained porphyrin fractions were then separated in a 250 mm single column, in the HPLC, and eluted with different mobile phases (methanol or methanol:toluene (80:20; v:v)). The quantification of V-porphyrins in the fractions eluted from HPLC was carried out by online measuring the 51V isotope in the ICP-MS, against vanadyl octaethylporphine standard solutions (VO-OEP), prepared in the same solvent as the mobile phase, and injected post-column directly into the plasma. A 20 μg L- 1 Ge in methanol was used as internal standard for minimizing non-spectral interference, such as short-term variations due to injection. The mathematical treatment of the signal based on Fast Fourier Transform smoothing algorithm was employed to improve the precision. The concentrations of V as V-porphyrins were between 2.7 and 11 mg kg- 1 in the fractions, which were close to the total concentration of V in the porphyrin fractions of the studied crude oil.

  7. Ultrasound-assisted enzymatic hydrolysis for iodinated amino acid extraction from edible seaweed before reversed-phase high performance liquid chromatography-inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Romarís-Hortas, Vanessa; Bermejo-Barrera, Pilar; Moreda-Piñeiro, Antonio

    2013-09-27

    The combination of reverse phase high performance liquid chromatography (RP-HPLC) with inductively coupled plasma mass spectrometry (ICP-MS) was used for the determination of monoiodotyrosine (MIT) and diiodotyrosine (DIT) in edible seaweed. A sample pre-treatment based on ultrasound assisted enzymatic hydrolysis was optimized for the extraction of these iodinated amino acids. Pancreatin was selected as the most adequate type of enzyme, and parameters affecting the extraction efficiency (pH, temperature, mass of enzyme and extraction time) were evaluated by univariate approaches. In addition, extractable inorganic iodine (iodide) was also quantified by anion exchange high performance liquid chromatography (AE-HPLC) coupled with ICP-MS. The proposed procedure offered limits of detection of 1.1 and 4.3ngg(-1) for MIT and DIT, respectively. Total iodine contents in seaweed, as well as total iodine in enzymatic digests were measured by ICP-MS after microwave assisted alkaline digestion with tetramethylamonium hydroxide (TMAH) for total iodine assessment, and also by treating the pancreatin extracts (extractable total iodine assessment). The optimized procedure was successfully applied to five different types of edible seaweed. The highest total iodine content, and also the highest iodide levels, was found in the brown seaweed Kombu (6646±45μgg(-1)). Regarding iodinated amino acids, Nori (a red seaweed) was by far the one with the highest amount of both species (42±3 and 0.41±0.024μgg(-1) for MIT and DIT, respectively). In general, MIT concentrations were much higher than the amounts of DIT, which suggests that iodine from iodinated proteins in seaweed is most likely bound in the form of MIT residues. PMID:23972456

  8. Fast Determination of Toxic Arsenic Species in Food Samples Using Narrow-bore High-Performance Liquid-Chromatography Inductively Coupled Plasma Mass Spectrometry.

    Science.gov (United States)

    Terol, Amanda; Marcinkowska, Monika; Ardini, Francisco; Grotti, Marco

    2016-01-01

    A new method for the speciation analysis of arsenic in food using narrow-bore high-performance liquid-chromatography inductively coupled plasma mass spectrometry (HPLC-ICP-MS) has been developed. Fast separation of arsenite, arsenate, monomethylarsonic acid and dimethylarsinic acid was carried out in 7 min using an anion-exchange narrow-bore Nucleosil 100 SB column and 12 mM ammonium dihydrogen phosphate of pH 5.2 as the mobile phase, at a flow rate of 0.3 mL min(-1). A PFA-ST micronebulizer jointed to a cyclonic spray chamber was used for HPLC-ICP-MS coupling. Compared with standard-bore HPLC-ICP-MS, the new method has provided higher sensitivity, reduced mobile-phase consumption, a lower matrix plasma load and a shorter analysis time. The achieved instrumental limits of detection were in the 0.3 - 0.4 ng As mL(-1) range, and the precision was better than 3%. The arsenic compounds were efficiently (>80%) extracted from various food samples using a 1:5 methanol/water solution, with additional ultrasonic treatment for rice products. The applicability of this method was demonstrated by the analysis of several samples, such as seafood (fish, mussels, shrimps, edible algae) and rice-based products (Jasmine and Arborio rice, spaghetti, flour, crackers), including three certified reference materials. PMID:27506720

  9. Nuclide analysis of an irradiated tantalum target of a spallation neutron source using high performance ion chromatography and inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Tantalum was used as target material in a spallation source where the neutrons are produced via spallation reactions between a highly energetic proton beam (Ep∼800 MeV) and the heavy tantalum target. The lanthanide metals were theoretically predicted in the irradiated tantalum target as a major fraction of spallation nuclides with quite significantly different nuclide abundances in comparison to the natural isotopic composition. Due to expected isobaric interferences of long-lived radionuclides and stable isotopes, all the lanthanide metals had to be separated chemically prior to their mass spectrometric determination by high performance ion chromatography (IC) after dissolution of tantalum in a HNO3/HF mixture and separation of the tantalum matrix by liquid-liquid extraction. An analytical procedure was applied for the determination of spallation nuclides of lanthanide metals in an irradiated tantalum target using IC coupled on-line to a sensitive double-focusing sector field inductively coupled plasma mass spectrometer (DF-ICP-MS).The experimental results of nuclide abundances of the lanthanides in the irradiated tantalum target obtained by on-line LC-ICP-MS are in good agreement with theoretically calculated values. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  10. Speciation of the bio-available iodine and bromine forms in edible seaweed by high performance liquid chromatography hyphenated with inductively coupled plasma-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Romaris-Hortas, Vanessa; Bermejo-Barrera, Pilar [Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, University of Santiago de Compostela, Avenida das Ciencias, s/n. 15782 - Santiago de Compostela (Spain); Moreda-Pineiro, Jorge [Department of Analytical Chemistry, Faculty of Sciences, University of A Coruna, Campus da Zapateira, s/n. 15071, A Coruna (Spain); Moreda-Pineiro, Antonio, E-mail: antonio.moreda@usc.es [Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, University of Santiago de Compostela, Avenida das Ciencias, s/n. 15782 - Santiago de Compostela (Spain)

    2012-10-01

    Highlights: Black-Right-Pointing-Pointer Bioavailable iodine and bromine speciation in edible seaweed were developed. Black-Right-Pointing-Pointer In vitro dialyzability was used to assess the bioavailable fractions. Black-Right-Pointing-Pointer AEC hyphenated with inductively coupled plasma-mass spectrometry was used. Black-Right-Pointing-Pointer Iodide, MIT, DIT, bromide and bromate were found in dialyzates from edible seaweed. Black-Right-Pointing-Pointer Positive correlation between bioavailability and protein contents was found. - Abstract: A bioavailability study based on an in vitro dialyzability approach has been applied to assess the bio-available fractions of iodine and bromine species from edible seaweed. Iodide, iodate, 3-iodo-tyrosine (MIT), 3,5-diiodo-tyrosine (DIT), bromide and bromate were separated by anion exchange chromatography under a gradient elution mode (175 mM ammonium nitrate plus 15% (v/v) methanol, pH 3.8, as a mobile phase, and flow rates within the 0.5-1.5 mL min{sup -1} range). Inductively coupled plasma-mass spectrometry (ICP-MS) was used as a selective detector for iodine ({sup 127}I) and bromine ({sup 79}Br). Low dialyzability ratios (within the 2.0-18% range) were found for iodine species; whereas, moderate dialyzability percentages (from 9.0 to 40%) were obtained for bromine species. Iodide and bromide were the major species found in the dialyzates from seaweed, although MIT and bromate were also found in the dialyzates from most of the seaweed samples analysed. However, DIT was only found in dialyzates from Wakame, Kombu, and NIES 09 (Sargasso) certified reference material; whereas, iodate was not found in any dialyzate. Iodine dialyzability was found to be dependent on the protein content (negative correlation), and on the carbohydrate and dietary fibre levels (positive correlation). However, bromine dialyzability was only dependent on the protein amount in seaweed (negative correlation).

  11. Speciation of the bio-available iodine and bromine forms in edible seaweed by high performance liquid chromatography hyphenated with inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Highlights: ► Bioavailable iodine and bromine speciation in edible seaweed were developed. ► In vitro dialyzability was used to assess the bioavailable fractions. ► AEC hyphenated with inductively coupled plasma-mass spectrometry was used. ► Iodide, MIT, DIT, bromide and bromate were found in dialyzates from edible seaweed. ► Positive correlation between bioavailability and protein contents was found. - Abstract: A bioavailability study based on an in vitro dialyzability approach has been applied to assess the bio-available fractions of iodine and bromine species from edible seaweed. Iodide, iodate, 3-iodo-tyrosine (MIT), 3,5-diiodo-tyrosine (DIT), bromide and bromate were separated by anion exchange chromatography under a gradient elution mode (175 mM ammonium nitrate plus 15% (v/v) methanol, pH 3.8, as a mobile phase, and flow rates within the 0.5–1.5 mL min−1 range). Inductively coupled plasma-mass spectrometry (ICP-MS) was used as a selective detector for iodine (127I) and bromine (79Br). Low dialyzability ratios (within the 2.0–18% range) were found for iodine species; whereas, moderate dialyzability percentages (from 9.0 to 40%) were obtained for bromine species. Iodide and bromide were the major species found in the dialyzates from seaweed, although MIT and bromate were also found in the dialyzates from most of the seaweed samples analysed. However, DIT was only found in dialyzates from Wakame, Kombu, and NIES 09 (Sargasso) certified reference material; whereas, iodate was not found in any dialyzate. Iodine dialyzability was found to be dependent on the protein content (negative correlation), and on the carbohydrate and dietary fibre levels (positive correlation). However, bromine dialyzability was only dependent on the protein amount in seaweed (negative correlation).

  12. Speciation of Selenium in Selenium-Enriched Sunflower Oil by High-Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry/Electrospray-Orbitrap Tandem Mass Spectrometry.

    Science.gov (United States)

    Bierla, Katarzyna; Flis-Borsuk, Anna; Suchocki, Piotr; Szpunar, Joanna; Lobinski, Ryszard

    2016-06-22

    The reaction of sunflower oil with selenite produces a complex mixture of selenitriglycerides with antioxidant and anticancer properties. To obtain insight into the identity and characteristics of the species formed, an analytical approach based on the combination of high-performance liquid chromatography (HPLC) with (78)Se-specific selenium detection by inductively coupled plasma mass spectrometry (ICP MS) and high-resolution (100 000), high mass accuracy (oil dissolved in isopropanol and methanol extract of the oil containing 65% selenium. HPLC-ICP MS showed 14 peaks, 11 of which could also be detected in the methanol extract. Isotopic patterns corresponding to molecules with one or two selenium atoms could be attributed by Orbitrap MS at the retention times corresponding to the HPLC-ICP MS peak apexes. Structural data for these species were acquired by MS(2) and MS(3) fragmentation of protonated or sodiated ions using high-energy collisional dissociation (HCD). A total of 11 selenium-containing triglycerol derivatives resulting from the oxidation of one or two double bonds of linoleic acid and analogous derivatives of glycerol-mixed linoleate(s)/oleinate(s) have been identified for the first time. The presence of these species was confirmed by the targeted analysis in the total oil isopropanol solution. Their identification corroborated the predicted elution order in reversed-phase chromatography: LLL (glycerol trilinoleate), LLO (glycerol dilinoleate-oleinate), LOO (glycerol linoleate-dioleinate), OOO (glycerol trioleinate), of which the extrapolation allowed for the prediction of the identity [glycerol dioleinate-stearate (OOS) and glycerol oleinate-distearate (OSS)] of the nonpolar species detected by ICP MS in the oil but not detected by electrospray MS. PMID:27214173

  13. Simultaneous speciation and preconcentration of ultra trace concentrations of mercury and selenium species in environmental and biological samples by hollow fiber liquid phase microextraction prior to high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Moreno, F; García-Barrera, T; Gómez-Ariza, J L

    2013-07-26

    Nowadays, hollow fiber membrane extraction techniques are widely used due to the high enrichment factors obtained with many different types of analytes and samples. In this paper, we propose a new analytical method that allows the simultaneous extraction of methylmercury, inorganic mercury and Se(4+) and determination by high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry (HPLC-ICP-MS). The detection limits obtained are very low (110-230ng/L) with relative standard deviations below 15% for all the analytes and averaged recoveries in fortified samples in the range of 71-99%. The precision of the analytical method is very good which overcomes one of the most important shortcomings of membrane extraction techniques. Several variables were studied to get optimal extraction conditions for the analytes. This method has been validated with real world samples such as water (tap, river and estuarine) and human blood plasma. PMID:23541655

  14. Evaluation of microwave and ultrasound extraction procedures for arsenic speciation in bivalve mollusks by liquid chromatography-inductively coupled plasma-mass spectrometry

    Science.gov (United States)

    Santos, Clarissa M. M.; Nunes, Matheus A. G.; Barbosa, Isa S.; Santos, Gabriel L.; Peso-Aguiar, Marlene C.; Korn, Maria G. A.; Flores, Erico M. M.; Dressler, Valderi L.

    2013-08-01

    Liquid chromatography-inductively coupled plasma-mass spectrometry (LC-ICP-MS) was used for arsenic speciation analysis in tissues of bivalve mollusks (Anomalocardia brasiliana sp. and Macoma constricta sp.). Microwave and ultrasound radiation, combined with different extraction conditions (solvent, sample amount, time, and temperature), were evaluated for As-species extraction from the mollusks' tissues. Accuracy, extraction efficiency, and the stability of As species were evaluated by analyzing certified reference materials (DORM-2, dogfish muscle; BCR-627, tuna fish tissue; and SRM 1566b, oyster tissue) and analyte recovery tests. The best conditions were found to be microwave-assisted extraction using 200 mg of samples and water at 80 °C for 6 min. The agreement of As-species concentration in samples ranged from 97% to 102%. Arsenobetaine (AsB) was the main species present in bivalve mollusk tissues, while monomethylarsonic acid (MMA) and arsenate (As(V)) were below the limit of quantification (0.001 and 0.003 μg g- 1, respectively). Two unidentified As species also were detected and quantified. The sum of the As-species concentration was in agreement (90 to 104%), with the total As content determined by ICP-MS after sample digestion.

  15. Investigation of trialkoxysilane hydrolysis kinetics using liquid chromatography with inductively coupled plasma atomic emission spectrometric detection and non-linear regression modeling

    International Nuclear Information System (INIS)

    A novel approach is demonstrated for measuring rates of the consecutive acid-base catalyzed hydrolysis reactions of (3-glycidoxypropyl)trimethoxysilane (GPTMS) and (3-aminopropyl)triethoxysilane (APTES) in dilute aqueous solution using liquid chromatography with inductively coupled plasma atomic emission spectrometric (ICP-AES) detection. The hydrolysis reactions are monitored by sampling kinetic solutions in a timewise manner and performing liquid chromatographic separations of the parent silane and organosilicon hydrolysis products. The column effluent is fed into the ICP through a direct injection nebulizer for online monitoring of silicon atomic emission at 251.611 nm, producing a series of silicon chromatograms for each kinetic run. Reversed phase separations are effected using acetonitrile-water gradients and are complete in 6 min or less. The systematic changes in peak areas provide information from which the rate constants of the consecutive hydrolysis reactions (k1, k2, and k3) are obtained by non-linear regression modeling. Using a quenching scheme, hydrolysis half-lives as brief as 3 min for the parent silane can be monitored. For each compound, a series of rate constants are obtained over a range of pH and buffer concentration, permitting estimation of the catalytic constants kH3O+ and kOH- for the consecutive acid-base catalyzed hydrolysis reactions by multiple regression analysis

  16. Capillary gas chromatography inductively coupled plasma mass spectrometry (CGC-ICPMS) for the enantiomeric analysis of D,L-selenomethionine in food supplements and urine.

    Science.gov (United States)

    Devos, Christophe; Sandra, Koen; Sandra, Pat

    2002-01-15

    Capillary gas chromatography inductively coupled plasma mass spectrometry (CGC-ICPMS) was applied to the determination of D- and L-selenomethionine in food supplements and in urine. Derivatization was performed with ethylchloroformate (ECF) offering the advantage that the reaction can be carried out in aqueous medium i.e. urine. The derivatives were separated on the chiral stationary phase (CSP) Chiralsil-L-Val. The method was validated with D- and L-seleno-ethionine as internal standard (IS) and the linearity for a seven point calibration from 12.5 pg to 2.5 ng per enantiomer was excellent (R(2) 0.9997). Repeatability of injection (n=3) was market contain L-selenomethionine for at least 90%. Repeatability of the whole procedure (n=6) was tested on one L-selenomethionine formulation and was 3.8 (R.S.D.%). Data for urine samples after a daily intake of L-selenomethionine or the racemate D,L-selenomethionine corresponding to 100 microg selenium indicate that the D-enantiomer is not metabolized. PMID:11755752

  17. Determination of organophosphate flame retardants and plasticizers in sediment samples using microwave-assisted extraction and gas chromatography with inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    García-López, M; Rodríguez, I; Cela, R; Kroening, K K; Caruso, J A

    2009-08-15

    A procedure for the determination of 10 organophosphates, used as flame retardants and plasticizers, in sediment samples is presented. Microwave-assisted extraction (MAE) and gas chromatography with inductively coupled plasma mass spectrometry (GC-ICP-MS) were used for sample preparation and analytes determination, respectively. Influence of different variables on the performance of extraction and determination processes is thoroughly discussed. Temperature, type and amount of organic solvent showed a major effect on the yield of MAE. Regarding GC-ICP-MS detection, the combination of pulsed splitless injection with low radio frequency (rf) power, hard extraction conditions (referred to lens voltage) and addition of nitrogen (0.03 L min(-1)) to the argon plasma provided the best sensitivity. Under final working conditions, recoveries between 78% and 105%, for samples spiked at different concentration levels, and limits of quantification from 2 to 4 ng g(-1) were achieved. Analysis of unspiked sediments confirmed the excellent selectivity of the proposed method for real-life polluted sample analysis. PMID:19576451

  18. Determination of vanadium species in sediment, mussel and fish muscle tissue samples by liquid chromatography-inductively coupled plasma-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Colina, Marinela [Universidad del Zulia, Facultad de Ciencias, Departamento de Quimica, Laboratorio de Quimica Ambiental, Maracaibo 4011, Zulia (Venezuela)]. E-mail: M.Colina@shu.ac.uk; Gardiner, P.H.E. [Sheffield Hallam University, Howard Street, Sheffield S1 1WB, Sheffield (United Kingdom); Rivas, Zulay [Instituto para la Conservacion del Lago de Maracaibo (ICLAM), Maracaibo, Plaza de las Banderas (Venezuela); Troncone, Federico [Instituto para la Conservacion del Lago de Maracaibo (ICLAM), Maracaibo, Plaza de las Banderas (Venezuela)

    2005-05-04

    Vanadium is introduced into the environment during the extraction of petrochemical products and in the production of steels and insecticides. In this study, a liquid chromatographic method for the separation of V(IV) and V(V) as ethylenediaminetetra acetic acid (EDTA) complexes was developed using reversed-phase ion-pair liquid chromatography with inductively coupled plasma-mass spectrometry detection. A C-8 reversed-phase column, 15 cm long, was used to separate the species. A solution containing ammonium acetate 0.06 M, tetrabutylammonium hydroxide 10 mM, ammonium di-phosphate 10 mM and EDTA 2.5 mM at pH 6 was used as the mobile phase in order to avoid the use of organic solvents that reduce the sensitivity of the determination. To prevent changes in distribution of the vanadium species, samples should be prepared freshly. The method developed was applied to the study the vanadium speciation in sediment, mussel and fish muscle samples collected from Lake Maracaibo, Venezuela. The concentration ranges of V(IV) and V(V) in sediment samples were 0.7-61 and 1.4-2.3 {mu}g g{sup -1}, respectively. The method is simple and has adequate sensitivity for these practical applications.

  19. Fast determination of arsenosugars in algal extracts by narrow bore high-performance liquid chromatography-inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Todolí, José Luis; Grotti, Marco

    2010-11-19

    The potential of narrow bore high-performance liquid chromatography (HPLC) with detection by inductively coupled plasma mass spectrometry (ICP-MS) for fast determination of arsenosugars in algal extracts was explored. The retention behavior of four naturally occurring dimethylarsinoylribosides on an anion-exchange microbore column was investigated, with the mobile phase flow rate ranging from 60 to 200μLmin(-1). A low sample consumption system consisting of a micronebulizer and a low inner volume cyclonic spray chamber was used as the interface between the micro-column and the ICP mass spectrometer. Both the high efficiency nebulizer, HEN, and the PFA micronebulizer were tested, with the former providing 20-50% greater sensitivity than PFA (depending on the liquid flow rate), but comparable limits of detection and slightly lower chromatographic resolution. With the setup employed and under the optimal conditions, a satisfactory separation of the arsenosugars was achieved in less than 5min. The instrumental limit of detection was 0.20μgAsL(-1) and the precision was better than 3% (RSD%, n=5). The accuracy of the determination was verified by the analysis of a reference algal extract, obtaining values in good agreement with the reference ones. PMID:20965508

  20. Determination of La in U3Si/Al spent nuclear fuel by ion chromatography-inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Lanthanum has been used as one of the burnup monitor in spent nuclear fuel. U3Si/Al spent nuclear fuel contains small amount of La in high concentration of U and Al. Therefore, chemical separation of La is required to remove matrix elements. At first, ion chromatography (IC) and inductively coupled plasma systems were installed in radiation shielded glove box to handle the radioactive samples. Retention behavior of uranium, aluminum, lanthanum and some interesting fission products (Sr, Zr, Y, Mo, Ru, Pd, Rh, Cs, Ba, Ce, Pr, Nd, Sm, Eu, and Gd) was investigated using the CG10 column and α-HiBA eluent. As all elements were eluted earlier than lanthanum in 0.2 M α-HiBA eluent, a portion of U and Al was directly passed to waste using a three way valve between the column and the nebulizer. Thus it was possible to determine the lanthanum in a high concentration of U and Al matrix. Retention time of La was about 12 minutes in this separation condition. Optimum range for the determination of La in U3Si/Al spent nuclear fuel was 1-10 μg/L(ppb) with this system and detection limit was 0.25 μg/L in case of 200 μL of sample volume. (author)

  1. Mercury speciation analysis in sea water by solid phase microextraction?gas chromatography?inductively coupled plasma mass spectrometry using ethyl and propyl derivatization. Matrix effects evaluation

    Science.gov (United States)

    Bravo-Sánchez, Luis R.; Ruiz Encinar, Jorge; Fidalgo Martínez, José I.; Sanz-Medel, Alfredo

    2004-01-01

    An approach to the speciation analysis of mercury in sea-water samples at sub-ppt levels by means of the hyphenation of solid phase microextraction to gas chromatography-inductively coupled plasma mass spectrometry was developed. Blank values turned out to be the limiting factor for lower detection limits of inorganic mercury. Thus, all the reagents were thoroughly cleaned using laboratory made microcolumns packed with 8-hydroxyquinoline on TSK gel. Sodium tetrapropylborate (NaBPr 4) synthesized for the purpose of derivatization of the mercury species resulted in better analytical performances of the method, probably due to lower mercury contamination, than commercial sodium tetraethylborate (NaBEt 4). Detection limits down to a few picogram per liter for both mercury and methylmercury were obtained using NaBPr 4. The high salt content of sea-water samples was responsible for strong matrix effects, which were overcome by using standards additions to the samples. The validation of the methodology was carried out by direct comparison of the results for inorganic mercury with those obtained using a flow injection system followed by preconcentration/trapping of the species and its detection by atomic absorption spectrometry. The proposed method was applied to the determination of mercury and methylmercury in coastal sea-water samples from Gijón (Asturias, Spain) and results obtained are discussed in the light of the butyltin levels previously determined in the same area.

  2. Rapid speciation and determination of vanadium compounds using ion-pair reversed-phase ultra-high-performance liquid chromatography inductively coupled plasma-sector field mass spectrometry.

    Science.gov (United States)

    Kilibarda, Nikola; Afton, Scott E; Harrington, James M; Yan, Fei; Levine, Keith E

    2013-08-23

    Environmental vanadium contamination is a potential concern to public health, as evidenced by its place on the U.S. Environmental Protection Agency Drinking Water Contaminant Candidate List as a priority contaminant. Vanadium toxicity varies significantly between different oxidation states; therefore, it is crucial to be able to monitor the speciation of vanadium in environmental samples. In this study, a novel method is described that utilizes ion-pair reversed-phase ultra-high-performance liquid chromatography with inductively coupled plasma-sector field mass spectrometry (IP-RP-UHPLC-ICP-SFMS) to separate vanadyl and vanadate ions and resolve a major polyatomic spectral interference ((35)Cl(16)O(+)) in less than a minute. Detection limits were obtained in the low ngL(-1) (part per trillion) range with linear calibrations across several orders of magnitude (50ngL(-1)-100μgL(-1)). The mechanism of chromatographic retention was elucidated through investigation of the role of ethylenediaminetetraacetic acid, tetrabutylammonium ion and pH on elution. The optimized method was then applied to the speciation of vanadium in local lake water samples. PMID:23871564

  3. Arsenic Species in Edible Seaweeds Using In Vitro Biomimetic Digestion Determined by High-Performance Liquid Chromatography Inductively Coupled Plasma Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Yan-Fang Zhao

    2014-01-01

    Full Text Available Arsenite [As (III], arsenate [As (V], methylarsonate (MMA, and dimethylarsinate (DMA in five edible seaweeds (the brown algae Laminaria japonica, red algae Porphyra yezoensis, brown algae Undaria pinnatifida, brown algae Hizikia fusiformis, and green algae Enteromorpha prolifera were analyzed using in vitro digestion method determined by high-performance liquid chromatography inductively coupled plasma mass spectrometry. The results showed that DMA was found in the water extracts of all samples; As (III were detected in L. japonica and U. pinnatifida and about 23.0 and 0.15 mg/kg of As (V were found in H. fusiformis and E. prolifera respectively. However, after the gastrointestinal digestion, As (V was not detected in any of the five seaweeds. About 0.19 and 1.47 mg/kg of As (III was detected in the gastric extracts of L. japonica and H. fusiformis, respectively, and about 0.31 and 0.10 mg/kg of As (III were extracted from the intestinal extracts of Porphyra yezoensis and U. pinnatifida, respectively. The present results successfully reveal the differences of As species and levels in the water and biomimetic extracts of five edible seaweeds. The risk assessment of the inorganic arsenic in the five edible seaweeds based on present data showed almost no hazards to human health.

  4. Simultaneous determination of arsenic and mercury species in rice by ion-pairing reversed phase chromatography with inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Fang, Yong; Pan, Yushi; Li, Peng; Xue, Mei; Pei, Fei; Yang, Wenjian; Ma, Ning; Hu, Qiuhui

    2016-12-15

    An analytical method using reversed phase chromatography-inductively coupled plasma mass spectrometry for arsenic and mercury speciation analysis was described. The effect of ion-pairing reagent on simultaneous separation of four arsenic (arsenite, arsenate, monomethlyarsonate and dimethylarsinate) and three mercury species (inorganic mercury (Hg(II)), methylmecury and ethylmercury) was investigated. Parameters including concentrations and pH of the mobile phase were optimized. The separation and re-equilibration time was attained within 20min. Meanwhile, a sequential extraction method for arsenic and mercury in rice was tested. Subsequently, 1% HNO3 microwave-assisted extraction was chosen. Calibration curves based on peak area measurements were linear with correlation coefficient greater than 0.9958 for each species in the range studied. The detection limits of the species were in the range of 0.84-2.41μg/L for arsenic and 0.01-0.04μg/L for mercury, respectively. The proposed method was then successfully applied for the simultaneous determination of arsenic and mercury species in rice flour standard material and two kinds of rice from local markets. PMID:27451225

  5. Method optimization and quality assurance in speciation analysis using high performance liquid chromatography with detection by inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Larsen, Erik H.

    1998-02-01

    Achievement of optimum selectivity, sensitivity and robustness in speciation analysis using high performance liquid chromatography (HPLC) with inductively coupled mass spectrometry (ICP-MS) detection requires that each instrumental component is selected and optimized with a view to the ideal operating characteristics of the entire hyphenated system. An isocratic HPLC system, which employs an aqueous mobile phase with organic buffer constituents, is well suited for introduction into the ICP-MS because of the stability of the detector response and high degree of analyte sensitivity attained. Anion and cation exchange HPLC systems, which meet these requirements, were used for the seperation of selenium and arsenic species in crude extracts of biological samples. Furthermore, the signal-to-noise ratios obtained for these incompletely ionized elements in the argon ICP were further enhanced by a factor of four by continously introducing carbon as methanol via the mobile phase into the ICP. Sources of error in the HPLC system (column overload), in the sample introduction system (memory by organic solvents) and in the ICP-MS (spectroscopic interferences) and their prevention are also discussed. The optimized anion and cation exchange HPLC-ICP-MS systems were used for arsenic speciation in contaminated ground water and in an in-house shrimp reference sample. For the purpose of verification, HPLC coupled with tandem mass spectrometry with electrospray ionization was additionally used for arsenic speciation in the shrimp sample. With this analytical technique the HPLC retention time in combination with mass analysis of the molecular ions and their collision-induced fragments provide almost conclusive evidence of the identity of the analyte species. The speciation methods are validated by establishing a mass balance of the analytes in each fraction of the extraction procedure, by recovery of spikes and by employing and comparing independent techniques. The urgent need for

  6. Report on three aliphatic dimethylarsinoyl compounds as common minor constituents in marine samples. An investigation using high-performance liquid chromatography inductively coupled plasma mass spectrometry and electrospray ionisation tandem mass spectrometry

    DEFF Research Database (Denmark)

    Sloth, Jens Jørgen; Larsen, Erik Huusfeldt; Julshamn, K.

    2005-01-01

    chromatography/inductively coupled plasma mass spectrometry (HPLC/ICPMS). Eluate fractions from the HPLC/ICPMS analyses containing the compounds in question were collected and subjected to analysis by electrospray ionisation tandem mass spectrometry (ESI-MS/MS), which provided supportive evidence for the...... DMAA and DMAE supports a proposed biosynthesis of arsenobetaine (AB) from dimethylarsinoylribosides. Alternative proposals, which explain the presence of the compounds in marine samples, are addressed briefly in the paper....

  7. Speciation of four selenium compounds using high performance liquid chromatography with on-line detection by inductively coupled plasma mass spectrometry or flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Pedersen, G.A. [National Food Agency of Denmark, Institute of Food Chemistry and Nutrition, Moerkhoej Bygade 19, DK-2860 Soeborg (Denmark); Larsen, E.H. [National Food Agency of Denmark, Institute of Food Chemistry and Nutrition, Moerkhoej Bygade 19, DK-2860 Soeborg (Denmark)

    1997-07-01

    An analytical method for the speciation of selenomethionine, selenocystine, selenite and selenate by high performance liquid chromatography (HPLC) with atomic spectrometric detection is presented. An organic polymeric strong anion exchange column was used as the stationary phase in combination with an aqueous solution of 6 mmol L{sup -1} of salicylate ion at pH 8.5 as the mobile phase which allowed the isocratic separation of the four selenium analytes within 8 minutes. The separated selenium species were detected on-line by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma mass spectrometry (ICP-MS). The signal-to-noise ratio of the FAAS detector was optimized using a hydrogen-argon entrained-air flame and a slotted-tube atom trap (STAT) in the flame. The limit of detection (3 {sigma}) achieved by the HPLC-FAAS system was 1 mg L{sup -1} of selenium (100 {mu}L injections) for each of the four selenium species. More powerful selenium detection was achieved using an ELAN 5000 ICP-MS instrument. Selenium was measured at m/z = 82. The ICP-MS signal intensity was enhanced by a factor of 3-4 after addition of 3% methanol to the chromatographic mobile phase and by using an increased plasma power input of 1300 W. The limit of detection achieved under these conditions was 1 {mu}g L{sup -1} (100 {mu}L injections). The HPLC-ICP-MS system was used for selenium speciation of selenite and selenate in aqueous solutions during a BCR certification exercise and for selenium speciation in the certified reference material, BCR No. 402 White Clover. Extraction experiments revealed that the selenium species in the biological material were extractable only in the presence of water in the extraction medium. The results indicated that selenate and a compound of unknown identity U were present in the plant sample. (orig.). With 5 figs., 5 tabs.

  8. Separation and determination of seleno amino acids using gas chromatography hyphenated with inductively coupled plasma mass spectrometry after hollow fiber liquid phase microextraction.

    Science.gov (United States)

    Duan, Jiankun; Hu, Bin

    2009-05-01

    A new derivatization-extraction method for preconcentration of seleno amino acids using hollow fiber liquid phase microextraction (HF-LPME) was developed for the separation and determination of seleno amino acids in biological samples by gas chromatography-inductively coupled plasma mass spectrometry (GC-ICP-MS). Derivatization was performed with ethyl chloroformate (ECF) to improve the volatility of seleno amino acids. Parameters influencing microextraction, including extraction solvent, pH of sample solution, extraction time, stirring speed, and inorganic salt concentration have been investigated. Under the optimal conditions, the limits of detection (LODs) obtained for Se-methyl-selenocysteine (SeMeCys), selenomethionine (SeMet), and selenoethionine (SeEth) were 23, 15, and 11 ng Se l(-1), respectively. The relative standard deviations (RSDs) were 14.6%, 16.4%, and 19.4% for SeMeCys, SeMet, and SeEth (c = 1.0 ng ml(-1), n = 7), respectively, and the RSDs for SeMeCys, SeMet could be improved obviously if SeEth was utilized as the internal standard. The proposed method was applied for the determination of seleno amino acids in extracts of garlic, cabbage, and mushroom samples, and the recoveries for the spiked samples were in the range of 96.8-108% and 93.4-115% with and without the use of SeEth as internal standard. The developed method was also applied to the analysis of SeMet in a certified reference material of SELM-1 yeast and the determined value is in good agreement with the certified value. PMID:19053158

  9. Determination of butyl-, phenyl-, octyl- and tributylmonomethyltin compounds in a marine environment (Bay of Bengal, India) using gas chromatography-inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Rajendran, R B; Tao, H; Miyazaki, A; Ramesh, R; Ramachandran, S

    2001-12-01

    Organotin compounds (butyl-, phenyl-, octyl- and tributylmonomethyltin) and inorganic tin were quantified in sea-water and sediments from two harbours and several locations on the southeast coast of India using highly sensitive and selective gas chromatography-inductively coupled plasma mass spectrometry (GC-ICP-MS), adopting new extraction and analytical techniques with extremely low detection limits (water, 0.019-0.85 pg l(-1); sediment, 0.23-0.48 ng g(-1)). The concentrations of monobutyltin (MBT), dibutyltin (DBT) and tributyltin (TBT) in sea-water from Tuticorin harbour varied from 0.64 to 4.97, 3.0 to 26.8 and 0.3 to 30.4 ng Sn l(-1), respectively. MBT, DBT and TBT in sediments from harbour areas ranged from 1.6 to 393, 1.3 to 394 and ND (not detected) to 1280 ng Sn g(-1) (dry weight), respectively. Natural methylation in both harbours was established by quantifying tributylmonomethyltin (TBMMT) residues (sea-water, ND-0.19 ng Sn l(-1); sediment, ND-765 ng Sn g(-1) dry weight). In sea-water, octyltins were also determined as monooctyltin (MOT) > dioctyltin (DOT) > trioctyltin (TOT). Butyltin contamination in commercial harbours is evident, but other coastal waters are not contaminated with organotin residues. The high concentration of inorganic tin in estuarine sediment indicates an elevated rate of debutylation in the estuarine environment. Both methylation and debutylation of TBT in Chennai harbour were greater than in Tuticorin harbour. A significant correlation (r2 = 0.75) between total butyltin and organic carbon contents in sediment was found. To our knowledge, this is the first report on the distribution of butyltins and methylated butyltin in sea-water and sediment and octyltins in sea-water in the Indian marine environment. PMID:11785637

  10. Analytical developments for the determination of monomethylmercury complexes with low molecular mass thiols by reverse phase liquid chromatography hyphenated to inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Bouchet, Sylvain; Björn, Erik

    2014-04-25

    The behavior of monomethylmercury (MMHg) is markedly influenced by its distribution among complexes with low molecular mass (LMM) thiols but analytical methodologies dedicated to measure such complexes are very scarce up to date. In this work, we selected 15 LMM thiols often encountered in living organisms and/or in the environment and evaluated the separation of the 15 corresponding MMHg-thiol complexes by various high performance liquid chromatography (HPLC) columns. Two C18 (Phenomenex Synergi Hydro-RP and LunaC18(2)), two phenyl (Inertsil Ph 3 and 5μm) and one mixed-mode (Restek Ultra IBD) stationary phases were tested for their retention and resolution capacities of the various complexes. The objective was to find simple separation conditions with low organic contents in the mobile phase to provide optimal conditions for detection by inductively coupled plasma mass spectrometry (ICPMS). The 15 complexes were synthesized in solution and characterized by electrospray ionization-mass spectrometry (ESI-MS). The C18 columns tested were either not resolutive enough or too retentive. The 3μm phenyl stationary phase was able to resolve 10 out of the 15 complexes in less than 25min, under isocratic conditions. The mixed-mode column was especially effective at separating the most hydrophilic complexes (6 complexes out of the 15), corresponding to the main LMM thiols found in living organisms. The detection limits (DLs) for these two columns were in the low nanomolar range and overall slightly better for the phenyl column. The possibilities offered by such methodology were exemplified by monitoring the time-course concentrations of four MMHg-thiol complexes within a phytoplankton incubation containing MMHg in the presence of an excess of four added thiols. PMID:24657146

  11. Rapid determination of plutonium isotopes in environmental samples using sequential injection extraction chromatography and detection by inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per; Miró, Manuel

    2009-10-01

    This article presents an automated method for the rapid determination of 239Pu and 240Pu in various environmental samples. The analytical method involves the in-line separation of Pu isotopes using extraction chromatography (TEVA) implemented in a sequential injection (SI) network followed by detection of isolated analytes with inductively coupled plasma mass spectrometry (ICP-MS). The method has been devised for the determination of Pu isotopes at environmentally relevant concentrations, whereby it has been successfully applied to the analyses of large volumes/amounts of samples, for example, 100-200 g of soil and sediment, 20 g of seaweed, and 200 L of seawater following analyte preconcentration. The investigation of the separation capability of the assembled SI system revealed that up to 200 g of soil or sediment can be treated using a column containing about 0.70 g of TEVA resin. The analytical results of Pu isotopes in the reference materials showed good agreement with the certified or reference values at the 0.05 significance level. Chemical yields of Pu ranged from 80 to 105%, and the decontamination factors for uranium, thorium, mercury and lead were all above 10(4). The duration of the in-line extraction chromatographic run was <1.5 h, and the proposed setup was able to handle up to 20 samples (14 mL each) in a fully automated mode using a single chromatographic column. The SI manifold is thus suitable for rapid and automated determination of Pu isotopes in environmental risk assessment and emergency preparedness scenarios. PMID:19722516

  12. Compensation of gradient related effects when using capillary liquid chromatography and inductively coupled plasma mass spectrometry for the absolute quantification of phosphorylated peptides.

    Science.gov (United States)

    Pröfrock, Daniel; Prange, Andreas

    2009-09-25

    The application of reversed phase liquid chromatography (RP-LC) hyphenated to inductively coupled plasma mass spectrometry (ICP-MS) for the accurate quantification of bio-molecules via covalently bound hetero atoms such as phosphorus is restricted, due to the known effects of increasing amounts of organic solvents on the ionization behavior of certain elements. An approach for the compensation of variations in the elemental response, due to changes in the solvent composition during the RP gradient separation of phosphorylated peptides is described, which includes the application of a second, matched reversed gradient, that is mixed post-column with the RP column outflow before entering the LC-ICP-MS interface. The experimental design allows the application of gradient separations, while the element-specific detection is carried out under isocratic conditions with a constant organic solvent intake into the plasma. A constant elemental response is a general pre-requisite for the application of ICP-MS for the absolute quantification of peptides via their hetero atom content, especially when no corresponding high purity standards are available or natural mono-isotopic hetero element tags are utilized. As complementary technique LC-electrospray ionization linear ion trap mass spectrometry (ESI-QTRAP-MS) has been used for peptide identification and to elucidate their phosphorus stoichiometry. Highly reproducible separations have been obtained with retention time and peak area RSDs of 0.05% and 7.6% (n=6), respectively. Detection limits for phosphorus of 6 microg L(-1) (6 pg absolute), have been realized, which corresponds to approximately 200 fmol of an average molecular weight, singly phosphorylated peptide. In addition an automatic routine for flow injection analysis (FIA) at the end of each chromatographic separation has been developed, to calibrate each chromatographic separation, which allows absolute quantification of the separated species, whenever their tag

  13. Measurement of isotopic composition of lanthanides in reprocessing process solutions by high-performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC/ICP-MS)

    International Nuclear Information System (INIS)

    Isotopic compositions of fission products in process solutions and wastes in a reprocessing plant are valuable to proceed safety study of the solutions and research/development concerning treatment/disposal of the wastes. The amount of neodymium-148 is a reliable indication to evaluate irradiation history. The isotopic compositions of samarium and gadolinium in high radioactive wastes are referred to as essential data to evaluate environmental impact in geological repositories. However, pretreatment of analysis must be done with complicated chemical separation such as solvent extraction and ion exchange. The actual measurement data of isotopic compositions of lanthanides comparable to the one of actinides in spent fuel reprocessing process has not been obtained enough. Rapid and high sensitive analytical technique based on high-performance liquid chromatography (HPLC) with an inductively coupled plasma mass spectrometry (ICP-MS) has been developed for the measurement of isotopic compositions of lanthanides in spent fuel reprocessing solutions. HPLC/ICP-MS measurement system was customized for a glove-box to be applied to the radioactive solutions. The cation exchange chromatographic columns (Shim-pack IC-C1) and injection valve (20μL) were located inside of the glove-box except the chromatographic pump. The elements of lanthanide group were separated by a gradient program of HPLC with α-hydroxyisobutyric acid. Isotopic compositions of lanthanides in eluate was sequentially analyzed by a quadruple ICP-MS. Optimization of parameter of HPLC and ICP-MS measurement system was examined with standard solutions containing 14 lanthanide elements. The elements of lanthanides were separated by HPLC and detected by ICP-MS within 25 minutes. The detection limits of Nd-146, Sm-147 and Gd-157 were 0.37 μg L-1, 0.69 μg L-1 and 0.47 μg L-1, respectively. The analytical precision of the above three isotopes was better than 10% for standard solutions of 100 μg L-1 with five

  14. A quantitative extraction method for the determination of trace amounts of both butyl- and phenyltin compounds in sediments by gas chromatography-inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Rajendran, R B; Tao, H; Nakazato, T; Miyazaki, A

    2000-10-01

    A simple and reliable extraction method was developed for quantitative determination of both butyl- and phenyltin compounds in sediments by capillary gas chromatography combined with inductively coupled plasma mass spectrometry (GC-ICP-MS). Both types of organotin compounds were extracted quantitatively from sediment by mechanical shaking into tropolone-toluene and HCl-methanol. After phase separation and pH adjustment, these organotins were ethylated with sodium tetraethylborate. The method was evaluated by analyzing PACS-2 and NIES No. 12 sediment certified reference materials. The dibutyltin (DBT; 1.14 +/- 0.02 micrograms g-1) and tributyltin (TBT; 1.01 +/- 0.04 micrograms g-1) values observed in PACS-2 sediment closely matched the certified values (DBT, 1.09 +/- 0.15; TBT, 0.98 +/- 0.13 microgram g-1 as tin). The monobutyltin (MBT) value was higher (0.62 +/- 0.02 microgram g-1) by more than two fold over the reference value (0.3 microgram g-1 as tin). The concentrations of TBT (0.18 +/- 0.04 microgram g-1) and triphenyltin (TPhT; 0.0099 +/- 0.002 microgram g-1) in the NIES No. 12 sediment were also in good agreement with the certified and reference values of TBT (0.19 +/- 0.03 microgram g-1 as compound) and TPhT (0.008 microgram g-1 as compound), respectively. Recoveries of TBT, tripentyltin (TPeT) and TPhT from spiked sediments were satisfactory (TBT, 102 +/- 3.4%; TPrT, 96 +/- 3.4%; TPhT, 99 +/- 8.5%). The detection limits as tin were in the range 0.23-0.48 ng g-1 for a 0.5 g sample size. It is also noteworthy that clean-up of the extract is not necessary because of the superior selectivity of ICP-MS detection. The present method was successfully applied to marine sediment samples. PMID:11070544

  15. Determination of thorium and light rare-earth elements in soil water and its high molecular mass organic fractions by inductively coupled plasma mass spectrometry and on-line-coupled size-exclusion chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Casartelli, Evelton A. [Universidade Federal Rural do Rio de Janeiro (UFFRJ), BR 465 km 7, 23851-970, Seropedica, RJ (Brazil); Miekeley, Norbert [Pontificia Universidade Catolica (PUC-Rio), Rua Marques de Sao Vicente 225, 22453-900, Rio de Janeiro (Brazil)

    2003-09-01

    Inductively coupled plasma mass spectrometry (ICP-MS) has been used for the determination of thorium and light rare-earth elements (LREEs) in soil and soil water samples from a mineral deposit (Morro do Ferro, Minas Gerais, Brazil). Size-exclusion chromatography (SEC) on-line coupled to ICP-MS and UV-detection was applied to verify possible association/complexation of these elements with organic matter in soil water separated by a centrifugation technique. Concentrations of DOC in soil waters are in the range of 10 to 500 mg L{sup -1} and correlate with the organic carbon content of the soil (r=0.950; p<0.001). Concentrations of 30 to 40 {mu}g L{sup -1} for the LREEs (La, Ce, Nd) and up to 14 {mu}g L{sup -1} for Th were measured in soil waters of highest DOC content. SEC chromatograms of these waters showed the association of elements with different nominal high-molecular-mass ranges, characteristic of soil humic and fulvic acids: >10,000 Da, with a retention time of about 10 min; 7000 to 8000 Da with retention times of 13 to 15 min; and 2000 to 4000 Da with retention times around 23 min. Elemental peaks associated with dissolved organic matter below 1000 Da were not observed, suggesting that complexation with simple plant organic acids or inorganic ligands is of minor importance in the environment studied in this work. (orig.)

  16. Determination of thorium and light rare-earth elements in soil water and its high molecular mass organic fractions by inductively coupled plasma mass spectrometry and on-line-coupled size-exclusion chromatography

    International Nuclear Information System (INIS)

    Inductively coupled plasma mass spectrometry (ICP-MS) has been used for the determination of thorium and light rare-earth elements (LREEs) in soil and soil water samples from a mineral deposit (Morro do Ferro, Minas Gerais, Brazil). Size-exclusion chromatography (SEC) on-line coupled to ICP-MS and UV-detection was applied to verify possible association/complexation of these elements with organic matter in soil water separated by a centrifugation technique. Concentrations of DOC in soil waters are in the range of 10 to 500 mg L-1 and correlate with the organic carbon content of the soil (r=0.950; p-1 for the LREEs (La, Ce, Nd) and up to 14 μg L-1 for Th were measured in soil waters of highest DOC content. SEC chromatograms of these waters showed the association of elements with different nominal high-molecular-mass ranges, characteristic of soil humic and fulvic acids: >10,000 Da, with a retention time of about 10 min; 7000 to 8000 Da with retention times of 13 to 15 min; and 2000 to 4000 Da with retention times around 23 min. Elemental peaks associated with dissolved organic matter below 1000 Da were not observed, suggesting that complexation with simple plant organic acids or inorganic ligands is of minor importance in the environment studied in this work. (orig.)

  17. Total zinc quantification by inductively coupled plasma-mass spectrometry and its speciation by size exclusion chromatography-inductively coupled plasma-mass spectrometry in human milk and commercial formulas: Importance in infant nutrition.

    Science.gov (United States)

    Fernández-Menéndez, Sonia; Fernández-Sánchez, María L; Fernández-Colomer, Belén; de la Flor St Remy, Rafael R; Cotallo, Gil Daniel Coto; Freire, Aline Soares; Braz, Bernardo Ferreira; Santelli, Ricardo Erthal; Sanz-Medel, Alfredo

    2016-01-01

    This paper summarises results of zinc content and its speciation in human milk from mothers of preterm and full-term infants at different stages of lactation and from synthetic formula milks. Human milk samples (colostrum, 7th, 14th, and 28th day after delivery) from Spanish and Brazilian mothers of preterm and full-term infants (and also formula milks) were collected. After adequate treatment of the sample, total Zn was determined, while speciation analysis of the Zn was accomplished by size exclusion chromatography coupled online with the ICP-MS. It is observed that total zinc content in human milk decreases continuously during the first month of lactation, both for preterm and full term gestations. All infant formulas analysed for total Zn were within the currently legislated levels. For Zn speciation analysis, there were no differences between preterm and full term human milk samples. Moreover Zn species elute mainly associated with immunoglobulins and citrate in human milk whey. Interestingly the speciation in formula milk whey turned out to be completely different as the observed Zn(2+) was bound almost exclusively to low molecular weight ligands (citrate) and only comparatively very low amounts of the metal appeared to be associated with higher mass biomolecules (e.g. proteins). PMID:26381570

  18. Investigation of metallodrug-protein interactions by size-exclusion chromatography coupled with inductively coupled plasma mass spectrometry (ICP-MS)

    Energy Technology Data Exchange (ETDEWEB)

    Szpunar, J.; Makarov, A. [CNRS, EP132, Helioparc 2, av. Pr. Angot, 64000 Pau (France); Pieper, T.; Keppler, B.K. [Institute of Inorganic Chemistry, University of Vienna, Waehringerstr. 42, A-1090 Vienna (Austria); Lobinski, R. [CNRS, EP132, Helioparc 2, av. Pr. Angot, 64000 Pau (France)

    1999-04-22

    The coupling of size-exclusion HPLC with ICP-MS was developed for the studies of the kinetics of metallodrug binding to human serum proteins. Two platinum- and three ruthenium-based drugs were investigated. Various SEC columns (of different lengths and with different packings) were compared for the separation of the protein-bound and unbound fractions of a metallodrug prior to on-line detection of the metal (Ru or Pt). The approach developed offers considerable advantages over the methods based on ultrafiltration followed by the off-line metal determination in terms of speed, simplicity, precision and selectivity regarding the molecular weight of the complexes involved. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  19. Investigation of metallodrug-protein interactions by size-exclusion chromatography coupled with inductively coupled plasma mass spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    The coupling of size-exclusion HPLC with ICP-MS was developed for the studies of the kinetics of metallodrug binding to human serum proteins. Two platinum- and three ruthenium-based drugs were investigated. Various SEC columns (of different lengths and with different packings) were compared for the separation of the protein-bound and unbound fractions of a metallodrug prior to on-line detection of the metal (Ru or Pt). The approach developed offers considerable advantages over the methods based on ultrafiltration followed by the off-line metal determination in terms of speed, simplicity, precision and selectivity regarding the molecular weight of the complexes involved. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  20. Report on three aliphatic dimethylarsinoyl compounds as common minor constituents in marine samples. An investigation using high-performance liquid chromatography inductively coupled plasma mass spectrometry and electrospray ionisation tandem mass spectrometry

    DEFF Research Database (Denmark)

    Sloth, Jens Jørgen; Larsen, Erik Huusfeldt; Julshamn, K.

    2005-01-01

    chromatography/inductively coupled plasma mass spectrometry (HPLC/ICPMS). Eluate fractions from the HPLC/ICPMS analyses containing the compounds in question were collected and subjected to analysis by electrospray ionisation tandem mass spectrometry (ESI-MS/MS), which provided supportive evidence for the...... of the 37 samples analysed, respectively. The limits of detection were 2-3 mug kg(-1) dry mass. The data illustrate that the three compounds are common minor constituents in marine samples. This is the first report on DMAE and DMAP as naturally occurring species in marine samples. The presence of...

  1. An Investigation on the Extraction and Quantitation of a Hexavalent Chromium in Acrylonitrile Butadiene Styrene Copolymer (ABS) and Printed Circuit Board (PCB) by Ion Chromatography Coupled with Inductively Coupled Plasma Atomic Emission Spectrometry

    International Nuclear Information System (INIS)

    A hexavalent chromium (Cr (VI)) is one of the hazardous substances regulated by the RoHS. The determination of Cr (VI) in various polymers and printed circuit board (PCB) has been very important. In this study, the three different analytical methods were investigated for the determination of a hexavalent chromium in Acrylonitrile Butadiene Styrene copolymer (ABS) and PCB. The results by three analytical methods were obtained and compared. An analytical method by UV-Visible spectrometer has been generally used for the determination of Cr (VI) in a sample, but a hexavalent chromium should complex with diphenylcarbazide for the detection in the method. The complexation did make an adverse effect on the quantitative analysis of Cr (VI) in ABS. The analytical method using diphenylcarbazide was also not applicable to printed circuit board (PCB) because PCB contained lots of irons. The irons interfered with the analysis of hexavalent chromium because those also could complex with diphenylcarbazide. In this study, hexavalent chromiums in PCB have been separated by ion chromatography (IC), then directly and selectively detected by inductively coupled plasma atomic emission spectrometry (ICP-AES). The quantity of Cr (VI) in PCB was 0.1 mg/kg

  2. Stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet/inductively coupled plasma mass spectrometry for analysis of thyroxine in urine samples.

    Science.gov (United States)

    Fan, Wenying; Mao, Xiangju; He, Man; Chen, Beibei; Hu, Bin

    2013-11-29

    tIn this work, polyethyleneglycol (PEG)/hydroxyl polydimethylsiloxane (OH-PDMS)/γ -mercaptopropyltrimethoxysilane (γ -MPTS) coated stir bar was prepared by sol–gel process and its extraction performance for the extraction of amphoteric thyroxines (3,3',5,5'-tetraiodothyronin, T(4); 3,3',5-triiodothyronine, T(3); reversed-3,3',5-triiodothyronine, rT(3)) and their metabolite (3,5-diiodothyronine,T2) was studied. The preparation reproducibility of PEG/OH-PDMS/γ -MPTS coated stir bar was investigated, and the relative standard deviations (RSDs) in the same batch and among different batches were 3.3–14.3% (n = 5) and 7.7–16.6% (n = 3), respectively. The prepared PEG/OH-PDMS/γ -MPTS coated stir bar could be reused for more than 20 times. Based on this fact, a novel method of stir bar sorptive extraction (SBSE) combined with high performance liquid chromatography (HPLC)-ultraviolet (UV)and HPLC-inductively coupled plasma mass spectrometry (ICP-MS) for the analysis of target thyroxinesin human urine samples was developed. The influencing factors of SBSE, such as sample pH, extraction time, stirring rate, salt effect, desorption solution and desorption time, were studied in detail, and the analytical performance of the proposed method was evaluated under the optimized conditions. The enrichment factors (EFs) of the developed method for four target thyroxines were in the range of 14.9–70.4(theoretical enrichment factor was 100). The RSDs were ranging from 4.0% to 13.8% for SBSE-HPLC-UV (c = 25 μg/L, n = 6) and from 3.7% to 6.1% for SBSE-HPLC-ICP-MS (c = 0.5 μg/L, n = 5). The linear range obtained by SBSE-HPLC-UV was 2–500 μg/L for T(2)and 5–500 μg/L for rT3, T(3)and T(4), with correlation coefficients (r) ranging from 0.9957 to 0.9998, respectively, while the linear range obtained by SBSE-HPLC-ICP-MS was 0.05–500 μg/L for T(2) and rT(3), 0.10–200 μg/L for T(3) and 0.05–200 μg/L for T(4)with r ranging from 0.9979 to 0.9998, respectively. The

  3. Bead Injection Extraction Chromatography using High-capacity Lab-on-Valve as a Front End to Inductively Coupled Plasma Mass Spectrometry for Rapid Urine Radiobioassay

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per;

    2013-01-01

    A novel bead injection (BI) extraction chromatographic microflow system exploiting high-capacity lab-on-valve (LOV) platform coupled with inductively coupled plasma mass spectrometric detection is developed for rapid and automated determination of plutonium in human urine. A microconduit (1 m......L) incorporated within the LOV processing unit is loaded on-line with a metered amount of disposable extraction chromatographic resin (up to 330 mg of TEVA) through programmable beads transport. Selective capture and purification of plutonium onto the resin beads is then performed by pressure driven flow after.......319 ± 0.004 g, n=5). The chemical yields of plutonium were averagely better than 90% under the optimal experimental conditions and the entire analytical procedure could be accomplished within a short timeframe (

  4. Investigation into the determination of trimethylarsine in natural gas and its partitioning into gas and condensate phases using (cryotrapping)/gas chromatography coupled to inductively coupled plasma mass spectrometry and liquid/solid sorption techniques

    Science.gov (United States)

    Krupp, E. M.; Johnson, C.; Rechsteiner, C.; Moir, M.; Leong, D.; Feldmann, J.

    2007-09-01

    Speciation of trialkylated arsenic compunds in natural gas, pressurized and stable condensate samples from the same gas well was performed using (Cryotrapping) Gas Chromatography-Inductively Coupled Plasma Mass Spectrometry. The major species in all phases investigated was found to be trimethylarsine with a highest concentration of 17.8 ng/L (As) in the gas phase and 33.2 μg/L (As) in the stable condensate phase. The highest amount of trimethylarsine (121 μg/L (As)) was found in the pressurized condensate, along with trace amounts of non-identified higher alkylated arsines. Volatile arsenic species in natural gas and its related products cause concern with regards to environment, safety, occupational health and gas processing. Therefore, interest lies in a fast and simple field method for the determination of volatile arsenicals. Here, we use simple liquid and solid sorption techniques, namely absorption in silver nitrate solution and adsorption on silver nitrate impregnated silica gel tubes followed by total arsenic determination as a promising tool for field monitoring of volatile arsenicals in natural gas and gas condensates. Preliminary results obtained for the sorption-based methods show that around 70% of the arsenic is determined with these methods in comparison to volatile arsenic determination using GC-ICP-MS. Furthermore, an inter-laboratory- and inter-method comparison was performed using silver nitrate impregnated silica tubes on 14 different gas samples with concentrations varying from below 1 to 1000 μg As/m 3 natural gas. The results obtained from the two laboratories differ in a range of 10 to 60%, but agree within the order of magnitude, which is satisfactory for our purposes.

  5. Investigation into the determination of trimethylarsine in natural gas and its partitioning into gas and condensate phases using (cryotrapping)/gas chromatography coupled to inductively coupled plasma mass spectrometry and liquid/solid sorption techniques

    Energy Technology Data Exchange (ETDEWEB)

    Krupp, E.M. [University of Aberdeen, College of Physical Sciences, Meston Walk, AB24 3UE, Aberdeen, Scotland (United Kingdom)], E-mail: e.krupp@abdn.ac.uk; Johnson, C. [METCO Services LTD, Denmore Road, Bridge of Don, AB23 8JW, Aberdeen, Scotland (United Kingdom)], E-mail: Charles.Johnson@metco-uk.com; Rechsteiner, C. [Chevron Energy Technology Co., 100 Chevron Way, MS 50-1279, Richmond, CA 94802 (United States)], E-mail: CRechsteiner@chevron.com; Moir, M. [Chevron Energy Technology Co., 100 Chevron Way, MS 50-1279, Richmond, CA 94802 (United States)], E-mail: MMoir@chevron.com; Leong, D. [Chevron Energy Technology Co., 100 Chevron Way, MS 50-1279, Richmond, CA 94802 (United States)], E-mail: DLeong@chevron.com; Feldmann, J. [University of Aberdeen, College of Physical Sciences, Meston Walk, AB24 3UE, Aberdeen, Scotland (United Kingdom)], E-mail: j.feldmann@abdn.ac.uk

    2007-09-15

    Speciation of trialkylated arsenic compunds in natural gas, pressurized and stable condensate samples from the same gas well was performed using (Cryotrapping) Gas Chromatography-Inductively Coupled Plasma Mass Spectrometry. The major species in all phases investigated was found to be trimethylarsine with a highest concentration of 17.8 ng/L (As) in the gas phase and 33.2 {mu}g/L (As) in the stable condensate phase. The highest amount of trimethylarsine (121 {mu}g/L (As)) was found in the pressurized condensate, along with trace amounts of non-identified higher alkylated arsines. Volatile arsenic species in natural gas and its related products cause concern with regards to environment, safety, occupational health and gas processing. Therefore, interest lies in a fast and simple field method for the determination of volatile arsenicals. Here, we use simple liquid and solid sorption techniques, namely absorption in silver nitrate solution and adsorption on silver nitrate impregnated silica gel tubes followed by total arsenic determination as a promising tool for field monitoring of volatile arsenicals in natural gas and gas condensates. Preliminary results obtained for the sorption-based methods show that around 70% of the arsenic is determined with these methods in comparison to volatile arsenic determination using GC-ICP-MS. Furthermore, an inter-laboratory- and inter-method comparison was performed using silver nitrate impregnated silica tubes on 14 different gas samples with concentrations varying from below 1 to 1000 {mu}g As/m{sup 3} natural gas. The results obtained from the two laboratories differ in a range of 10 to 60%, but agree within the order of magnitude, which is satisfactory for our purposes.

  6. Investigation into the determination of trimethylarsine in natural gas and its partitioning into gas and condensate phases using (cryotrapping)/gas chromatography coupled to inductively coupled plasma mass spectrometry and liquid/solid sorption techniques

    International Nuclear Information System (INIS)

    Speciation of trialkylated arsenic compunds in natural gas, pressurized and stable condensate samples from the same gas well was performed using (Cryotrapping) Gas Chromatography-Inductively Coupled Plasma Mass Spectrometry. The major species in all phases investigated was found to be trimethylarsine with a highest concentration of 17.8 ng/L (As) in the gas phase and 33.2 μg/L (As) in the stable condensate phase. The highest amount of trimethylarsine (121 μg/L (As)) was found in the pressurized condensate, along with trace amounts of non-identified higher alkylated arsines. Volatile arsenic species in natural gas and its related products cause concern with regards to environment, safety, occupational health and gas processing. Therefore, interest lies in a fast and simple field method for the determination of volatile arsenicals. Here, we use simple liquid and solid sorption techniques, namely absorption in silver nitrate solution and adsorption on silver nitrate impregnated silica gel tubes followed by total arsenic determination as a promising tool for field monitoring of volatile arsenicals in natural gas and gas condensates. Preliminary results obtained for the sorption-based methods show that around 70% of the arsenic is determined with these methods in comparison to volatile arsenic determination using GC-ICP-MS. Furthermore, an inter-laboratory- and inter-method comparison was performed using silver nitrate impregnated silica tubes on 14 different gas samples with concentrations varying from below 1 to 1000 μg As/m3 natural gas. The results obtained from the two laboratories differ in a range of 10 to 60%, but agree within the order of magnitude, which is satisfactory for our purposes

  7. Speciation of four selenium compounds using high performance liquid chromatography with on-line detection by inductively coupled plasma mass spectrometry or flame atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Pedersen, Gitte Alsing; Larsen, Erik Huusfeldt

    1997-01-01

    with an aqueous solution of 6 mmol L-1 of salicylate ion at pH 8.5 as the mobile phase which allowed the isocratic separation of the four selenium analytes within 8 minutes. The separated selenium species were detected on-line by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma mass...... spectrometry (ICP-MS). The signal-to-noise ratio of the FAAS detector was optimized using a hydrogen-argon entrained-air flame and a slotted-tube atom trap (STAT) in the flame. The limit of detection (3 sigma) achieved by the HPLC-FAAS system was 1 mg L-1 of selenium (100 mu L injections) for each of the four...

  8. Inductively coupled plasma-mass spectrometry for elemental analysis and isotope ratio determinations in individual organic compounds separated by gas chromatography

    International Nuclear Information System (INIS)

    A gas chromatograph (GC) with a packed column was interfaced to an inductively coupled plasma-mass spectrometer (ICP-MS) to yield atomic mass spectra from volatile organic compounds. Atomization of injected compounds was nearly complete and independent of molecular structure, so that elemental ratios could be determined. Detection limits were in the range 0.001 to 400 ng s-1, depending on the ionization energy of the element and its abundance in the background spectrum. The relative standard deviation of measured isotope ratios varied from 0.4% for Br (i.e., a ratio close to unity) to 18% for N (a very large ratio). Thus, GC-ICP-MS provides elemental and isotope ratio information that is complementary to the molecular information derived from GC-MS with conventional ionization methods

  9. Inductively coupled plasma-mass spectrometry for elemental analysis and isotope ratio determinations in individual organic compounds separated by gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Chong, N.S.; Houk, R.S.

    1987-01-01

    A gas chromatograph (GC) with a packed column was interfaced to an inductively coupled plasma-mass spectrometer (ICP-MS) to yield atomic mass spectra from volatile organic compounds. Atomization of injected compounds was nearly complete and independent of molecular structure, so that elemental ratios could be determined. Detection limits were in the range 0.001 to 400 ng s/sup -1/, depending on the ionization energy of the element and its abundance in the background spectrum. The relative standard deviation of measured isotope ratios varied from 0.4% for Br (i.e., a ratio close to unity) to 18% for N (a very large ratio). Thus, GC-ICP-MS provides elemental and isotope ratio information that is complementary to the molecular information derived from GC-MS with conventional ionization methods.

  10. Arsenic speciation in seafood samples with emphasis on minor constituents. An investigation by high performance liquid chromatography with inductively coupled plasma mass spectrometric detection

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Pritzl, G.; Hansen, S. H.

    1993-01-01

    Extracts of 11 samples of shrimp, crab, fish, fish liver, shellfish and lobster digestive gland (hepatopancreas), including five certified reference materials, were investigated for their contents of arsenic compounds (arsenic speciation). The cation-exchange high performance liquid chromatography...

  11. Rapid Determination of Plutonium Isotopes in Environmental Samples Using Sequential Injection Extraction Chromatography and Detection by Inductively Coupled Plasma Mass Spectrometry

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per;

    2009-01-01

    This article presents an automated method for the rapid determination of 239Pu and 240Pu in various environmental samples. The analytical method involves the in-line separation of Pu isotopes using extraction chromatography (TEVA) implemented in a sequential injection (SI) network followed by det...

  12. Sm isotope composition and Sm/Eu ratio determination in an irradiated 153Eu sample by ion exchange chromatography-quadrupole inductively coupled plasma mass spectrometry combined with double spike isotope dilution technique

    International Nuclear Information System (INIS)

    Within the framework of the research undertaken by the French Atomic Energy Commission on transmutation of long-lived radionuclides, targets of highly enriched actinides and fission products were irradiated in the fast neutron reactor Phenix. Precise and accurate measurements of the isotopic and elemental composition of the enriched elements are therefore required. In order to obtain the uncertainties of several per mil and to reduce handling time and exposure to analyst on radioactive material, the on-line coupling of ion exchange chromatography with quadrupole inductively coupled plasma mass spectrometry has been associated with the technique of the double spike isotope dilution. We present in this paper the results obtained on an irradiated sample of Europium oxide powder (enriched at 99.13% in 153Eu). After irradiation of around 5 mg of Eu2O3 powder the theoretical calculations predict the formation of several micrograms of gadolinium and samarium isotopes. In relation to the very high activity of the sample after irradiation and the very low quantity of Sm formed, the on-line ion exchange chromatography separation of Gd, Sm and Eu before Sm isotope ratio measurements has been developed for the quantification of the 152Sm/153Eu ratio. These on-line measurements were associated with the double spike isotope dilution technique after calibration of a 147Sm/151Eu spike solution. The external reproducibility of Sm isotopic ratios was determined to be around 0.5% (2 σ) resulting in a final uncertainty on the 152Sm/153Eu ratio of around 1% (2 σ). These on-line measurements present therefore a robust and high-throughput alternative to the thermal-ionisation mass spectrometry technique used so far in combination with off-line chromatographic separation, particularly in nuclear applications where characterisation of high activity sample solutions is required. (authors)

  13. Arsenic speciation by liquid chromatography coupled with ionspray tandem mass spectrometry

    DEFF Research Database (Denmark)

    Corr, J. J.; Larsen, Erik Huusfeldt

    1996-01-01

    Ionspray mass spectrometry, a well established organic analysis technique, has been coupled to high-performance liquid chromatography for speciation of organic arsenic compounds, The ionspray source and differentially pumped interface of the mass spectrometer were operated in dual modes for...... fragmentation patterns showing molecular dissociation through an expected common product ion were obtained for the four arsenosugars, Molecular mode detection was utilized for qualitative verification of speciation analysis by high-performance liquid chromatography coupled to inductively coupled plasma mass...

  14. Determination of Ni(CO)4, Fe(CO)5, Mo(CO)6, and W(CO)6 in sewage gas by using cryotrapping gas chromatography inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Feldmann, J

    1999-02-01

    Evidence for the occurrence of Ni(CO)4 in addition to Mo(CO)6 and W(CO)6 in fermentation gases from a municipal sewage treatment plant is presented for the first time. The gases were sampled at the top of the sewage sludge digester using Tedlar bags, and were analysed using cryotrapping followed by gas chromatography coupled with inductively coupled mass spectrometry (GC-ICP-MS). The use of an ICP-MS as an element-specific detector gives sufficiently low detection limits for metals and was coupled to a packed column gas chromatograph. This method provides information about the speciation of volatile transition metals in contrast to previously used methods for the determination of Ni(CO)4 in gas samples. The element-specific detection of three different isotopes (m/z 58, 60, 62) and the correspondence of the samples' retention times with those of the standard provided convincing evidence that Ni(CO)4 is present in the fermentation gas. The concentrations found were in the sub-ppb level, which is at least one order of magnitude lower than the threshold level of 1 ppb (v/v). In addition, Mo(CO)6 and W(CO)6 were also measured in the sub-ppb range in contrast to the absence of Fe(CO)5. The stabilities of Ni(CO)4, Fe(CO)5, and Mo(CO)6 were tested in a carbon monoxide atmosphere. In the presence of distilled water, the following order of stability was found after 11 weeks: Fe(CO)5 GC-ICP-MS can be employed to identify species-specific traces of metal carbonyls in process gases such as sewage gas. PMID:11529076

  15. Determination of aminopolycarboxylic acids at ultra-trace levels by means of online coupling ion exchange chromatography and inductively coupled plasma-mass spectrometry with indirect detection via their Pd2+-complexes

    International Nuclear Information System (INIS)

    Highlights: • 8 important APCA’s analyzed in one run instead of 3 in the previous method. • Pd2+ extents the methods applicability to 3 and more dentate amino carboxylic acids. • Separation system optimized for the isocratic determination of important APCA’s. • Thermodynamic stability of APCA–Pd2+ complexes is higher than for Fe3+ and In3+. • Pd2+ is kinetically much slower than Fe3+ and In3+ and makes the method more rugged. - Abstract: A new indirect IC-ICP-MS method for the determination of aminopolycarboxylic acids in water samples is described. It is based on the addition of an excess of Pd(II) to water samples. The analytes are forced into very strong and negatively charged palladium complexes, separated by ion exchange chromatography and detected by their palladium content, utilizing an on-line coupled ICP-MS. This method is suitable to determine the concentration of 8 aminopolycarboxylic acids (nitrilotriacetic acid (NTA), (2-carboxyethyl) iminodiacetic acid (β-ADA), methylglycinediacetic acid (MGDA), 2-hydroxyethyl) ethylenediamine triacetic acid (HEDTA), diethylene triamine pentaacetic acid (DTPA), ethylendiamine tetraacetic acid (EDTA), 1,3-diaminopropane tetraacetic acid (1,3-PDTA) and 1,2-diaminopropane tetraacetic acid (1,2-PDTA) at the ng kg−1 level. The method is faster and easier than the established gas chromatography (GC)-method ISO 16588:2002 [1] and up to two orders of magnitude more sensitive than the ion pair chromatography based method of DIN 38413-8. Analytic performance is superior to ISO 16588:2002 and the comparability is good

  16. Determination of aminopolycarboxylic acids at ultra-trace levels by means of online coupling ion exchange chromatography and inductively coupled plasma-mass spectrometry with indirect detection via their Pd{sup 2+}-complexes

    Energy Technology Data Exchange (ETDEWEB)

    Nette, David; Seubert, Andreas, E-mail: seubert@staff.uni-marburg.de

    2015-07-16

    Highlights: • 8 important APCA’s analyzed in one run instead of 3 in the previous method. • Pd{sup 2+} extents the methods applicability to 3 and more dentate amino carboxylic acids. • Separation system optimized for the isocratic determination of important APCA’s. • Thermodynamic stability of APCA–Pd{sup 2+} complexes is higher than for Fe{sup 3+} and In{sup 3+}. • Pd{sup 2+} is kinetically much slower than Fe{sup 3+} and In{sup 3+} and makes the method more rugged. - Abstract: A new indirect IC-ICP-MS method for the determination of aminopolycarboxylic acids in water samples is described. It is based on the addition of an excess of Pd(II) to water samples. The analytes are forced into very strong and negatively charged palladium complexes, separated by ion exchange chromatography and detected by their palladium content, utilizing an on-line coupled ICP-MS. This method is suitable to determine the concentration of 8 aminopolycarboxylic acids (nitrilotriacetic acid (NTA), (2-carboxyethyl) iminodiacetic acid (β-ADA), methylglycinediacetic acid (MGDA), 2-hydroxyethyl) ethylenediamine triacetic acid (HEDTA), diethylene triamine pentaacetic acid (DTPA), ethylendiamine tetraacetic acid (EDTA), 1,3-diaminopropane tetraacetic acid (1,3-PDTA) and 1,2-diaminopropane tetraacetic acid (1,2-PDTA) at the ng kg{sup −1} level. The method is faster and easier than the established gas chromatography (GC)-method ISO 16588:2002 [1] and up to two orders of magnitude more sensitive than the ion pair chromatography based method of DIN 38413-8. Analytic performance is superior to ISO 16588:2002 and the comparability is good.

  17. Determination of trace amounts of rare-earth elements in highly pure neodymium oxide by sector field inductively coupled plasma mass spectrometry (ICP-SFMS) and high-performance liquid chromatography (HPLC) techniques

    International Nuclear Information System (INIS)

    Recently rare-earth elements (REE) have received much attention in fields of geochemistry and industry. Rapid and accurate determinations of them are increasingly required as industrial demands expand. Sector field inductively coupled plasma mass spectrometry (ICP-SFMS) with high-performance liquid chromatography (HPLC) has been applied to the determination of REE. HR ICP-MS was used as an element-selective detector for HPLC in highly pure materials. The separation of REE with HPLC helped to avoid erroneous analytical results due to spectral interferences. Sixteen elements (Sc, Y and 14 lanthanides) were determined selectively with the HPLC/ICP-SFMS system using a concentration gradient methods. The detection limits with the HPLC/ICP-SFMS system were about 0.5-10 pg mL-1. The percentage recovery ranged from 90% to 100% for different REE. The %RSD of the methods varying between 2.5% and 4.5% for a set of five (n=5) replicates was found for the IPEN's material and for the certificate reference sample. Determination of trace REEs in two highly pure neodymium oxides samples (IPEN and Johnson Matthey Company) were performed. In short, the IPEN's materials which are highly pure (>99.9%) were successfully analyzed without spectral interferences

  18. Determination of Am and Cm in spent nuclear fuels by isotope dilution inductively coupled plasma mass spectrometry and isotope dilution thermal ionization mass spectrometry after separation by high-performance liquid chromatography

    International Nuclear Information System (INIS)

    Elemental and isotopic determination of americium and curium in spent nuclear fuels is necessary to validate neutronic calculation codes and for nuclear waste disposal purposes. Prior to mass spectrometric analysis, it is mandatory to perform separations in order to eliminate isobaric interferences between U, Pu, Am and Cm. In the spent fuels samples analyzed, a separation of U and Pu has been first realized with an anion-exchange resin. Then a rapid Am/Cm separation has been developed by high-performance liquid chromatography (HPLC) with an on-line detection using the Am and Cm α-emission. The influence of the different parameters on the chromatographic separation are described and discussed. Inductively coupled plasma mass spectrometry (ICP-MS) and thermal-ionization mass spectrometry (TIMS) have been used to measure the isotopic composition of U, Am and Cm and to determine the 241Am/238U and 244Cm/238U ratios with the double spike isotope dilution method. The measurement procedures and the accuracy and precision of the results obtained with a quadrupole ICP-MS on different spent fuels samples are discussed and compared with those obtained by TIMS, used as a reference technique. (orig.)

  19. Superconducting Resonant Inductive Power Coupling Project

    Data.gov (United States)

    National Aeronautics and Space Administration — The proposed effort will develop a technology to wirelessly and efficiently transfer power over hundreds of meters via resonant inductive coupling. The key...

  20. Comparison of copper labeling followed by liquid chromatography-inductively coupled plasma mass spectrometry and immunochemical assays for serum hepcidin-25 determination.

    Science.gov (United States)

    Konz, Tobias; Alonso-García, Javier; Montes-Bayón, María; Sanz-Medel, Alfredo

    2013-10-17

    Hepcidin-25 has been defined as the key biomarker in iron metabolism. This peptide binds to the iron transporter ferroportin to cause its degradation. Therefore, the need for specific, accurate and precise methods for the quantification of hepcidin-25 in biological fluids is dramatically increasing. In this regard, the use of rapid immunochemical methods that provide low limit of quantification is desired for routine clinical use. However, such fast methodologies should be first analytically evaluated and compared with alternative strategies to check for their advantages and limitations. Here we compare the use of a commercial immunochemical assay for hepcidin determination with a novel analytical approach based on Cu-labeling of the peptide followed by Cu determination using liquid chromatography (HPLC) and plasma mass spectrometry (ICP-MS). The figures of merit of both systems reveal similar analytical characteristics and both seem to be adequate for the determination of the peptide at biologically relevant concentrations in human serum samples. The analysis of a larger number of samples (n=50) by both techniques showed a good agreement in the concentrations found. Such finding permits to address the hepcidin recovery in the sample preparation procedure necessary for the HPLC-ICP-MS analysis in human serum that turn out to be 76-85%. Additionally, limitations due to cross-reactivity issues of the ELISA method could be addressed in some of the samples by using LC-ICP-MS and were confirmed by LC-Electrospray-MS. PMID:24091368

  1. Robust Method Using Online Steric Exclusion Chromatography-Ultraviolet-Inductively Coupled Plasma Mass Spectrometry To Investigate Nanoparticle Fate and Behavior in Environmental Samples.

    Science.gov (United States)

    Al-Sid-Cheikh, Maya; Pédrot, Mathieu; Bouhnik-Le Coz, Martine; Dia, Aline; Davranche, Mélanie; Neaime, Chrystelle; Grasset, Fabien

    2015-10-20

    The foundation of nanoscience is that the properties of materials change as a function of their physical dimensions, and nanotechnology exploits this premise by applying selected property modifications for a specific benefit. However, to investigate the fate and effect of the engineered nanoparticles on toxic metal (TM) mobility, the analytical limitations in a natural environment remain a critical problem to overcome. Recently, a new generation of size exclusion chromatography (SEC) columns developed with spherical silica is available for pore sizes between 5 and 400 nm, allowing the analysis of nanoparticles. In this study, these columns were applied to the analysis of metal-based nanoparticles in environmental and artificial samples. The new method allows quantitative measurements of the interactions among nanoparticles, organic matter, and metals. Moreover, because of the new nanoscale SEC, our method allows the study of these interactions for different size ranges of nanoparticles and weights of organic molecules with a precision of 1.2 × 10(-2) kDa. The method was successfully applied to the study of nanomagnetite spiked in complex matrixes, such as sewage sludge, groundwater, tap water, and different artificial samples containing Leonardite humic acid and different toxic metals (i.e., As, Pb, Th). Finally, our results showed that different types of interactions, such as adsorption, stabilization, and/or destabilization of nanomagnetite could be observed using this new method. PMID:26383030

  2. Simultaneous determination of Cr(iii) and Cr(vi) using reversed-phased ion-pairing liquid chromatography with dynamic reaction cell inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Wolf, R.E.; Morrison, J.M.; Goldhaber, M.B.

    2007-01-01

    A method for the simultaneous determination of Cr(iii) and Cr(vi) species in waters, soil leachates and synthetic bio-fluids is described. The method uses reversed-phase ion-pairing liquid chromatography to separate the chromium species and a dynamic reaction cell (DRC??) equipped ICP-MS for detection of chromium. Separation of the chromium species is carried out in less than 2 min. Cr(iii) is complexed with ethylenediaminetetraacetic acid (EDTA) prior to separation by mixing samples with the mobile phase containing 2.0 mM tetrabutylammonium hydroxide (TBAOH), 0.5 mM EDTA (dipotassium salt), and 5% (vol/vol) methanol, adjusted to pH 7.6. The interfering 40Ar 12C+ background peak at mass 52 was reduced by over four orders of magnitude to less than 200 cps by using 0.65 mL min-1 ammonia as a reaction gas and an RPq setting on the DRC of 0.75. Method detection limits (MDLs) of 0.09 ??g L-1 for Cr(iii) and 0.06 ??g L-1 for Cr(vi) were obtained based on peak areas at mass 52 for 50 ??L injections of low level spikes. Reproducibility at 2 ??g L-1 was 3% RSD for 5 replicate injections. The tolerance of the method to various levels of common cations and anions found in natural waters and to matrix constituents found in soil leachates and simulated gastric and lung fluids was tested by performing spike recovery calculations for a variety of samples. ?? The Royal Society of Chemistry.

  3. Determination of trace elements in high pure rare earth oxide by double focusing inductively coupled plasma mass spectrometry (HR ICP-MS) and high performance liquid chromatography (HPLC) techniques

    International Nuclear Information System (INIS)

    Rare earth oxides are used in several technological fields whose applications can be observed in several areas of modern technology, among which are included: lasers, semiconductors semi, high purity materials and metallic alloys. The field of applications of the rare earth elements is quite wide. Several important industrial applications are ceramics, catalysts and metallurgical as well as research areas and high technology sectors. Such applications have been presenting an accentuated growth in the last years. Chemical characterization of rare earth oxides of high purity has been constituting one of the major challenges of analytical chemistry. Several analytical techniques were used for chemical characterization of high purity rare earth the oxides. Even so, those techniques present limitations when one needs to characterize materials of a high level of purity, as in the case of rare earth oxides. Some of those limitations are associated, for example, to spectral interference. Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is a powerful analytical tool for quantitative analysis of metal impurities in high purity materials. The Instituto de Pesquisas Energeticas e Nucleares (IPEN) has an unit of production and purification of rare earth oxides, with above 99,9% level of purity. In this work, the rare earth impurities were characterized in samples (La2O3; CeO2; Pr6O11; Nd2O3; Sm2O3; Gd2O3; Y2O3) produced at the IPEN and certified standard materials produced by Johnson Matthey Chemical (JMC). The technique of high performance liquid chromatography (HPLC) was used in the separation of the impurities. Quantification of metallic impurities was carried out as inductively coupled plasma mass spectrometer (HR-ICP MS). In this work it is presented a new analytical methodology in the chemical characterization of metallic impurities in rare earth oxides of high purity (> 99,9%) with and without separation of the matrix. Analyses of standard certified materials and

  4. Sampling and probing volatile metal(loid) species in natural waters by in-situ purge and cryogenic trapping followed by gas chromatography and inductively coupled plasma mass spectrometry (P-CT-GC-ICP/MS)

    International Nuclear Information System (INIS)

    An in situ purge and cryogenic trapping method for the pre-concentration of volatile metal and metalloid compounds dissolved in natural waters was developed. The analytes were collected in cryogenic trap stored at -196C until analysis in the laboratory. Cryogenic traps were then introduced into a flash desorption, cryofocusing gas chromatography system hyphenated to an inductively coupled plasma mass spectrometer (ICP/MS). This multi-element detection technique allowed to determine volatile compounds of selected elements in aqueous solution simultaneously by scanning their corresponding stable isotopes.Blanks and recoveries for the whole analytical procedure of several volatile compounds of selected elements (Me2Se, Me2Se2, Me2Hg, Et2Hg, Me4Sn, Et4Sn, Me4Pb, Et4Pb) were determined and are discussed. Method detection limits for 1 l water sample were estimated for Se, Hg, Sn and Pb volatile species to be as low as 10.0 (0.8), 1.0 (0.2), 0.4 (0.05) and 0.4 (0.08) fmol/l (pg/l), respectively.The occurrence of volatile compounds of selenium, tin, mercury and lead was evidenced and investigated in three major European estuaries such as the Gironde (F), the Rhine (NL) and the Scheldt (B/NL). The presence of these volatile species in natural waters seems to be related to both exchanges between environmental compartments and anthropogenic inputs. (Copyright (c) 1998 Elsevier Science B.V., Amsterdam. All rights reserved.)

  5. Sampling and probing volatile metal(loid) species in natural waters by in-situ purge and cryogenic trapping followed by gas chromatography and inductively coupled plasma mass spectrometry (P-CT-GC-ICP/MS)

    Energy Technology Data Exchange (ETDEWEB)

    Amouroux, D.; Tessier, E.; Pecheyran, C.; Donard, O.F.X. [Laboratoire de Chimie Bio-Inorganique et Environnement, EP CNRS 132, Universite de Pau et des Pays de l' Adour, Centre Helioparc, 2 Avenue du President Angot, 64000 Pau (France)

    1998-12-31

    An in situ purge and cryogenic trapping method for the pre-concentration of volatile metal and metalloid compounds dissolved in natural waters was developed. The analytes were collected in cryogenic trap stored at -196C until analysis in the laboratory. Cryogenic traps were then introduced into a flash desorption, cryofocusing gas chromatography system hyphenated to an inductively coupled plasma mass spectrometer (ICP/MS). This multi-element detection technique allowed to determine volatile compounds of selected elements in aqueous solution simultaneously by scanning their corresponding stable isotopes.Blanks and recoveries for the whole analytical procedure of several volatile compounds of selected elements (Me{sub 2}Se, Me{sub 2}Se{sub 2}, Me{sub 2}Hg, Et{sub 2}Hg, Me{sub 4}Sn, Et{sub 4}Sn, Me{sub 4}Pb, Et{sub 4}Pb) were determined and are discussed. Method detection limits for 1 l water sample were estimated for Se, Hg, Sn and Pb volatile species to be as low as 10.0 (0.8), 1.0 (0.2), 0.4 (0.05) and 0.4 (0.08) fmol/l (pg/l), respectively.The occurrence of volatile compounds of selenium, tin, mercury and lead was evidenced and investigated in three major European estuaries such as the Gironde (F), the Rhine (NL) and the Scheldt (B/NL). The presence of these volatile species in natural waters seems to be related to both exchanges between environmental compartments and anthropogenic inputs. (Copyright (c) 1998 Elsevier Science B.V., Amsterdam. All rights reserved.)

  6. Selenium speciation in radix puerariae using ultrasonic assisted extraction combined with reversed phase high performance liquid chromatography-inductively coupled plasma-mass spectrometry after magnetic solid-phase extraction with 5-sulfosalicylic acid functionalized magnetic nanoparticles

    Science.gov (United States)

    Cao, Yupin; Yan, Lizhen; Huang, Hongli; Deng, Biyang

    2016-08-01

    A new method for determination of selenium species in radix puerariae was described. The method consists of sample enrichment with 5-sulfosalicylic acid (SSA)-functionalized silica-coated magnetic nanoparticles (SMNPs), high performance liquid chromatography (HPLC) separation, and online detection using inductively coupled plasma mass spectrometry (ICP-MS). The selenium species were extracted using ultrasonic extraction system with a mixture of protease K and lipase. The SSA-SMNPs were used to enrich trace amounts of selenite [Se(IV)], selenate [Se(VI)], selenomethionine (SeMet), and selenocystine (SeCys2) from lower selenium containing samples. Under the optimal conditions, the limits of detection (3σ) for SeCys2, Se(IV), SeMet and Se(VI) were observed as 0.0023, 0.0015, 0.0043, and 0.0016 ng mL- 1, respectively. The RSD values (n = 6) of method for intraday were observed between 0.5% and 0.9%. The RSD values of method for interday were less than 1.3%. The linear concentration ranges for SeCys2, Se(IV), SeMet and Se(VI) were 0.008-1000, 0.005-200, 0.015-500 and 0.006-200 ng mL- 1, respectively. The detection limits of this method were improved by 10 times due to the enrichment with the SSA-SMNP extraction. The contents of SeCys2, Se(IV), SeMet, and Se(VI) in radix puerariae were determined as 0.0140, 0.171, 0.0178, and 0.0344 μg g- 1, respectively. The recoveries were in the range of 95.6%-99.4% and the RSDs (n = 6) of recoveries were less than 1.5%.

  7. Antenna-coupled microwave kinetic inductance detectors

    Energy Technology Data Exchange (ETDEWEB)

    Day, P.K. [Jet Propulsion Laboratory, 4800 Oak Grove Dr., Pasadena, CA 91109 (United States)]. E-mail: Peter.K.Day@jpl.nasa.gov; Leduc, H.G. [Jet Propulsion Laboratory, 4800 Oak Grove Dr., Pasadena, CA 91109 (United States); Goldin, A. [Jet Propulsion Laboratory, 4800 Oak Grove Dr., Pasadena, CA 91109 (United States); Vayonakis, T. [California Institute of Technology, 1200 E. California Blvd., Pasadena, CA 91125 (United States); Mazin, B.A. [Jet Propulsion Laboratory, 4800 Oak Grove Dr., Pasadena, CA 91109 (United States); Kumar, S. [California Institute of Technology, 1200 E. California Blvd., Pasadena, CA 91125 (United States); Gao, J. [California Institute of Technology, 1200 E. California Blvd., Pasadena, CA 91125 (United States); Zmuidzinas, J. [California Institute of Technology, 1200 E. California Blvd., Pasadena, CA 91125 (United States)

    2006-04-15

    We report on the development of Microwave Kinetic Inductance Detectors (MKIDs) coupled to planar antennas for millimeter/submillimeter wavelengths. The MKID is a relatively new type of superconducting photon detector which is applicable from millimeter-wave frequencies to X-rays. Photons are absorbed in a superconductor, producing quasiparticle excitations, which change the surface reactance (kinetic inductance) of the superconductor. The changes in kinetic inductance are monitored using microwave high-Q thin-film superconducting resonators. Because the MKID is particularly amenable to frequency-domain multiplexing, with likely detector multiplexing factors of {approx}10{sup 3} or more per cryogenic amplifier, these detectors are well suited for use in large arrays. We have fabricated MKIDs coupled to submillimeter slot-array antennas using microstrip lines and have detected power from a thermal radiation source. We discuss the potential of antenna-coupled MKID arrays for ground and space-based millimeter/submillimeter imaging.

  8. Inductively coupled wireless RF coil arrays.

    Science.gov (United States)

    Bulumulla, S B; Fiveland, E; Park, K J; Foo, T K; Hardy, C J

    2015-04-01

    As the number of coils increases in multi-channel MRI receiver-coil arrays, RF cables and connectors become increasingly bulky and heavy, degrading patient comfort and slowing workflow. Inductive coupling of signals provides an attractive "wireless" approach, with the potential to reduce coil weight and cost while simplifying patient setup. In this work, multi-channel inductively coupled anterior arrays were developed and characterized for 1.5T imaging. These comprised MR receiver coils inductively (or "wirelessly") linked to secondary or "sniffer" coils whose outputs were transmitted via preamps to the MR system cabinet. The induced currents in the imaging coils were blocked by passive diode circuits during RF transmit. The imaging arrays were totally passive, obviating the need to deliver power to the coils, and providing lightweight, untethered signal reception with easily positioned coils. Single-shot fast spin echo images were acquired from 5 volunteers using a 7-element inductively coupled coil array and a conventionally cabled 7-element coil array of identical geometry, with the inductively-coupled array showing a relative signal-to-noise ratio of 0.86 +/- 0.07. The concept was extended to a larger 9-element coil array to demonstrate the effect of coil element size on signal transfer and RF-transmit blocking. PMID:25523607

  9. Speciation of Volatile Selenium Species in Plants Using Gas Chromatography/Inductively Coupled Plasma Mass Spectrometry%气相色谱/电感耦合等离子体质谱测定植物中挥发性硒化合物

    Institute of Scientific and Technical Information of China (English)

    Juris MEIJA; Maria MONTES-BAY(O)N; Joseph A CARUSO; Danika L LEDUC; Norman TERRY

    2004-01-01

    Gas chromatography/inductively coupled plasma mass spectrometry (GC/ICP-MS) coupled with solid phase micro-extraction can provide a simple, extremely selective and sensitive technique for the analysis of volatile sulfur and selenium compounds in the headspace of growing plants. In this work, the technique was used to evaluate the volatilization of selenium in wild-type and genetically-modified Brassica juncea seedlings. By converting toxic inorganic selenium in the soil to less toxic, volatile organic selenium, B. juncea might be useful in bioremediation of selenium contaminated soil.

  10. Determination of methylmercury and estimation of total mercury in seafood using high performance liquid chromatography (HPLC) and inductively coupled plasma-mass spectrometry (ICP-MS): Method development and validation

    International Nuclear Information System (INIS)

    A method was developed for determination of methylmercury and estimation of total mercury in seafood. Mercury (Hg) compounds were extracted from 0.5 g edible seafood or 0.2 g lyophilized reference material by adding 50 ml aqueous 1% w/v L-cysteine.HCl.H2O and heating 120 min at 60 deg. C in glass vials. Hg compounds in 50 μl of filtered extract were separated by reversed-phase high performance liquid chromatography using a C-18 column and aqueous 0.1% w/v L-cysteine.HCl.H2O + 0.1% w/v L-cysteine mobile phase at room temperature and were detected by inductively coupled plasma-mass spectrometry at mass-to-charge ratio 202. Total Hg was calculated as the mathematical sum of methyl and inorganic Hg determined in extracts. For seafoods containing 0.055-2.78 mg kg-1 methylmercury and 0.014-0.137 mg kg-1 inorganic Hg, precision of analyses was ≤5% relative standard deviation (R.S.D.) for methylmercury and ≤9% R.S.D. for inorganic Hg. Recovery of added analyte was 94% for methylmercury and 98% for inorganic Hg. Methyl and total Hg results for reference materials agreed with certified values. Limits of quantitation were 0.007 mg kg-1 methylmercury and 0.005 mg kg-1 inorganic Hg in edible seafood and 0.017 mg kg-1 methylmercury and 0.012 mg kg-1 inorganic Hg in lyophilized reference materials. Evaluation of analyte stability demonstrated that L-cysteine both stabilized and de-alkylated methylmercury, depending on holding time and cysteine concentration. Polypropylene adversely affected methylmercury stability. Total Hg results determined by this method were equivalent to results determined independently by cold vapour-atomic absorption spectrometry. Methylmercury was the predominant form of Hg in finfish. Ratios of methylmercury/total Hg determined by this method were 93-98% for finfish and 38-48% for mollusks

  11. Mercury speciation in liquid petroleum product : comparison between on-site approach and lab measurement using size exclusion chromatography with high resolution inductively coupled plasma mass spectrometric detection (SEC-ICP-HR MS).

    OpenAIRE

    Gaulier, Florine; Gibert, Alexandre; Walls, David; Langford, Michael; Baker, Stuart; Baudot, Arnaud; Porcheron, Fabien; Lienmann, Charles-Philippe

    2015-01-01

    The accuracy of two different analytical methods dedicated to the speciation of mercury in liquid hydrocarbons isdiscussed in the present paper. A first step involving the comparison of a modified UOP 938 method—based onfiltration, purge and extraction—with size exclusion chromatography coupled to ICP-HR MS (SEC-ICP-HR MS)was carried out on specific synthetic model mercury compounds. The modified UOP 938 method (defined hereas operational speciation) allowed various mercury compounds to be gr...

  12. Resonant inductive coupling wireless power transfer

    OpenAIRE

    Bou Balust, Elisenda

    2012-01-01

    Recent research on wireless power transfer (WPT) using resonant inductive coupling has demonstrated very promising efficiencies (above 80%) [1] at large distances compared to the antenna dimensions (more than three times the receiver/transmitter diameters). Due to the number of applications that could benefit from WPT: from electric vehicles to sensor networks, commercial electronic devices, health equipment, biomedical implants, in-space systems and so on, the development and optimizat...

  13. Speciation of arsenic of liquid and gaseous emissions from soil in a microcosmos experiment by liquid and gas chromatography with inductively coupled plasma mass spectrometer (ICP-MS) detection

    Energy Technology Data Exchange (ETDEWEB)

    Prohaska, T.; Stingeder, G. [University of Agricultural Sciences - BOKU Wien (Austria). Inst. of Chemistry; Pfeffer, M.; Tulipan, M.; Mentler, A.; Wenzel, W.W. [Vienna University of Agricultural Sciences - BOKU Wien (Austria). Inst. of Soil Science

    1999-07-01

    Gas chromatography and high-performance liquid chromatography coupled to a double focusing sectorfield ICP-MS as sensitive element specific detector are used for the speciation of arsenic of liquid and gaseous emissions from soil samples, which were equilibrated in a microcosmos experiment. Speciation of liquid samples was performed by HPLC and hydride generation was used as introduction system to ICP-MS. An online prereduction step was introduced to enhance the sensitivity for As(V). A home-built and laboratory-ready transfer line from GC to ICP-MS is presented and quantification of As in gaseous emissions was performed by external calibration via hydride generation. The microcosmos experiment revealed only low production rates of organoarsenic compounds and reflected a limited capability of the biovolatilization experiment for the simulation of natural systems. (orig.) With 5 figs., 5 tabs., 29 refs.

  14. Species-specific isotope dilution analysis of mono-, di, and tri-butyltin compounds in sediment using gas chromatography-inductively coupled plasma mass spectrometry with synthesized 118Sn-enriched butyltins.

    Science.gov (United States)

    Inagaki, Kazumi; Takatsu, Akiko; Watanabe, Takuro; Aoyagi, Yoshie; Okamoto, Kensaku

    2003-03-01

    A species-specific isotope dilution (ID) method is described for the determination of mono-, di, and tri-butyltin compounds in sediment by gas chromatography-inductively coupled plasma mass spectrometry (GC-ICP-MS), where the mixture of 118Sn-enriched butyltin compounds synthesized in our laboratory was used as a spike. A correction method for the mass bias, a quantitative extraction of the butyltins from sediment, and an assay for the concentration of the standard solution for the reverse ID procedure were investigated to achieve a reliable ID analysis. The spike solution was added with tri-propyltin (TPrT), and the butyltins were extracted by mechanical shaking into acetic acid-tropolone-toluene. The extracted butyltins were ethylated with sodium tetraethylborate and measured by GC-ICP-MS. The mass bias correction factor for the butyltins was calculated with the measured area ratio of 120Sn/118Sn of TPrT in each chromatographic run, and the correction was carried out. The mass bias was well corrected with this in-run correction (the standard uncertainties of the corrected 120Sn/118Sn for the butyltins were in the range 0.03-0.45%, typically 0.25%, with triplicate measurement corresponding to 0.02-0.37% mass bias). The extraction efficiency of mono-butyltin (MBT) from sediment was improved by using tropolone-toluene as the solvent. Well-defined standard solutions for the reverse-ID procedure could be obtained by an assay for the purities of the natural abundance butyltin chloride reagents used for preparing the standard solutions. Overall uncertainties associated with the present method were estimated, where the sediment certified reference materials, PACS-2 and BCR 646, were analyzed. The uncertainty arising from the extraction was the main contributor to the overall uncertainties for MBT and di-butyltin (DBT) determinations, while with the case of tri-butyltin (TBT) determination the uncertainties arising from the purity of TBT chloride reagent used for

  15. Wireless Power Transmission Using Resonance Inductive Coupling

    Directory of Open Access Journals (Sweden)

    Prof. Vishal V. Pande,

    2014-04-01

    Full Text Available In this paper, we present the concept of transmitting power without using wires i.e.transmitting power as Magnetic waves from one place to another is in order to reduce the transmission and distribution losses. This concept is known as Resonance Inductive Coupling (RIC. We also discussed the technological developments in Wireless Power Transmission (WPT. The advantages, disadvantages, biological impacts and applications of WPT are also presented. Wireless power or wireless energy transmission is the transmission of electrical energy from a power source to an electrical load without man-made conductors. Wireless transmission is useful in cases where interconnecting wires are inconvenient, hazardous, or impossible. the proportion of energy received becomes critical only if it is too low for the signal to be distinguished from the background noise. With wireless power, efficiency is the more significant parameter. A large part of the energy sent out by the generating plant must arrive at the receiver or receivers to make the system economical.The most common form of wireless power transmission is carried out using direct induction followed by resonant magnetic induction. Other methods under consideration are electromagnetic radiation in the form of microwaves or lasers and electrical conduction through natural media

  16. Rapid determination of ¹³⁵Cs and precise ¹³⁵Cs/¹³⁷Cs atomic ratio in environmental samples by single-column chromatography coupled to triple-quadrupole inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Yang, Guosheng; Tazoe, Hirofumi; Yamada, Masatoshi

    2016-02-18

    For source identification, measurement of (135)Cs/(137)Cs atomic ratio not only provides information apart from the detection of (134)Cs and (137)Cs, but it can also overcome the application limit that measurement of the (134)Cs/(137)Cs ratio has due to the short half-life of (134)Cs (2.06 y). With the recent advancement of ICP-MS, it is necessary to improve the corresponding separation method for rapid and precise (135)Cs/(137)Cs atomic ratio analysis. A novel separation and purification technique was developed for the new generation of triple-quadrupole inductively coupled plasma-mass spectrometry (ICP-MS/MS). The simple chemical separation, incorporating ammonium molybdophosphate selective adsorption of Cs and subsequent single cation-exchange chromatography, removes the majority of isobaric and polyatomic interference elements. Subsequently, the ICP-MS/MS removes residual interference elements and eliminates the peak tailing effect of stable (133)Cs, at m/z 134, 135, and 137. The developed analytical method was successfully applied to measure (135)Cs/(137)Cs atomic ratios and (135)Cs activities in environmental samples (soil and sediment) for radiocesium source identification. PMID:26826700

  17. Isotope dilution inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    The potential of isotope dilution inductively coupled plasma mass spectrometry (ICP-MS) was evaluated for the determination of trace amounts of uranium and thorium in silicate rocks. Compared with conventional isotope dilution methods using thermal ionization mass spectrometers, the major benefit is a large increase in sample through-put without a significant decrease in precision and accuracy. This results from direct liquid sampling at atmospheric pressure and from the capability of measuring isotope ratios on raw solutions, without chemical separation of the analytes from the matrix elements. Isotope dilution ICP-MS alleviates the need for matrix-matched standards. Further, it is insensitive to possible causes of intensity drift (e.g., clogging of the plasma/mass spectrometer interface and defocusing of the ion beam) and to chemical effects (e.g. oxide formulation). Results obtained on some international rock standards are in good agreement with recommended values. (author). 26 refs.; 1 fig., tabs

  18. Titanium oxidation by rf inductively coupled plasma

    Science.gov (United States)

    Valencia-Alvarado, R.; de la Piedad-Beneitez, A.; López-Callejas, R.; Barocio, S. R.; Mercado-Cabrera, A.; Peña-Eguiluz, R.; Muñoz-Castro, A. E.; Rodríguez-Méndez, B. G.; de la Rosa-Vázquez, J. M.

    2014-05-01

    The development of titanium dioxide (TiO2) films in the rutile and anatase phases is reported. The films have been obtained from an implantation/diffusion and sputtering process of commercially pure titanium targets, carried out in up to 500 W plasmas. The experimental outcome is of particular interest, in the case of anatase, for atmospheric pollution degradation by photocatalysis and, as to the rutile phase, for the production of biomaterials required by prosthesis and implants. The reactor employed consists in a cylindrical pyrex-like glass vessel inductively coupled to a 13.56 MHz RF source. The process takes place at a 5×10-2 mbar pressure with the target samples being biased from 0 to -3000 V DC. The anatase phase films were obtained from sputtering the titanium targets over glass and silicon electrically floated substrates placed 2 cm away from the target. The rutile phase was obtained by implantation/diffusion on targets at about 700 °C. The plasma was developed from a 4:1 argon/oxygen mixture for ~5 hour processing periods. The target temperature was controlled by means of the bias voltage and the plasma source power. The obtained anatase phases did not require annealing after the plasma oxidation process. The characterization of the film samples was conducted by means of x-ray diffraction, scanning electron microscopy, x-ray photoelectron spectroscopy and Raman spectroscopy.

  19. Inductive Coupling of Power Converter’s – EMC

    Directory of Open Access Journals (Sweden)

    Irena Kováčová

    2009-07-01

    Full Text Available The paper presents a computer analysis of inductive coupling of theelectromagnetic compatibility (EMC problem. Its focus is on power electronics andelectrical drives and tests performed by a numerical computer simulation that can disclosesuite surprising findings about EMC.

  20. Progress in antenna coupled kinetic inductance detectors

    NARCIS (Netherlands)

    Baryshev, A.; Baselmans, J.J.A.; Freni, A.; Gerini, G.; Hoevers, H.; Iacono, A.; Neto, A.

    2011-01-01

    This paper describes the combined Dutch efforts toward the development of large wideband focal plane array receivers based on kinetic inductance detectors (KIDs). Taking into account strict electromagnetic and detector sensitivity requirements for future ground and space based observatories, this wo

  1. Validation of methodologies for the analysis of lead and methyl-ether in gasoline, using the techniques of atomic emission with plasma source coupled inductively and micellar liquid chromatography

    International Nuclear Information System (INIS)

    This study established and optimized the experimental variables for the lead quantization through the Icp-Aes technique, in aqueous media. A comparative study of several proposal methods, that appears in the literature for the extraction in aqueous media of the lead in gasoline was made. It determined that it is not possible, to make this procedure using the reaction of hydrolysis of tetraethyl lead. The op tim conditions were established, for the lead quantization in gasoline, using methyl-isobutyl-ketone and also ethanol as dis solvents. The conditions of the proposed methodologies were optimized, and the variables of analytical performance were defined. It was demonstrated, that it is possible to prepare lead dissolution patterns, in organic media, starting from inorganic salts of this metal. The techniques of chromatography of gases and of liquid chromatography of high pressure, in the analysis of methyl-ter butyl-ether (Mtbe), were compared. It demonstrated that it is possible, to quantize the Mtbe through the HPLC technique, and it found that the 'micellar' liquid chromatography. (author)

  2. Inductively coupled plasma mass spectrometery: an overview

    International Nuclear Information System (INIS)

    A general description of the instrumentation for an d analytical capabilities of ICP-MS will be given. The following areas will be emphasized: (1) characteristics of the ICP that make it an effective ion source; (2) extraction of ions from the ICP and the fundamental processes occurring therein; (3) techniques for focusing, mass analyzing, and detecting ions; (4) use of ICP-MS as an element or isotope-selective detector for chromatography; (5) sources of interferences and experimental ways to alleviate their effects; (6) isotope labelling studies of trace element metabolism in human nutrition; (7) representative analytical applications; and (8) diagnostic studies of ICPs by MS. Finally, the experimental techniques developed for ICP-MS have led to some innovative ways to observe emission from ICPs (direct probe sampling, extraction discharge emission, and afterglow emission), which will be described briefly

  3. Separation of seven arsenic compounds by high-performance liquid chromatography with on-line detection by hydrogen–argon flame atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, S. H.; Larsen, E. H.; Pritzl, G.;

    1992-01-01

    of mixtures of arsenic standards into the HPLC system were: arsenite, As(III) 1.1; arsenate, As(V) 1.4; MMA 1.4; DMA 0.7; AsB 0.3; AsC 0.5; and the TMAs 0.4. The HPLC-AAS system was used for the analysis of arsenic species in aqueous extracts of soil samples from a polluted land site. Only arsenate was found......Seven molecular forms of arsenic were separated by anion- and cation-exchange high-performance liquid chromatography (HPLC) with on-line detection by flame atomic absorption spectrometry (FAAS). The interfacing was established by a vented poly(tetrafluoroethylene) capillary tubing connecting...... the HPLC column to the nebulizer of the atomic absorption spectrometer. Arsenite, arsenate, monomethylarsonate (MMA) and dimethylarsinate (DMA) were separated from each other and from the co-injected cationic arsenic compounds, arsenobetaine (AsB), arsenocholine (AsC) and the tetramethylarsonium ion (TMAs...

  4. Separation of seven arsenic compounds by high performance liquid chromatography with on-line detection by hydrogen-argon flame atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, S. H.; Larsen, Erik Huusfeldt; Pritzl, G.;

    1992-01-01

    of mixtures of arsenic standards into the HPLC system were: arsenite, As(III) 1.1; arsenate, As(V) 1.4; MMA 1.4; DMA 0.7; AsB 0.3; AsC 0.5; and the TMAs 0.4. The HPLC-AAS system was used for the analysis of arsenic species in aqueous extracts of soil samples from a polluted land site. Only arsenate was found......Seven molecular forms of arsenic were separated by anion- and cation-exchange high-performance liquid chromatography (HPLC) with on-line detection by flame atomic absorption spectrometry (FAAS). The interfacing was established by a vented poly(tetrafluoroethylene) capillary tubing connecting...... the HPLC column to the nebulizer of the atomic absorption spectrometer. Arsenite, arsenate, monomethylarsonate (MMA) and dimethylarsinate (DMA) were separated from each other and from the co-injected cationic arsenic compounds, arsenobetaine (AsB), arsenocholine (AsC) and the tetramethylarsonium ion (TMAs...

  5. Determination Of Hafnium In Zirconium Dioxide Using Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    A method for determination of hafnium (Hf) in zirconium dioxide (ZrO2) using inductively coupled plasma mass spectrometry (ICP-MS) is proposed. The method involves the decomposition of ZrO2 sample, the chemical separation of Hf from zirconium (Zr) matrix by ion-exchange chromatography with sulfuric acid as a medium of sample solution and an eluent as well. The methods are suitable for analysis of Hf impurity in ZrO2, which is used as nuclear material. The procedure was well applied for determination of Hf in ZrO2 product of the Institute for Technology of Radioactive and Rare Elements (ITRRE), VAEI. (author)

  6. Estimation of detection limits in inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Prudnikov, E.D. [Earth`s Crust Inst., State Univ., St. Petersburg (Russian Federation); Barnes, R.M. [Department of Chemistry, University of Massachusetts, Amherst, MA (United States)

    1998-11-01

    The theoretical estimation of the detection limits in inductively coupled plasma mass spectrometry has been investigated. This calculation includes significant parameters of the ICP source and mass spectrometer. The calculated values show generally good agreement with experimental results. The development of a mathematical relationship may be useful for evaluation of instrumental parameters and sample introduction techniques. (orig.) With 1 tab., 28 refs.

  7. Zinc isotope discrimination effect in inductively coupled plasma mass spectrometer

    International Nuclear Information System (INIS)

    Inductively coupled plasma mass spectrometry (ICPMS) has recently been used for isotope ratio analysis. The isotope discrimination effect in the mass spectrometer is a primary factor contributing to loss of precision and accuracy in isotope ratio analysis. The discrimination effect of zinc isotopes was investigated by comparing the results obtained using a quadrupole type ICPMS with those obtained using a thermal ionization mass spectrometer

  8. Design And Construction Of Wireless Charging System Using Inductive Coupling

    Directory of Open Access Journals (Sweden)

    Do Lam Mung

    2015-06-01

    Full Text Available Abstract Wireless charging system described by using the method of inductive coupling. In this project oscillation circuit converts DC energy to AC energytransmitter coil to transmit magnetic field by passing frequency and then induce the receiver coil. The properties of Induction coupling are wavemagnetic field-wideband rangevery shortcm efficiencyhight and operation frequencyLF-bandseveral handred kHz.The project shows as a small charging for 5V battery of phone in this method. The system bases on coupling magnetic field then designed and constructed as two parts. There are transmitter part and receiver part. The transmitter coil transmitter part transmits coupling magnetic field to receiver coil receiver part by passing frequency at about 1.67MHz. The Amperes law Biot-Savart law and Faraday law are used to calculate the inductive coupling between the transmitter coil and the receiver coil. The calculation of this law shows how many power transfer in receiver part when how many distance between the transmitter coil and the receiver coil. The system is safe for users and neighbouring electronic devices. To get more accurate wireless charging system it needs to change the design of the following keywords.

  9. Superposition of Inductive and Capacitive Coupling in Superconducting LC Resonators

    Science.gov (United States)

    Gladchenko, Sergiy; Khalil, Moe; Lobb, C. J.; Wellstood, F. C.; Osborn, Kevin D.

    2011-06-01

    We present an experimental investigation of lumped-element superconducting LC resonators designed to provide different types of coupling to a transmission line. We have designed four resonator geometries including dipole and quadrupole configured inductors connected in parallel with low loss SiNx dielectric parallel-plate capacitors. The design of the resonator allows a small change in the symmetry of the inductor or grounding of the capacitor to allow LC resonators with: 1) inductive coupling, 2) capacitive coupling, 3) both types of coupling, or 4) greatly reduced coupling. We measured all four designs at a temperature of 30mK at different values of power. We compare the extracted data from the four resonator types and find that both capacitive and inductive coupling can be included and that when left off, only a minor change in the circuit design is necessary. We also find a variation in the measured loss tangent of less than a few percent, which is a test of the systematic precision of the measurement technique.

  10. Magnetic superlens-enhanced inductive coupling for wireless power transfer

    OpenAIRE

    Huang, Da; Urzhumov, Yaroslav; Smith, David R; Teo, Koon Hoo; Zhang, Jinyun

    2012-01-01

    We investigate numerically the use of a negative-permeability "perfect lens" for enhancing wireless power transfer between two current carrying coils. The negative permeability slab serves to focus the flux generated in the source coil to the receiver coil, thereby increasing the mutual inductive coupling between the coils. The numerical model is compared with an analytical theory that treats the coils as point dipoles separated by an infinite planar layer of magnetic material [Urzhumov et al...

  11. Superconducting atomic contacts inductively coupled to a microwave resonator

    OpenAIRE

    Janvier, C.; Tosi, L.; Girit, Ç. Ö.; Goffman, M.F.; Pothier, H.; Urbina, C.

    2014-01-01

    We describe and characterize a microwave setup to probe the Andreev levels of a superconducting atomic contact. The contact is part of a superconducting loop inductively coupled to a superconducting coplanar resonator. By monitoring the resonator reflection coefficient close to its resonance frequency as a function of both flux through the loop and frequency of a second tone we perform spectroscopy of the transition between two Andreev levels of highly transmitting channels of the contact. Th...

  12. Interference analysis on resonant inductive coupled wireless power transfer

    OpenAIRE

    Bou Balust, Elisenda; Alarcón Cot, Eduardo José; Sedwick, Raymond; Fisher, Peter

    2013-01-01

    Resonant Inductive Coupling Wireless Power Transfer is a key technology to provide an efficient and harmless wireless energy channel to consumer electronics, biomedical implants and wireless sensor networks. However, there are two factors that are limiting the applicability of this technology: the effects of distance variation between transmitter and receiver and the effects of interfering objects. While distance variation in WPT has been thoroughly studied, the effects of interfering objects...

  13. Volumetric loss quantification using ultrasonic inductively coupled transducers

    Science.gov (United States)

    Gong, Peng; Hay, Thomas R.; Greve, David W.; Oppenheim, Irving J.

    2015-03-01

    The pulse-echo method is widely used for plate and pipe thickness measurement. However, the pulse echo method does not work well for detecting localized volumetric loss in thick-wall tubes, as created by erosion damage, when the morphology of volumetric loss is irregular and can reflect ultrasonic pulses away from the transducer, making it difficult to detect an echo. In this paper, we propose a novel method using an inductively coupled transducer to generate longitudinal waves propagating in a thick-wall aluminum tube for the volumetric loss quantification. In the experiment, longitudinal waves exhibit diffraction effects during the propagation which can be explained by the Huygens-Fresnel principle. The diffractive waves are also shown to be significantly delayed by the machined volumetric loss on the inside surface of the thick-wall aluminum tube. It is also shown that the inductively coupled transducers can generate and receive similar ultrasonic waves to those from wired transducers, and the inductively coupled transducers perform as well as the wired transducers in the volumetric loss quantification when other conditions are the same.

  14. LLNL large-area inductively coupled plasma (ICP) source: Experiments

    International Nuclear Information System (INIS)

    We describe initial experiments with a large (76-cm diameter) plasma source chamber to explore the problems associated with large-area inductively coupled plasma (ICP) sources to produce high density plasmas useful for processing 400-mm semiconductor wafers. Our experiments typically use a 640-nun diameter planar ICP coil driven at 13.56 MHz. Plasma and system data are taken in Ar and N2 over the pressure range 3-50 mtorr. RF inductive power was run up to 2000W, but typically data were taken over the range 100-1000W. Diagnostics include optical emission spectroscopy, Langmuir probes, and B probes as well as electrical circuit measurements. The B and E-M measurements are compared with models based on commercial E-M codes. Initial indications are that uniform plasmas suitable for 400-mm processing are attainable

  15. Systematic analysis and experiment of inductive coupling and induced voltage for inductively coupled wireless implantable neurostimulator application

    International Nuclear Information System (INIS)

    The main strategy for wireless power transfer to implantable devices is to use inductive coupling technology. The induced voltage of implanted devices highly depends on factors such as mutual inductance between the external transmitter coil and the receiver coil, quality factor of the receiver circuit and operation frequency. In this paper, the mutual inductance under a variety of geometries of external coil and under the condition of different vertical distances, lateral displacements and angular misalignments between two coils were theoretically calculated and simulated. To ascertain the condition of maximum power transmission for certain coils’ position requirements, an LC tank (2.7 mm × 2 mm) consisting of a microfabricated gold inductor coil and a small surface mounted capacitor was designed and fabricated as the telemetric part of a neurostimulator. The induced voltage of the LC tank was measured in both air and artificial tissue media under different sizes of power coil and operation frequencies. As a result, the optimum size of a transmitter coil is selected to be of 4 mm inner radius with six turns of coil, while the whole coupling system operates at 94 MHz resonant frequency within 5–11 mm vertical distance, 0–4 mm lateral and 0°–50° angular misalignment between two coils. With the change of the above coils’ positions, the measured induced voltage drops within 30%, satisfying the surgical requirement for neurostimulator implantation. (paper)

  16. Multidimensional chromatography coupled to mass spectrometry in analysing complex proteomics samples

    NARCIS (Netherlands)

    Horvatovich, Peter; Hoekman, Berend; Govorukhina, Natalia; Bischoff, Rainer

    2010-01-01

    Multidimensional chromatography coupled to mass spectrometry (LC(n)-MS) provides more separation power and an extended measured dynamic concentration range to analyse complex proteomics samples than one dimensional liquid chromatography coupled to mass spectrometry (1D-LC-MS). This review gives an o

  17. SU-8 etching in inductively coupled oxygen plasma

    DEFF Research Database (Denmark)

    Rasmussen, Kristian Hagsted; Keller, Stephan Sylvest; Jensen, Flemming;

    2013-01-01

    Structuring or removal of the epoxy based, photo sensitive polymer SU-8 by inductively coupled plasma reactive ion etching (ICP-RIE) was investigated as a function of plasma chemistry, bias power, temperature, and pressure. In a pure oxygen plasma, surface accumulation of antimony from the photo......-initiator introduced severe roughness and reduced etch rate significantly. Addition of SF6 to the plasma chemistry reduced the antimony surface concentration with lower roughness and higher etch rate as an outcome. Furthermore the etch anisotropy could be tuned by controlling the bias power. Etch rates up to 800 nm...

  18. Quantum Effects of Mesoscopic Inductance and Capacity Coupling Circuits

    Institute of Scientific and Technical Information of China (English)

    LIU Jian-Xin; AN Zhan-Yuan; SONG Yong-Hua

    2006-01-01

    Using the quantum theory for a mesoscopic circuit based on the discretenes of electric charges, the finitedifference Schrodinger equation of the non-dissipative mesoscopic inductance and capacity coupling circuit is achieved.The Coulomb blockade effect, which is caused by the discreteness of electric charges, is studied. Appropriately choose the components in the circuits, the finite-difference Schrodinger equation can be divided into two Mathieu equations in p representation. With the WKBJ method, the currents quantum fluctuations in the ground states of the two circuits are calculated. The results show that the currents quantum zero-point fluctuations of the two circuits are exist and correlated.

  19. Superconducting atomic contacts inductively coupled to a microwave resonator

    Science.gov (United States)

    Janvier, C.; Tosi, L.; Girit, Ç. Ö.; Goffman, M. F.; Pothier, H.; Urbina, C.

    2014-11-01

    We describe and characterize a microwave setup to probe the Andreev levels of a superconducting atomic contact. The contact is part of a superconducting loop inductively coupled to a superconducting coplanar resonator. By monitoring the resonator reflection coefficient close to its resonance frequency as a function of both flux through the loop and frequency of a second tone we perform spectroscopy of the transition between two Andreev levels of highly transmitting channels of the contact. The results indicate how to perform coherent manipulation of these states.

  20. A double inductively coupled plasma for sterilization of medical devices

    International Nuclear Information System (INIS)

    A double inductively coupled low pressure plasma for sterilization of bio-medical materials is introduced. It is developed for homogeneous treatment of three-dimensional objects. The short treatment times and low temperatures allow the sterilization of heat sensitive materials like ultra-high-molecular-weight-polyethylene or polyvinyl chloride. Using a non-toxic atmosphere reduces the total process time in comparision with common methods. Langmuir probe measurements are presented to show the difference between ICP- and CCP-mode discharges, the spatial homogeneity and the influence on the sterilization efficiency. To know more about the sterilization mechanisms optical emission is measured and correlated with sterilization results

  1. A study of Trace Gold Chloride and Hydroxide Speciation in Weak Alkaline Solution by Ion Chromatography-Inductively Coupled Plasma Mass Spectrometry%离子色谱电感耦合等离子体质谱研究痕量氯金酸在弱碱性体系中金(Ⅲ)的形态

    Institute of Scientific and Technical Information of China (English)

    刘德晔; 朱醇; 马永建

    2012-01-01

    A method based on ion chromatography-inductively coupled plasma mass spectrometry(IC-ICP-MS) was developed to study trace gold chloride and hydroxide speciation in weak alkaline solu-tion. The results revealed that, the main compounds in weak alkaline solution were [AuCl2(OH)2]~ and [AuCKOH)3]-when the total Au mass was between 4. 0 30 ng. Unlike high HAuCl4 4H2O concentration, trace [AuCl2 (OH)2]~ could exist between pH 7. 0 to 10. 0, at least. Additional chlo-ride brought promotion to [AuCl2(OH)2]~ and reduction to CAuCl(OH)3]~. When pH was 7. 0 or chloride concentration was above 0. 050 mol/L, AuflE) would generate a compound which could not be flushed out of chromatography system. According to hydrolysis process. that compound was deduced as [AuCl3(OH)]-. The equilibrium constant K3 of [AuCl2(OH)2]- + OH ←[AuCl (OH)3]-+Cl always changed with pH values and chloride concentrations. Therefore, there might exist other factor to influence the trace Au(Ⅲ) hydrolysis.%采用离子色谱电感耦合等离子体质谱联用方法研究弱碱性体系下痕量氯金酸中Au(Ⅲ)的形态.结果表明:在弱碱性条件下,总金含量在4.0~30 ng之间,Au(Ⅲ)主要以[AuCl2( OH)2]-和[AuCl(OH)3]-的形式存在.与较高含量的氯金酸溶渡相比,痕量氯金酸溶液中的[AuCl2(OH)2]-至少可以在pH 7.0~10.0范围内存在.溶液外加的Cl-可使[AuCl2 (OH)2]-含量升高同时降低[AuCl (OH)3]-含量;当pH=7.0或Cl-浓度高于0.050 mol/L,会产生不随色谱流出的金络合物,根据水解过程推断该络合物为[AuC13 (OH)]-.在pH 8.0~10.0,Cl-浓度在0.000~0.020 mol/L时,[AuCl2(OH)2]-+OH-=[AuCl (OH)3]-+Cl-的水解平衡常数为不定值,说明痕量氯金酸的水解不仅受pH值和Cl-浓度影响,还受其它因素影响.

  2. Development of a low-cost inductively coupled argon plasma

    International Nuclear Information System (INIS)

    The aim of this investigation is to drastically reduce running costs of an inductively coupled plasma. This is done by reducing the argon consumption from 20 l/min to about 1 l/min. First, a sample introduction system operating on 0.1 l/min of carrier argon is described. This system ensures a high ratio of plasma argon and carrier argon even at the low total argon consumptions intended. Next, the developed low consumption plasma is presented. In the proposed design, air is blown perpendicularly against the outside of the torch. A different coil has been developed to make air-cooling efficient. Preliminary data on coupling efficiency for the air-cooled plasma are presented. A similarly low argon consumption has been achieved with water as an external coolant medium. It is concluded that a cheaper alternative to the current ICP has become available. (Auth.)

  3. Microwave Kinetic Inductance Detector with Selective Polarization Coupling

    Science.gov (United States)

    Wollack, Edward; U-yen, Kongpop; Stevenson, Thomas; Brown, Ari; Moseley, Samuel; Hsieh, Wen-Ting

    2013-01-01

    A conventional low-noise detector requires a technique to both absorb incident power and convert it to an electrical signal at cryogenic temperatures. This innovation combines low-noise detector and readout functionality into one device while maintaining high absorption, controlled polarization sensitivity, and broadband detection capability. The resulting far-infrared detectors can be read out with a simple approach, which is compact and minimizes thermal loading. The proposed microwave kinetic inductance detector (MKID) consists of three basic elements. The first is the absorptive section in which the incident power is coupled to a superconducting resonator at far-infrared frequency above its superconducting critical frequency (where superconductor becomes normal conductor). This absorber's shape effectively absorbs signals in the desired polarization state and is resonant at the radio frequency (RF) used for readout of the device. Control over the metal film used in the absorber allows realization of structures with either a 50% broadband or 100% resonance absorptance over a 30% fractional bandwidth. The second element is a microwave resonator - which is realized from the thin metal films used to make the absorber as transmission lines - whose resonance frequency changes due to a variation in its kinetic inductance. The resonator's kinetic inductance is a function of the power absorbed by the device. A low-loss dielectric (mono-crystalline silicon) is used in a parallel-plate transmission line structure to realize the desired superconducting resonators. There is negligible coupling among the adjacent elements used to define the polarization sensitivity of each detector. The final component of the device is a microwave transmission line, which is coupled to the resonator, and allows detection of changes in resonance frequency for each detector in the focal plane array. The spiral shape of the detector's absorber allows incident power with two polarizations to

  4. Extended-field electromagnetic model for inductively coupled plasma

    International Nuclear Information System (INIS)

    An extended-field (EF), two dimensional (2D) model formulation is proposed for inductively coupled plasma. By extending the calculating domain of the electromagnetic (EM) field outside of the plasma discharge region, the boundary conditions of vector potential used by the standard (ST) 2D model are replaced by simpler far field boundary conditions. The extended model converges faster than the standard formulation and gives rise to consistent solutions throughout the computational domain. Vector potential equations are solved with corresponding continuity, momentum, and energy transfer equations using the commercial code 'FLUENT'. The computational domain for vector potential equations are extended well beyond the induction coil region, while for all the other equations, computations are limited to the discharge region inside the plasma confinement tube. The computational results are compared with those obtained using the ST 2D model. The difference between the results of the two models is noted mostly in the entrance regions of the flow, and close to the induction coil. To validate the EF model, a load with constant electric conductivity is placed centrally in the coil region and the calculated radial profile of the axial magnetic field is compared with existing analytical solutions. The results are in good agreement within an uncertainty of 1%. (author)

  5. Inductively coupled plasma mass spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    The period of investigation for the previous general remarks on the progress of ICP-MS was from January, 1991 to September, 1993. In the investigation of this time, for the object of the Chemical Abstracts from January, 1994 to September, 1996, retrieval was carried out by using the STN International. As the key words, ICP-MS, Inductively Coupled Plasma Mass Spectrometry or Inductively Coupled Plasma Mass Spectrometer was used. The number of hit was 373 in 1994, 462 in 1995, and 356 as of September, 1996, 1191 in total. The cumulative number of the papers from 1980 to 1996 is shown. It is known how rapidly the ICP-MS has pervaded as the means of analysis. In order to cope with the enormous number of papers, this time, it was decided to do the review by limiting to the papers which were published in the main journals deeply related to analytical chemistry. As to the tendency in the last three years, it is summarized as how to overcome the spectrum interference and matrix effect in the ICP-MS and the trend of using the ICP-MS as the high sensitivity detector for separation techniques. The technical basic research of the ICP-MS on spectrum interference, sample introduction method and others and the analysis of living body samples are reported. (K.I.)

  6. Inductively coupled plasma mass spectrometry for stable isotope metabolic tracer studies of living systems

    Energy Technology Data Exchange (ETDEWEB)

    Luong, E.

    1999-05-10

    This dissertation focuses on the development of methods for stable isotope metabolic tracer studies in living systems using inductively coupled plasma single and dual quadrupole mass spectrometers. Sub-nanogram per gram levels of molybdenum (Mo) from human blood plasma are isolated by the use of anion exchange alumina microcolumns. Million-fold more concentrated spectral and matrix interferences such as sodium, chloride, sulfate, phosphate, etc. in the blood constituents are removed from the analyte. The recovery of Mo from the alumina column is 82 {+-} 5% (n = 5). Isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS) is utilized for the quantitative ultra-trace concentration determination of Mo in bovine and human blood samples. The average Mo concentration in reference bovine serum determined by this method is 10.2 {+-} 0.4 ng/g, while the certified value is 11.5 {+-} 1.1 ng/g (95% confidence interval). The Mo concentration of one pool of human blood plasma from two healthy male donors is 0.5 {+-} 0.1 ng/g. The inductively coupled plasma twin quadrupole mass spectrometer (ICP-TQMS) is used to measure the carbon isotope ratio from non-volatile organic compounds and bio-organic molecules to assess the ability as an alternative analytical method to gas chromatography combustion isotope ratio mass spectrometry (GC-combustion-IRMS). Trytophan, myoglobin, and {beta}-cyclodextrin are chosen for the study, initial observation of spectral interference of {sup 13}C{sup +} with {sup 12}C{sup 1}H{sup +} comes from the incomplete dissociation of myoglobin and/or {beta}-cyclodextrin.

  7. Determination of rare earth elements by liquid chromatographic separation using inductively coupled plasma mass spectrometric detection

    International Nuclear Information System (INIS)

    High-performance liquid chromatography (HPLC) is used to separate the rare earth elements (REEs) prior to detection by inductively coupled plasma mass spectrometry (ICP-MS). The use of HPLC-ICP-MS in series combines the separation power and speed of HPLC with the sensitivity, isotopic selectivity and speed of ICP-MS. The detection limits for the REEs are in the sub-ng ml-1 range and the response is linear over four orders of magnitude. A preliminary comparison of isotope dilution and external standard results for the determination of REEs in National Institute of Standards and Technology (NIST) Standard Reference Material (SRM 1633a) Fly Ash is presented. (author)

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

    International Nuclear Information System (INIS)

    Inductively coupled plasma -- mass spectrometry (ICP-MS) was used to concurrently determine multiple long-lived (t1/2 > 104 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 (239Pu) to 2 μBq L-1 (235U) Hydride adducts of 232Th and 238U interfered with the determinations of 233U 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 230Th, 239Pu, and the 234U/238U 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 234U and 238U activities

  9. Using Some Coupled Numerical Models in Problems of Designing an Inductive Electrothermal Equipment

    Directory of Open Access Journals (Sweden)

    LEUCA Teodor

    2014-05-01

    Full Text Available This paper focuses on the numerical modeling of coupling the electromagnetic and the thermal field, in the process of inductive heating, for inductive electrothermal equipments. Numerical results are carried out by using a FLUX2D application.

  10. Exchange-coupled magnetic nanoparticles for efficient heat induction

    Science.gov (United States)

    Lee, Jae-Hyun; Jang, Jung-Tak; Choi, Jin-Sil; Moon, Seung Ho; Noh, Seung-Hyun; Kim, Ji-Wook; Kim, Jin-Gyu; Kim, Il-Sun; Park, Kook In; Cheon, Jinwoo

    2011-07-01

    The conversion of electromagnetic energy into heat by nanoparticles has the potential to be a powerful, non-invasive technique for biotechnology applications such as drug release, disease treatment and remote control of single cell functions, but poor conversion efficiencies have hindered practical applications so far. In this Letter, we demonstrate a significant increase in the efficiency of magnetic thermal induction by nanoparticles. We take advantage of the exchange coupling between a magnetically hard core and magnetically soft shell to tune the magnetic properties of the nanoparticle and maximize the specific loss power, which is a gauge of the conversion efficiency. The optimized core-shell magnetic nanoparticles have specific loss power values that are an order of magnitude larger than conventional iron-oxide nanoparticles. We also perform an antitumour study in mice, and find that the therapeutic efficacy of these nanoparticles is superior to that of a common anticancer drug.

  11. Transition of electron kinetics in weakly magnetized inductively coupled plasmas

    International Nuclear Information System (INIS)

    Transition of the electron kinetics from nonlocal to local regime was studied in weakly magnetized solenoidal inductively coupled plasma from the measurement of the electron energy probability function (EEPF). Without DC magnetic field, the discharge property was governed by nonlocal electron kinetics at low gas pressure. The electron temperatures were almost same in radial position, and the EEPFs in total electron energy scale were radially coincided. However, when the DC magnetic field was applied, radial non-coincidence of the EEPFs in total electron energy scale was observed. The electrons were cooled at the discharge center where the electron heating is absent, while the electron temperature was rarely changed at the discharge boundary with the magnetic field. These changes show the transition from nonlocal to local electron kinetics and the transition is occurred when the electron gyration diameter was smaller than the skin depth. The nonlocal to local transition point almost coincided with the calculation results by using nonlocal parameter and collision parameter

  12. A new nebulizer for inductively coupled plasma spectrometry

    International Nuclear Information System (INIS)

    A nebulizer for use in Inductively Coupled Plasma Emission Spectroscopy (ICP-ES) is designed. An unusual concept is used to generate the aerosol. The system is mechanically reliable, relatively simple and cheap to construct compared to the currently available commercial systems. The effect of geometrical design parameters (e.g. the droplet size mass distribution of the aerosol particles) on performance of the system is presented. The analytical merit of the newly designed system is determined by measuring its analytical performance. Detection limits and analytical range are measured for Cu, Ag, Au, Pt, Pb, Cd, V, Fe, Mn, Mo, B, Se and Zn. These values are compared with detection limits and analytical ranges obtained with commercial systems. The persistence of memory effects is found to be the major disadvantage of the system. Results are presented showing these effects and possible ways to eliminate them. (author)

  13. Monitoring microbial metabolites using an inductively coupled resonance circuit

    Science.gov (United States)

    Karnaushenko, Daniil; Baraban, Larysa; Ye, Dan; Uguz, Ilke; Mendes, Rafael G.; Rümmeli, Mark H.; de Visser, J. Arjan G. M.; Schmidt, Oliver G.; Cuniberti, Gianaurelio; Makarov, Denys

    2015-08-01

    We present a new approach to monitor microbial population dynamics in emulsion droplets via changes in metabolite composition, using an inductively coupled LC resonance circuit. The signal measured by such resonance detector provides information on the magnetic field interaction with the bacterial culture, which is complementary to the information accessible by other detection means, based on electric field interaction, i.e. capacitive or resistive, as well as optical techniques. Several charge-related factors, including pH and ammonia concentrations, were identified as possible contributors to the characteristic of resonance detector profile. The setup enables probing the ionic byproducts of microbial metabolic activity at later stages of cell growth, where conventional optical detection methods have no discriminating power.

  14. High voltage breakdown in an inductively coupled ion source

    International Nuclear Information System (INIS)

    An inductively coupled plasma source, designed for ion beam applications, is allowed to float up to several kilovolt positive. If one side of the radio frequency (rf) antenna is grounded and the dielectric source tube and the surrounding air are allowed to reach a threshold temperature corona breakdown at the rf antenna occurs. The experiments presented here show that a dc corona can be ignited with the presence of a dielectric barrier, which normally precludes dc breakdown. The formation of a negative barrier corona initiates a transition to a continuous arc from the rf antenna to the source tube. It is suggested that the onset of the first filaments heat the dielectric locally, such that the dielectric strength drops. DC current channels are then formed in the source tube, allowing a resistive corona with continuous arcs to exist

  15. Molecular Nitrogen Vibrational Temperature in an Inductively Coupled Plasma

    Institute of Scientific and Technical Information of China (English)

    康正德; 蒲以康

    2002-01-01

    Using a technique applied previously to vibrationally excited molecular nitrogen (N*2) in the region of daytime and nighttime aurora, the emission intensity of the N2 second positive band system in an inductively coupled plasma (ICP) has been analysed and the vibrational temperature of nitrogen molecules in the ICP is thus determined. The result shows that the vibrational temperature increases with the increase of the neutral gas pressure from 0.04Pa to 10Pa, then decreases with the further increase of the pressure from 10Pa to 100Pa. Also,this is explained by using the Boltzmann relation between the vibrational temperature and the concentration of the vibrationally excited N*2(X1∑+g ) molecules.

  16. Matrix effects in inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Xiaoshan

    1995-07-07

    The inductively coupled plasma is an electrodeless discharge in a gas (usually Ar) at atmospheric pressure. Radio frequency energy generated by a RF power source is inductively coupled to the plasma gas through a water cooled load coil. In ICP-MS the {open_quotes}Fassel{close_quotes} TAX quartz torch commonly used in emission is mounted horizontally. The sample aerosol is introduced into the central flow, where the gas kinetic temperature is about 5000 K. The aerosol is vaporized, atomized, excited and ionized in the plasma, and the ions are subsequently extracted through two metal apertures (sampler and skimmer) into the mass spectrometer. In ICP-MS, the matrix effects, or non-spectroscopic interferences, can be defined as the type of interferences caused by dissolved concomitant salt ions in the solution. Matrix effects can be divided into two categories: (1) signal drift due to the deposition of solids on the sampling apertures; and/or (2) signal suppression or enhancement by the presence of the dissolved salts. The first category is now reasonably understood. The dissolved salts, especially refractory oxides, tend to deposit on the cool tip of the sampling cone. The clogging of the orifices reduces the ion flow into the ICP-MS, lowers the pressure in the first stage of ICP-MS, and enhances the level of metal oxide ions. Because the extent of the clogging increases with the time, the signal drifts down. Even at the very early stage of the development of ICP-MS, matrix effects had been observed. Houk et al. found out that the ICP-MS was not tolerant to solutions containing significant amounts of dissolved solids.

  17. Matrix effects in inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    The inductively coupled plasma is an electrodeless discharge in a gas (usually Ar) at atmospheric pressure. Radio frequency energy generated by a RF power source is inductively coupled to the plasma gas through a water cooled load coil. In ICP-MS the open-quotes Fasselclose quotes TAX quartz torch commonly used in emission is mounted horizontally. The sample aerosol is introduced into the central flow, where the gas kinetic temperature is about 5000 K. The aerosol is vaporized, atomized, excited and ionized in the plasma, and the ions are subsequently extracted through two metal apertures (sampler and skimmer) into the mass spectrometer. In ICP-MS, the matrix effects, or non-spectroscopic interferences, can be defined as the type of interferences caused by dissolved concomitant salt ions in the solution. Matrix effects can be divided into two categories: (1) signal drift due to the deposition of solids on the sampling apertures; and/or (2) signal suppression or enhancement by the presence of the dissolved salts. The first category is now reasonably understood. The dissolved salts, especially refractory oxides, tend to deposit on the cool tip of the sampling cone. The clogging of the orifices reduces the ion flow into the ICP-MS, lowers the pressure in the first stage of ICP-MS, and enhances the level of metal oxide ions. Because the extent of the clogging increases with the time, the signal drifts down. Even at the very early stage of the development of ICP-MS, matrix effects had been observed. Houk et al. found out that the ICP-MS was not tolerant to solutions containing significant amounts of dissolved solids

  18. Trace analysis of acrylamide by high-performance thin-layer chromatography coupled to mass spectrometry

    OpenAIRE

    Alpmann, Alexander

    2011-01-01

    Planar-chromatography (High-Performance Thin-Layer Chromatography, HPTLC) is a rapid and cost-effective offline separation method. Through advances in the automatization of each step the system reproducibility, from application and development to detection, has been improved. This makes planar-chromatography a highly reliable technique. HPTLC shows a couple of features that make it unique. There is great flexibility concerning application, development and detection that distinguishes HPTLC fr...

  19. Investigations of the use of inductively coupled plasma emissions for chemical analysis

    Science.gov (United States)

    Heine, D. R.

    Investigations of applications of the inductively coupled plasma (ICP) for analytical atomic emission spectroscopy are performed. Emissions below 185 nm, analysis of wear metals in lubricating oils, and use of the ICP as a selective detector for high performance liquid chromatography (HPLC) are studied. A unique plasma coolant tube containing a side arm which allows direct observation of the discharge is used to investigate emissions in the vacuum ultraviolet spectral region between 120 and 185 nm. Emission from elements which do not emit radiation in the visible region are observed. A heated sample introduction system attached to a Babington nebulizer is investigated as a means to aerosolize lubricating oils for introduction into the ICP. This allows direct analysis of wear metals in oil samples without requiring the usual sample dilutions. The ICP is used as a selective detector for HPLC. Nucleotides separated by anion exchange chromatography are determined in the ICP by observing phosphorous emissions. Methanol and acetonitrile used for reverse phase HPLC are successfully run in the IPC.

  20. Sulfur-based absolute quantification of proteins using isotope dilution inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Lee, Hyun-Seok; Heun Kim, Sook; Jeong, Ji-Seon; Lee, Yong-Moon; Yim, Yong-Hyeon

    2015-10-01

    An element-based reductive approach provides an effective means of realizing International System of Units (SI) traceability for high-purity biological standards. Here, we develop an absolute protein quantification method using double isotope dilution (ID) inductively coupled plasma mass spectrometry (ICP-MS) combined with microwave-assisted acid digestion for the first time. We validated the method and applied it to certify the candidate protein certified reference material (CRM) of human growth hormone (hGH). The concentration of hGH was determined by analysing the total amount of sulfur in hGH. Next, the size-exclusion chromatography method was used with ICP-MS to characterize and quantify sulfur-containing impurities. By subtracting the contribution of sulfur-containing impurities from the total sulfur content in the hGH CRM, we obtained a SI-traceable certification value. The quantification result obtained with the present method based on sulfur analysis was in excellent agreement with the result determined via a well-established protein quantification method based on amino acid analysis using conventional acid hydrolysis combined with an ID liquid chromatography-tandem mass spectrometry. The element-based protein quantification method developed here can be generally used for SI-traceable absolute quantification of proteins, especially pure-protein standards.

  1. Studies of selenium and xenon in inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bricker, T.

    1994-07-27

    Since its development, inductively coupled plasma mass spectrometry (ICP-MS) has been a widely used analytical technique. ICP-MS offers low detection limits, easy determination of isotope ratios, and simple mass spectra from analyte elements. ICP-MS has been successfully employed for many applications including geological, environmental, biological, metallurgical, food, medical, and industrial. One specific application important to many areas of study involves elemental speciation by using ICP-MS as an element specific detector interfaced to liquid chromatography. Elemental speciation information is important and cannot be obtained by atomic spectrometric methods alone which measure only the total concentration of the element present. Part 1 of this study describes the speciation of selenium in human serum by size exclusion chromatography (SEC) and detection by ICP-MS. Although ICP-MS has been widely sued, room for improvement still exists. Difficulties in ICP-MS include noise in the background, matrix effects, clogging of the sampling orifice with deposited solids, and spectral interference caused by polyatomic ions. Previous work has shown that the addition of xenon into the central channel of the ICP decreases polyatomic ion levels. In Part 2 of this work, a fundamental study involving the measurement of the excitation temperature is carried out to further understand xenon`s role in the reduction of polyatomic ions. 155 refs.

  2. Studies of selenium and xenon in inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Since its development, inductively coupled plasma mass spectrometry (ICP-MS) has been a widely used analytical technique. ICP-MS offers low detection limits, easy determination of isotope ratios, and simple mass spectra from analyte elements. ICP-MS has been successfully employed for many applications including geological, environmental, biological, metallurgical, food, medical, and industrial. One specific application important to many areas of study involves elemental speciation by using ICP-MS as an element specific detector interfaced to liquid chromatography. Elemental speciation information is important and cannot be obtained by atomic spectrometric methods alone which measure only the total concentration of the element present. Part 1 of this study describes the speciation of selenium in human serum by size exclusion chromatography (SEC) and detection by ICP-MS. Although ICP-MS has been widely sued, room for improvement still exists. Difficulties in ICP-MS include noise in the background, matrix effects, clogging of the sampling orifice with deposited solids, and spectral interference caused by polyatomic ions. Previous work has shown that the addition of xenon into the central channel of the ICP decreases polyatomic ion levels. In Part 2 of this work, a fundamental study involving the measurement of the excitation temperature is carried out to further understand xenon's role in the reduction of polyatomic ions. 155 refs

  3. Determination of myo-inositol hexakisphosphate (phytate) in urine by inductively coupled plasma atomic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Grases, F.; Perello, J.; Isern, B.; Prieto, R.M

    2004-05-10

    Myo-inositol hexakisphosphate (phytate) is a substance present in urine with an important role in preventing calcium renal calculi development. In spite of this, the use of urinary phytate levels on stone-formers' evaluation and treatment is still notably restricted as a consequence of the enormous difficulty to analyze this substance in urine. In this paper, a simple procedure for routinary urinary phytate determination based on phosphorus determination through inductively coupled plasma atomic emission spectrometry is described. The method only requires a previous separation of phytate from other components by column anion exchange chromatography. The working linear range used was 0-2 mg l{sup -1} phosphorus (0-7 mg l{sup -1} phytate). The limit of detection was 64 {mu}g l{sup -1} of phytate and the limit of quantification was 213 {mu}g l{sup -1}. The relative standard deviation (R.S.D.) for 1.35 mg l{sup -1} phytate was 2.4%. Different urine samples were analyzed using an alternative analytical methodology based on gas chromatography (GC)/mass detection used for inositol determination (phytate was previously hydrolyzed), resulting both methods comparable using as criterion to assess statistical significance P<0.05.

  4. Magnetic superlens-enhanced inductive coupling for wireless power transfer

    Science.gov (United States)

    Huang, Da; Urzhumov, Yaroslav; Smith, David R.; Hoo Teo, Koon; Zhang, Jinyun

    2012-03-01

    We investigate numerically the use of a negative-permeability "perfect lens" for enhancing wireless power transfer between two current carrying coils. The negative permeability slab serves to focus the flux generated in the source coil to the receiver coil, thereby increasing the mutual inductive coupling between the coils. The numerical model is compared with an analytical theory that treats the coils as point dipoles separated by an infinite planar layer of magnetic material [Urzhumov et al., Phys. Rev. B 19, 8312 (2011)]. In the limit of vanishingly small radius of the coils, and large width of the metamaterial slab, the numerical simulations are in excellent agreement with the analytical model. Both the idealized analytical and realistic numerical models predict similar trends with respect to metamaterial loss and anisotropy. Applying the numerical models, we further analyze the impact of finite coil size and finite width of the slab. We find that, even for these less idealized geometries, the presence of the magnetic slab greatly enhances the coupling between the two coils, including cases where significant loss is present in the slab. We therefore conclude that the integration of a metamaterial slab into a wireless power transfer system holds promise for increasing the overall system performance.

  5. Inductively Coupled Plasma Zoom-Time-of-Flight Mass Spectrometry

    Science.gov (United States)

    Dennis, Elise A.; Ray, Steven J.; Enke, Christie G.; Hieftje, Gary M.

    2016-03-01

    A zoom-time-of-flight mass spectrometer has been coupled to an inductively coupled plasma (ICP) ionization source. Zoom-time-of-flight mass spectrometry (zoom-TOFMS) combines two complementary types of velocity-based mass separation. Specifically, zoom-TOFMS alternates between conventional, constant-energy acceleration (CEA) TOFMS and energy-focused, constant-momentum acceleration (CMA) (zoom) TOFMS. The CMA mode provides a mass-resolution enhancement of 1.5-1.7× over CEA-TOFMS in the current, 35-cm ICP-zoom-TOFMS instrument geometry. The maximum resolving power (full-width at half-maximum) for the ICP-zoom-TOFMS instrument is 1200 for CEA-TOFMS and 1900 for CMA-TOFMS. The CMA mode yields detection limits of between 0.02 and 0.8 ppt, depending upon the repetition rate and integration time—compared with single ppt detection limits for CEA-TOFMS. Isotope-ratio precision is shot-noise limited at approximately 0.2% relative-standard deviation (RSD) for both CEA- and CMA-TOFMS at a 10 kHz repetition rate and an integration time of 3-5 min. When the repetition rate is increased to 43.5 kHz for CMA, the shot-noise limited, zoom-mode isotope-ratio precision is improved to 0.09% RSD for the same integration time.

  6. An inductively coupled miniature plasma jet source at microwave frequencies

    International Nuclear Information System (INIS)

    A miniature double plasma jet source driven at microwave frequencies (∼2.45 GHz) was developed and analyzed. The source consists of a copper resonator (screened within an aluminum housing) that excites plasma simultaneously in two alumina tubes of 5 mm internal diameter. Field and plasma simulations were performed using the software Comsol. Assuming a homogeneous electron distribution we calculate the plasma impedance as a function of its conductivity. The electron density and the plasma conductivity are estimated as a function of the absorbed power in plasma for argon and oxygen. Experimentally it was shown that the microwave energy is coupled into oxygen plasma with an efficiency of >85% and into argon plasma with ∼30%. The source efficiently produces atomic oxygen and nitrogen as is demonstrated by plasma-enhanced atomic layer deposition. Finally, the time evolution during ignition, the transition from low efficient capacitive to highly efficient inductive coupling, the free electron distribution as a function of time and other parameters are analyzed. (paper)

  7. Investigations on Capacitor Compensation Topologies Effects of Different Inductive Coupling Links Configurations

    Directory of Open Access Journals (Sweden)

    Norezmi Jamal

    2015-06-01

    Full Text Available This paper presents investigations on capacitor compensation topologies with different inductive coupling links for loosely coupled inductive power transfer (IPT system. In general, the main constraint of the loosely coupled IPT system is power losses due to the large leakage inductances. Therefore, to overcome the aforementioned problem, in this work, capacitor compensation is proposed to be used by adding an external capacitor to the system. By using this approach, the resonant inductive coupling can be achieved efficiently and hence the efficiency of the system is also increased significantly. This paper analyzes the performance of two different compensation topologies, which are primary series-secondary series (SS and primary series- secondary parallel (SP topology. The performance of such topologies is evaluated through the experimental results at 1MHz operating frequency for different types of inductive coupling. From the results, SS topology produces a high power transfer but SP topology gives better efficiency.

  8. Etching of oxynitride thin films using inductively coupled plasma

    International Nuclear Information System (INIS)

    In this study, silicon oxynitride (SiON) has been etched in a C2F6 inductively coupled plasma. The process parameters examined include a radio frequency source power, bias power, pressure, and C2F6 flow rate. For process optimization, a statistical experimental design was employed to investigate parameter effects under various plasma conditions. The etch rate increased almost linearly with increasing the source or bias power. Main effect analysis revealed that the etch rate is dominated by the source power. The C2F6 flow rate exerted the least impact on both etch rate and profile angle. It was estimated that the C2F6 effect is transparent only as the etchant is supplied sufficiently. Depending on the pressure levels, the etch rate varied in a complicated way. Parameter effects on the profile angle were very small and the profile angle varied between 83 deg. and 87 deg. for all etching experiments. In nearly all experiments, microtrenching was observed. The etch rate and profile angle, optimized at 1000 W source power, 30 W bias power, 6 mTorr pressure, and 60 sccm C2F6 flow rate, are 434 nm/min and 86 deg., respectively

  9. AETHER: A simulation platform for inductively coupled plasma

    Science.gov (United States)

    Turkoz, Emre; Celik, Murat

    2015-04-01

    An in-house code is developed to simulate the inductively coupled plasma (ICP). The model comprises the fluid, electromagnetic and transformer submodels. Fluid equations are solved to evaluate the plasma flow parameters, including the plasma and neutral densities, ion and neutral velocities, electron flux, electron temperature, and electric potential. The model relies on the ambipolar approximation and offers the evaluation of plasma parameters without solving the sheath region. The electromagnetic model handles the calculation of the electric and magnetic fields using the magnetic vector potential. The transformer model captures the effect of the matching circuit utilized in laboratory experiments for RF power deposition. The continuity and momentum equations are solved using finite volume method. The energy, electric potential, and magnetic vector potential equations are solved using finite difference method. The resulting linear systems of equations are solved with iterative solvers including Jacobi and GMRES. The code is written using the C++ programming language, it works in parallel and has graphical user interface. The model is applied to study ICP characteristics of a plasma confined within a cylindrical chamber with dielectric walls for two different power deposition cases. The results obtained from the developed model are verified using the plasma module of COMSOL Multiphysics. The model is also applied to a plasma source configuration, and it is demonstrated that there is an overall increase in the plasma potential when current is extracted from ICP with a biased wall electrode.

  10. Negative ion density in inductively coupled chlorine plasmas

    International Nuclear Information System (INIS)

    Laser photodetachment spectroscopy has been used to infer the density of chlorine negative ions in an inductively coupled chlorine plasma. Time dependent, excess electron density produced by photodetaching electrons from Cl- was detected by a microwave interferometer operating at 80 GHz. By focusing the microwave probe beam through the center of the discharge, negative ion density measurements could be performed in a small, 1.5 cm3, volume. As the rf power into the plasma increased from 155 to 340 W at 20 mTorr, the Cl- density in the center of the bulk plasma increased from 3.4 to 5.2x1011 cm-3. As the pressure was increased from 15 to 50 mTorr at 240 W, the Cl- density increased from 3.5 to 5x1011 cm3. Over this parameter space, the negative ion density equaled the electron density to within a factor of 2. The negative ion radial distribution was relatively constant, with a 20% decrease in the center of the plasma for some operating conditions. When the surface of the bias electrode was changed from stainless steel to silicon, the electron density remained constant but the Cl- density decreased by a factor of 2 to 3. copyright 1996 American Vacuum Society

  11. Chemically active species in an Oxygen Inductively Coupled Plasma

    Science.gov (United States)

    Ly, Nathaniel; Boffard, John; Lin, Chun; Wendt, Amy; Radovanov, Svetlana; Persing, Harold; Likhanskii, Alexandre

    2015-09-01

    Oxygen plasmas are used in a wide variety of applications including ion implantation and photoresist striping. Here we combine noninvasive optical emission spectroscopy (OES) measurements and numerical simulations to investigate the plasma parameters in both oxygen inductively coupled plasmas (ICP) and oxygen-argon ICPs. An emission model makes use of available electron impact excitation cross sections for atomic and molecular oxygen to relate measured O and O2+emission intensities to corresponding plasma parameters, including the electron temperature, electron density, and the dissociation fraction of the neutral oxygen. For plasma simulations we use the CRTRS, 2D/3D code that selfconsistently solves for ICP power deposition, electrostatic potential and plasma dynamics in the driftdiffusion approximation (or full momentum equations). Comparison of the experimental OES measurements are used to check the validity of the plasma simulation which yields results that the OES approach has difficulty in measuring including the relative fluxes of O+ and O2+,which is important for ion implantation. The authors acknowledge support from NSF Grant PHY-1068670, and from Dr. Shahid Rauf for developing CRTRS.

  12. Chemical characterization of materials by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    An Inductively Coupled Plasma Mass Spectrometer was procured for trace elemental determination in diverse samples. Since its installation a number of analytical measurements have been carried out on different sample matrices. These include chemical quality control measurements of nuclear fuel and other materials such as uranium metal. Uranium peroxide, ADU, ThO2, UO2; isotopic composition of B, Li; chemical characterization of simulated ThO2 + 2%UO2 fuel; sodium zirconium phosphate and trace metallic elements in zirconium; Antarctica rock samples and wet phosphoric acid. Necessary separation methodologies required for effective removal of matrix were indigenously developed. In addition, a rigorous analytical protocol, which includes various calibration methodologies such as mass calibration, response calibration, detector cross calibration and linearity check over the entire dynamic range of 109 required for quantitative determination of elements at trace and ultra trace level,, has been standardized. This report summarizes efforts of RACD that have been put in this direction for the application of ICP-MS for analytical measurements. (author)

  13. Separation Of Uranium And Plutonium Isotopes For Measurement By Multi Collector Inductively Coupled Plasma Mass Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Martinelli, R E; Hamilton, T F; Williams, R W; Kehl, S R

    2009-03-29

    Uranium (U) and plutonium (Pu) isotopes in coral soils, contaminated by nuclear weapons testing in the northern Marshall Islands, were isolated by ion-exchange chromatography and analyzed by mass spectrometry. The soil samples were spiked with {sup 233}U and {sup 242}Pu tracers, dissolved in minerals acids, and U and Pu isotopes isolated and purified on commercially available ion-exchange columns. The ion-exchange technique employed a TEVA{reg_sign} column coupled to a UTEVA{reg_sign} column. U and Pu isotope fractions were then further isolated using separate elution schemes, and the purified fractions containing U and Pu isotopes analyzed sequentially using multi-collector inductively coupled plasma mass spectrometer (MCICP-MS). High precision measurements of {sup 234}U/{sup 235}U, {sup 238}U/{sup 235}U, {sup 236}U/{sup 235}U, and {sup 240}Pu/{sup 239}Pu in soil samples were attained using the described methodology and instrumentation, and provide a basis for conducting more detailed assessments of the behavior and transfer of uranium and plutonium in the environment.

  14. Three-phase inductive-coupled structures for contactless PHEV charging system

    Science.gov (United States)

    Lee, Jia-You; Shen, Hung-Yu; Li, Cheng-Bin

    2016-07-01

    In this article, a new-type three-phase inductive-coupled structure is proposed for the contactless plug-in hybrid electric vehicle (PHEV) charging system regarding with SAE J-1773. Four possible three-phase core structures are presented and subsequently investigated by the finite element analysis. To study the correlation between the core geometric parameter and the coupling coefficient, the magnetic equivalent circuit model of each structure is also established. In accordance with the simulation results, the low reluctance and the sharing of flux path in the core material are achieved by the proposed inductive-coupled structure with an arc-shape and three-phase symmetrical core material. It results in a compensation of the magnetic flux between each phase and a continuous flow of the output power in the inductive-coupled structure. Higher coupling coefficient between inductive-coupled structures is achieved. A comparison of coupling coefficient, mutual inductance, and self-inductance between theoretical and measured results is also performed to verify the proposed model. A 1 kW laboratory scale prototype of the contactless PHEV charging system with the proposed arc-shape three-phase inductive-coupled structure is implemented and tested. An overall system efficiency of 88% is measured when two series lithium iron phosphate battery packs of 25.6 V/8.4 Ah are charged.

  15. An investigation of algebraic quantum dynamics for mesoscopic coupled electric circuits with mutual inductance

    Science.gov (United States)

    Pahlavani, H.; Kolur, E. Rahmanpour

    2016-08-01

    Based on the electrical charge discreteness, the Hamiltonian operator for the mutual inductance coupled quantum mesoscopic LC circuits has been found. The persistent current on two driven coupled mesoscopic electric pure L circuits (two quantum loops) has been obtained by using algebraic quantum dynamic approach. The influence of the mutual inductance on energy spectrum and quantum fluctuations of the charge and current for two coupled quantum electric mesoscopic LC circuits have been investigated.

  16. A tightly coupled non-equilibrium model for inductively coupled radio-frequency plasmas

    International Nuclear Information System (INIS)

    The objective of the present work is the development of a tightly coupled magneto-hydrodynamic model for inductively coupled radio-frequency plasmas. Non Local Thermodynamic Equilibrium (NLTE) effects are described based on a hybrid State-to-State approach. A multi-temperature formulation is used to account for thermal non-equilibrium between translation of heavy-particles and vibration of molecules. Excited electronic states of atoms are instead treated as separate pseudo-species, allowing for non-Boltzmann distributions of their populations. Free-electrons are assumed Maxwellian at their own temperature. The governing equations for the electro-magnetic field and the gas properties (e.g., chemical composition and temperatures) are written as a coupled system of time-dependent conservation laws. Steady-state solutions are obtained by means of an implicit Finite Volume method. The results obtained in both LTE and NLTE conditions over a broad spectrum of operating conditions demonstrate the robustness of the proposed coupled numerical method. The analysis of chemical composition and temperature distributions along the torch radius shows that: (i) the use of the LTE assumption may lead to an inaccurate prediction of the thermo-chemical state of the gas, and (ii) non-equilibrium phenomena play a significant role close the walls, due to the combined effects of Ohmic heating and macroscopic gradients

  17. A tightly coupled non-equilibrium model for inductively coupled radio-frequency plasmas

    Energy Technology Data Exchange (ETDEWEB)

    Munafò, A., E-mail: munafo@illinois.edu; Alfuhaid, S. A., E-mail: alfuhai2@illinois.edu; Panesi, M., E-mail: mpanesi@illinois.edu [Department of Aerospace Engineering, University of Illinois at Urbana-Champaign, Talbot Laboratory, 104 S. Wright St., Urbana, Illinois 61801 (United States); Cambier, J.-L., E-mail: jean-luc.cambier@us.af.mil [Edwards Air Force Base Research Laboratory, 10 E. Saturn Blvd., Edwards AFB, California 93524 (United States)

    2015-10-07

    The objective of the present work is the development of a tightly coupled magneto-hydrodynamic model for inductively coupled radio-frequency plasmas. Non Local Thermodynamic Equilibrium (NLTE) effects are described based on a hybrid State-to-State approach. A multi-temperature formulation is used to account for thermal non-equilibrium between translation of heavy-particles and vibration of molecules. Excited electronic states of atoms are instead treated as separate pseudo-species, allowing for non-Boltzmann distributions of their populations. Free-electrons are assumed Maxwellian at their own temperature. The governing equations for the electro-magnetic field and the gas properties (e.g., chemical composition and temperatures) are written as a coupled system of time-dependent conservation laws. Steady-state solutions are obtained by means of an implicit Finite Volume method. The results obtained in both LTE and NLTE conditions over a broad spectrum of operating conditions demonstrate the robustness of the proposed coupled numerical method. The analysis of chemical composition and temperature distributions along the torch radius shows that: (i) the use of the LTE assumption may lead to an inaccurate prediction of the thermo-chemical state of the gas, and (ii) non-equilibrium phenomena play a significant role close the walls, due to the combined effects of Ohmic heating and macroscopic gradients.

  18. Speciation Analysis of Mercury in Milk Powder using Ion Chromatography-Inductively Coupled Plasma Mass Spectrometry Technique%离子色谱-电感耦合等离子体质谱法测定乳粉的汞形态

    Institute of Scientific and Technical Information of China (English)

    林立; 王琳琳; 孙海波; 孙继红

    2014-01-01

    Sample pre-treatment difficulties arise during the analysis for mercury speciation in milk powder due to the complexity of the sample matrix. The organic mercury combines easily with sulfydryl of proteins in the matrix sample,to form a stable complex. Therefore it is very important to ensure that all forms are extracted completely and do not transform during the pre-treatment process. The method with a lower detection limit was necessary because the concentration of mercury was too low. For this purpose,the method for determination of mercury speciation( inorganic mercury,methylmercury,ethylmercury ) in milk was established by ion chromatography inductively coupled plasma mass spectrometry with optimized pre-treatment conditions. Protein,fat,and starch in milk powder were dissociated using a variety of composite enzymes( protease,lipase and amylase). The sample was ultrasonically extracted using mixed solution of L-cysteine,hydrochloric acid with methanol and was further purified by RP solid phase column. Mercury speciation was separated by Agilent Eclipse XDB-C18 column(5μm, 4. 6 mm × 150 mm). The mobile phase contained 10 mmol/L ammonium acetate,0. 12% L-cysteine,and 5%(m:m)methanol solution. Three kinds of mercury speciation were baseline separated within 5 min. The spiked recoveries of inorganic mercury,methylmercury and ethylmercury were obtained in the range of 79. 9% -111. 2%. The instrument detection limits were 0. 5 μg/kg,0. 6 μg/kg and 0. 9 μg/kg,respectively. The results obtained from actual sample testing show that the extraction rate of total mercury can reach more than 70% in low concentration mercury milk powder,which meets the test requirements. The extraction rate can reach more than 80% because the composite enzyme was used in this method to dissociate mercury speciation from the complex matrix during sample pre-treatment processing. Methanol was applied as a sensitizer to improve detection sensitivity. A simple,rapid and reliable method was

  19. Mass spectrometric measurements in inductively coupled CF4/Ar plasmas

    International Nuclear Information System (INIS)

    Positive ion fluxes, mean ion energies and ion energy distribution functions in low pressure CF4/Ar plasmas have been measured. The experiments were conducted in a Gaseous Electronics Conference cell using an inductively coupled plasma device powered by a 13.56 MHz radiofrequency (rf) power source. The measurements were made at 200 and 300 W of input rf power and at 10, 20, 30 and 50 mTorr gas pressures for three gas mixtures: (i) 20% CF4 : 80% Ar, (ii) 50% CF4 : 50% Ar and (iii) 80% CF4 : 20% Ar. A Langmuir probe was also used to measure plasma parameters such as ne, ni+ and electron energy distribution functions (EEDF) which were subsequently used to reconcile the mass spectrometer data. CF3+ is the most dominant fluorocarbon ion product of the plasma, followed by CF2+ and CF+. Ar+ is also detected in significant amounts with its relative flux increasing with the increase in Ar content in the gas mixture. Significant amounts of etch products, SiFx+/COF+x (x = 0-3), of the quartz window were also detected. The fluorocarbon ions are produced by direct electron impact and by ion-molecule reactions between Ar+ and CF4 as well as between CF3+ and CF4. However, the concentrations of CF2+ and CF+ are much larger than that which can be possibly produced from these two processes. The available cross-section data suggest that the direct electron impact ionization of the fragment neutrals and negative ion production by electron attachment may be responsible for the increase in the concentrations of the minor ions. F- densities, estimated by using the measured EEDF and positive ion flux data and the available cross-section data, agree well with the published experimental data

  20. Advanced Burnup Method using Inductively Coupled Plasma Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hilton, Bruce A. [Idaho Natonal Laboratory, P.O. Box 1625, Idaho Falls, ID 83415-6188 (United States); Glagolenko, Irina; Giglio, Jeffrey J.; Cummings, Daniel G

    2009-06-15

    Nuclear fuel burnup is a key parameter used to assess irradiated fuel performance, to characterize the dependence of property changes due to irradiation, and to perform nuclear materials accountability. For advanced transmutation fuels and high burnup LWR fuels that have multiple fission sources, the existing Nd-148 ASTM burnup determination practice requires input of calculated fission fractions (identifying the specific fission source isotope and neutron energy that yielded fission, e.g., U-235 from thermal neutron, U-238 from fast neutron) from computational neutronics analysis in addition to the measured concentration of a single fission product isotope. We report a novel methodology of nuclear fuel burnup determination, which is completely independent of model predictions and reactor types. The proposed method leverages the capability of Inductively Coupled Plasma Mass Spectrometry (ICP-MS) to quantify multiple fission products and actinides and uses these data to develop a system of burnup equations whose solution is the fission fractions. The fission fractions are substituted back in the equations to determine burnup. This technique requires high fidelity fission yield data, which is not uniformly available for all fission products. We discuss different means that can potentially assist in indirect determination, verification and improvement (refinement) of the ambiguously known fission yields. A variety of irradiated fuel samples are characterized by ICP-MS and the results used to test the advanced burnup method. The samples include metallic alloy fuel irradiated in fast spectrum reactor (EBRII) and metallic alloy in a tailored spectrum and dispersion fuel in the thermal spectrum of the Advanced Test Reactor (ATR). The derived fission fractions and measured burnups are compared with calculated values predicted by neutronics models. (authors)

  1. Advanced Burnup Method using Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    Nuclear fuel burnup is a key parameter used to assess irradiated fuel performance, to characterize the dependence of property changes due to irradiation, and to perform nuclear materials accountability. For advanced transmutation fuels and high burnup LWR fuels that have multiple fission sources, the existing Nd-148 ASTM burnup determination practice requires input of calculated fission fractions (identifying the specific fission source isotope and neutron energy that yielded fission, e.g., U-235 from thermal neutron, U-238 from fast neutron) from computational neutronics analysis in addition to the measured concentration of a single fission product isotope. We report a novel methodology of nuclear fuel burnup determination, which is completely independent of model predictions and reactor types. The proposed method leverages the capability of Inductively Coupled Plasma Mass Spectrometry (ICP-MS) to quantify multiple fission products and actinides and uses these data to develop a system of burnup equations whose solution is the fission fractions. The fission fractions are substituted back in the equations to determine burnup. This technique requires high fidelity fission yield data, which is not uniformly available for all fission products. We discuss different means that can potentially assist in indirect determination, verification and improvement (refinement) of the ambiguously known fission yields. A variety of irradiated fuel samples are characterized by ICP-MS and the results used to test the advanced burnup method. The samples include metallic alloy fuel irradiated in fast spectrum reactor (EBRII) and metallic alloy in a tailored spectrum and dispersion fuel in the thermal spectrum of the Advanced Test Reactor (ATR). The derived fission fractions and measured burnups are compared with calculated values predicted by neutronics models. (authors)

  2. Determination of Oxidized Phosphatidylcholines by Hydrophilic Interaction Liquid Chromatography Coupled to Fourier Transform Mass Spectrometry

    OpenAIRE

    Pia Sala; Sandra Pötz; Martina Brunner; Martin Trötzmüller; Alexander Fauland; Alexander Triebl; Jürgen Hartler; Ernst Lankmayr; Köfeler, Harald C

    2015-01-01

    A novel liquid chromatography-mass spectrometry (LC-MS) approach for analysis of oxidized phosphatidylcholines by an Orbitrap Fourier Transform mass spectrometer in positive electrospray ionization (ESI) coupled to hydrophilic interaction liquid chromatography (HILIC) was developed. This method depends on three selectivity criteria for separation and identification: retention time, exact mass at a resolution of 100,000 and collision induced dissociation (CID) fragment spectra in a linear ion ...

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

    International Nuclear Information System (INIS)

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

  4. Development of a multi-species method by GC-coupling with inductively coupled plasma isotope dilution mass spectrometry for the simultaneous determination of alkylated lead, mercury and tin compounds

    OpenAIRE

    Poperechna, Nataliya

    2005-01-01

    An accurate and sensitive species-specific GC-ICP-IDMS (gas chromatography inductively coupled plasma isotope dilution mass spectrometry) method for the determination of trimethyllead and a multi-species-specific GC-ICP-IDMS method for the simultaneous determination of trimethyllead, methylmercury, and butyltins in biological and environmental samples were developed. They allow the determination of corresponding elemental species down to the low ng g-1 range. The developed synthesis scheme fo...

  5. Inductively coupled plasma - mass spectrometry (ICP-MS) and inductively coupled plasma – optical emission spectrometry (IP-OES) analysis of elements in Macedonian wines

    OpenAIRE

    Ivanova, Violeta; Wiltsche, Helmar; Stafilov, Trajče; Motter, Herber; Stefova, Marina; Lankmayr, Ernst

    2013-01-01

    In this study the major, minor and trace elements in 25 Macedonian white, rose and red wines from different wine regions were determined. Analysis was performed with inductively coupled plasma - mass spectrometry (ICP-MS) and inductively coupled plasma – optical emission spectrometry (ICP-OES) for accurate determination of the concentration of 42 elements (Ag, Al, Au, B, Ba, Be, Bi, Ca, Cd, Ce, Co, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Ho, La, Lu, Mg, Mn, Mo, Na, Nd, Ni, P, Pb, Pr, S, Sm, Tb, Ti, T...

  6. Determination of cobalamins using capillary electrophoresis inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Baker, S. A.; Miller-Ihli, N. J.

    2000-12-01

    The determination of cobalamins using capillary electrophoresis inductively coupled plasma mass spectrometry (CE-ICP-MS) was investigated. Both capillary zone electrophoresis (CZE) and micellar electrokinetic chromatography (MEKC) modes of operation were studied. The optimal separation of four cobalamin species (cyanocobalamin, hydroxocobalamin, methylcobalamin, and 5'-deoxyadenosylcobalamin) and a potentially harmful corrinoid analogue (cobinamide dicyanide) was obtained using CZE at a pH of 2.5. Both 20 mM phosphate and 20 mM formate buffers were used with success, although the formate buffer provided improved resolution. The CZE-ICP-MS method was used to quantify cyanocobalamin in a vitamin supplement and the analytical results were in good agreement (±5%) with values obtained by ICP-MS for total Co levels. The solution detection limits for cobalamins using CZE-ICP-MS were approximately 50 ng/ml. MEKC was found to be useful for the screening of vitamin preparations because it provided a rapid means of distinguishing cyanocobalamin (the form most commonly used in vitamin preparations) from free cobalt. The separation of free cobalt and cyanocobalamin using MEKC was achieved in less than 10 min.

  7. Aerosol detection efficiency in inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Hubbard, Joshua A.; Zigmond, Joseph A.

    2016-05-01

    An electrostatic size classification technique was used to segregate particles of known composition prior to being injected into an inductively coupled plasma mass spectrometer (ICP-MS). Size-segregated particles were counted with a condensation nuclei counter as well as sampled with an ICP-MS. By injecting particles of known size, composition, and aerosol concentration into the ICP-MS, efficiencies of the order of magnitude aerosol detection were calculated, and the particle size dependencies for volatile and refractory species were quantified. Similar to laser ablation ICP-MS, aerosol detection efficiency was defined as the rate at which atoms were detected in the ICP-MS normalized by the rate at which atoms were injected in the form of particles. This method adds valuable insight into the development of technologies like laser ablation ICP-MS where aerosol particles (of relatively unknown size and gas concentration) are generated during ablation and then transported into the plasma of an ICP-MS. In this study, we characterized aerosol detection efficiencies of volatile species gold and silver along with refractory species aluminum oxide, cerium oxide, and yttrium oxide. Aerosols were generated with electrical mobility diameters ranging from 100 to 1000 nm. In general, it was observed that refractory species had lower aerosol detection efficiencies than volatile species, and there were strong dependencies on particle size and plasma torch residence time. Volatile species showed a distinct transition point at which aerosol detection efficiency began decreasing with increasing particle size. This critical diameter indicated the largest particle size for which complete particle detection should be expected and agreed with theories published in other works. Aerosol detection efficiencies also displayed power law dependencies on particle size. Aerosol detection efficiencies ranged from 10- 5 to 10- 11. Free molecular heat and mass transfer theory was applied, but

  8. Quantum Fluctuation of a Mesoscopic Inductance Coupling Circuit at Finite Temperature

    Institute of Scientific and Technical Information of China (English)

    SONG Tong-Qiang; ZHU Yue-Jin

    2003-01-01

    We study the quantization of mesoscopic inductance coupling circuit and discuss its time evolution. Bymeans of the thermal field dynamics theory we study the quantum fluctuation of the system at finite temperature.

  9. Application of inductively coupled plasma mass spectrometry (ICP-MS) to radioecology

    International Nuclear Information System (INIS)

    The advantages of Inductively Coupled Plasma Mass Spectrometry (ICP-MS) over conventional radioanalytical measurements are presented and the applications of the ICP-MS technique to environmental samples are given

  10. Determination of traces of thorium in uranium by inductively coupled plasma mass spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    An analytical methodology for the determination of traces of thorium in uranium oxide by Inductively Coupled Plasma Mass Spectrometry has been developed. Recovery studies were carried out by standard addition and also by tracer technique to validate the methodology. (author)

  11. Design of an Improved Type Rotary Inductive Coupling Structure for Rotatable Contactless Power Transfer System

    Directory of Open Access Journals (Sweden)

    Lee Jia-You

    2015-01-01

    Full Text Available This paper is aimed at analyzing the rotary inductive coupling structure of contactless rotary transformer. The main feature of the proposed rotatable contactless power transfer system is which winding is coaxial-interlayered for improving the magnetic coupling capability. There is no ferrite core used in the secondary-side of the rotary inductive coupling structure, this helps to ease the exerted force that is stress by the secondary-side on spindle. In order to verify the feasibility of the proposed contactless power transfer system for rotary applications, an inductive powered rotary machinery and the control system have been integrated. The experimental results show that the maximum power transfer efficiency of the proposed rotary inductive coupling structure is about 94.8%. The maximum output power received in the load end is 1030 W with transmission efficiency of 88%.

  12. Arsenic speciation by liquid chromatography coupled with ionspray tandem mass spectrometry

    DEFF Research Database (Denmark)

    Corr, J. J.; Larsen, Erik Huusfeldt

    1996-01-01

    Ionspray mass spectrometry, a well established organic analysis technique, has been coupled to high-performance liquid chromatography for speciation of organic arsenic compounds, The ionspray source and differentially pumped interface of the mass spectrometer were operated in dual modes for...

  13. Velocity field measurements in an inductively coupled plasma

    International Nuclear Information System (INIS)

    With the rapid development of laser doppler anemometry, a new tool became available that proved to be quite useful for gas and particle velocity measurements under plasma conditions. The objective of the present study was to adapt this technique to measurements in an induction plasma and to obtain gas and particle velocity data in the discharge zone under different operating conditions

  14. Modelling of Continual Induction Hardening in Quasi-Coupled Formulation

    Czech Academy of Sciences Publication Activity Database

    Barglik, J.; Doležel, Ivo; Karban, P.; Ulrych, B.

    2005-01-01

    Roč. 24, č. 1 (2005), s. 251-260. ISSN 0332-1649 Grant ostatní: PSRC(PL) 4T08C 04823 Institutional research plan: CEZ:AV0Z20570509 Keywords : mathematical modelling * electromagnetism * induction Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering Impact factor: 0.188, year: 2005

  15. Modelling of Continual Induction Hardening in Quasi-Coupled Formulation

    Czech Academy of Sciences Publication Activity Database

    Barglik, J.; Doležel, Ivo; Karban, P.; Ulrych, B.

    Padua: University of Padua, 2004 - (Lupi, S.; Dughiero, F.), s. 599-606 ISBN 88-86281-92-7. [International Symposium on Heating by Electromagnetic Sources (HES-04). Padua (IT), 22.06.2004-25.06.2004] Institutional research plan: CEZ:AV0Z2057903 Keywords : electromagnetic field * induction heating * numerical analysis Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering

  16. Velocity field measurements in an inductively coupled plasma

    Energy Technology Data Exchange (ETDEWEB)

    Boulos, M.I. Lesinski, J.; Barnes, R.M.

    1982-01-01

    With the rapid development of laser doppler anemometry, a new tool became available that proved to be quite useful for gas and particle velocity measurements under plasma conditions. The objective of the present study was to adapt this technique to measurements in an induction plasma and to obtain gas and particle velocity data in the discharge zone under different operating conditions.

  17. Low wireless power transfer using inductive coupling for mobile phone charger

    International Nuclear Information System (INIS)

    A wireless power transfer (WPT) using inductive coupling for mobile phone charger is studied. The project is offer to study and fabricate WPT using inductive coupling for mobile phone charger that will give more information about distance is effect for WPT performance and WPT is not much influenced by the presence of hands, books and types of plastics. The components used to build wireless power transfer can be divided into 3 parts components, the transceiver for power transmission, the inductive coils in this case as the antenna, receiver and the rectifier which act convert AC to DC. Experiments have been conducted and the wireless power transfer using inductive coupling is suitable to be implemented for mobile phone charger.

  18. Analysis of Bifurcation Phenomena of Voltage-fed inductively Coupled Power Transfer System Varying with Coupling Coefficient

    Directory of Open Access Journals (Sweden)

    Zhihui Wang

    2013-01-01

    Full Text Available This study investigates the frequency bifurcation phenomena of a typical voltage-fed resonant converter based on mutual induction model. It is found that the Zero Current Switching (ZCS operating frequency has the bifurcation region as the coupling coefficient varies due to the distance. The expression for the bifurcation boundary is derived and analyzed. Such results are very useful for guiding the design of practical Inductively Coupled Power Transfer (ICPT systems especially in applications which have the requirement of the position flexibility. Analytical results are verified both via MATLAB simulations and experimental prototype.

  19. Speciation of mercury by chromatography coupled with atomic spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Armstrong, H.E.L

    2000-03-01

    A commercial GC-AFS instrument has been developed and optimised for the speciation of organomercury. This instrument couples a GC oven to a modified atomic fluorescence detector via a ceramic pyrolyser. Organomercury compounds in dichloromethane solvent were directly injected through a Programmable Temperature Vaporiser Injector onto a DB1 Megabore column. Once separated, the compounds eluted from the column and were atomised in the pyrolyser then detected by AFS. The direct injection technique, ceramic pyrolysis design and argon purged detector have improved previous instrument designs by enhancing and maintaining sensitivity. The instrumental limit of detection was determined to be 0.25 pg Hg absolute. Methods were developed for the extraction of methylmercury from a variety of marine samples. The techniques were validated using mussel homogenate and dogfish liver (IAEA 142, SRM 8044 and DOLT-2) certified reference materials. An interlaboratory comparison exercise was participated in and a method was developed for the determination of methylmercury in Fucus sea plant (IAEA 140). A concentration of 0.63 {+-} 0.006 ng g{sup -1} was reported. The material is now certified at 0.626 {+-} 0.139 ng g{sup -1}. Of all the participating laboratories, this was the closest result to the certified value. The instrument and methods were also applied to soil and sediment samples. Once again validation was performed with a CRM sediment, IAEA 356. Although this material has been reported to give positive artifact formation when using a steam distillation sample preparation procedure, good agreement and no artifacts were observed upon analysis. A further contaminated land, an uncontaminated soil and sediment sample were also studied. For all the samples studied by GC-AFS total mercury measurements were also made following an appropriate digestion procedure and CV-AFS. A gas chromatograph was also coupled with ICP-MS and HPLC was coupled to CV-AFS as comparative techniques. Both

  20. Speciation of mercury by chromatography coupled with atomic spectrometry

    International Nuclear Information System (INIS)

    A commercial GC-AFS instrument has been developed and optimised for the speciation of organomercury. This instrument couples a GC oven to a modified atomic fluorescence detector via a ceramic pyrolyser. Organomercury compounds in dichloromethane solvent were directly injected through a Programmable Temperature Vaporiser Injector onto a DB1 Megabore column. Once separated, the compounds eluted from the column and were atomised in the pyrolyser then detected by AFS. The direct injection technique, ceramic pyrolysis design and argon purged detector have improved previous instrument designs by enhancing and maintaining sensitivity. The instrumental limit of detection was determined to be 0.25 pg Hg absolute. Methods were developed for the extraction of methylmercury from a variety of marine samples. The techniques were validated using mussel homogenate and dogfish liver (IAEA 142, SRM 8044 and DOLT-2) certified reference materials. An interlaboratory comparison exercise was participated in and a method was developed for the determination of methylmercury in Fucus sea plant (IAEA 140). A concentration of 0.63 ± 0.006 ng g-1 was reported. The material is now certified at 0.626 ± 0.139 ng g-1. Of all the participating laboratories, this was the closest result to the certified value. The instrument and methods were also applied to soil and sediment samples. Once again validation was performed with a CRM sediment, IAEA 356. Although this material has been reported to give positive artifact formation when using a steam distillation sample preparation procedure, good agreement and no artifacts were observed upon analysis. A further contaminated land, an uncontaminated soil and sediment sample were also studied. For all the samples studied by GC-AFS total mercury measurements were also made following an appropriate digestion procedure and CV-AFS. A gas chromatograph was also coupled with ICP-MS and HPLC was coupled to CV-AFS as comparative techniques. Both approaches were

  1. Elemental speciation by capillary electrophoresis with inductively coupled plasma spectrometry: A new approach by flow focusing® nebulization

    OpenAIRE

    Kovachev, Nikolay; Aguirre Pastor, Miguel Ángel; Hidalgo Núñez, Montserrat; Simitchiev, Kiril; Stefanova, Violeta M.; Kmetov, Veselin Y.; Canals Hernández, Antonio

    2014-01-01

    A novel system for Capillary Electrophoresis (CE) and Inductively Coupled Plasma (ICP) sample introduction that incorporates a dedicated Flow-Focusing® based nebulizer as aerosol generation unit is presented, aiming to provide high signal sensitivity and low detection limits for element speciation at short analysis times. To prove its viability, the system prototype constructed has been coupled to an inductively coupled plasma - optical emission spectrometer (ICP-OES) and an inductively coupl...

  2. Interfacing capillary electrophoresis with inductively coupled plasma mass spectrometry by direct injection nebulization for selenium speciation

    DEFF Research Database (Denmark)

    Bendahl, Lars; Gammelgaard, Bente; Jons, O.;

    2001-01-01

    A demountable direct injection high efficiency nebulizer operating at low sample uptake rates was developed and used for coupling of capillary electrophoresis (CE) with inductively coupled plasma mass spectrometry (ICP-MS). When the nebulizer was used for continuous sample introduction, detection...

  3. Effects of leakage inductances on magnetically-coupled impedance-source networks

    DEFF Research Database (Denmark)

    Siwakoti, Yam P.; Loh, Poh Chiang; Blaabjerg, Frede;

    2014-01-01

    Coupled inductors have lately been used with impedance-source networks for keeping their shoot-through times short, while providing higher voltage boosts. The parameter that is critical to the operation of such impedance network based converter with coupled inductors is the leakage inductances. H...

  4. Development of NbTiN-Al direct antenna coupled kinetic inductance detectors

    OpenAIRE

    Lankwarden, Y.J.Y.; Endo, A; Baselmans, J. J. A.; Bruijn, M.P.

    2012-01-01

    We have developed a coplanar waveguide (CPW) Kinetic Inductance Detector consisting of Al and NbTiN, coupled at its shorted end to a planar antenna. To suppress the odd mode due to direct coupling to sky radiation by the KID we have also developed freestanding metal air bridges

  5. Ultra-wide bandwidth improvement of piezoelectric energy harvesters through electrical inductance coupling

    Science.gov (United States)

    Abdelmoula, H.; Abdelkefi, A.

    2015-11-01

    The design and analysis of innovative ultra-wide bandwidth piezoelectric energy harvesters are deeply investigated. An electrical inductance is considered in the harvester's circuit to be connected in series or parallel to a load resistance. A lumped-parameter model is used to model the electromechanical response of the harvester when subjected to harmonic excitations. A linear comprehensive analysis is performed to investigate the effects of an electrical inductance on the coupled frequencies and damping of the harvester. It is shown that including an electrical inductance connected in series or in parallel to an electrical load resistance can result in the appearance of a second coupled frequency of electrical type. The results show that the inclusion of an inductance may give the opportunity to tune one of the coupled frequencies of mechanical and electrical types to the available excitation frequency in the environment. Using the gradient method, an optimization analysis is then performed to determine the optimum values of the electrical inductance and load resistance that maximize the harvested power. It is demonstrated that, for each excitation frequency, there is a combination of optimum values of the electrical inductance and resistance in such a way an optimum constant value of the harvested power is found. Numerical analysis is then performed to show the importance of considering an additional inductance in the harvester's circuitry in order to design broadband energy harvesters. The results show that the presence of the second coupled frequency of electrical type due to the inductance gives the possibility to design optimal broadband inductive-resistive piezoelectric energy harvesters with minimum displacement due to shunt damping effect.

  6. Characterization of the fermentation process by gas chromatography Lasiodiplodia theobromae and gas chromatography coupled with mass spectrometry

    International Nuclear Information System (INIS)

    Lasiodiplodia theobromae is a fungus, which has been reported by some authors as a high yield producer of the phytohormone jasmonic acid (JA). An indigenous strain of this fungus has been used for producing a fermentation broth with a high JA concentration by the Cuban Research Institute for Sugar Cane Derivatives (ICIDCA), registered as BIOJAS. The broth has been applied to some agricultural crops and demonstrated its economic feasibility as plant growth regulator and biological control of various phytopathogenic microorganisms and pests. Both fermentation broth and biomass from this fungus contain some other metabolites having bioactive properties, for instance, fatty acids. This paper shows the composition and quantification of fatty acids in the biomass using Gas Chromatography (GC) and the identification of substances profile in fermentation broth by Gas Chromatography coupled to Mass Spectrometry (GC-MS). The most fatty acids in the biomass are palmitic, stearic, oleic, linoleic and linolenic acids, being oleic acid the major component. On the other hand, 2,32 % of fatty acid esters; 2,47 % of alkenes; 14,40 % of alcohols; 30,15 % of aldehydes and 21,73 % of paraffins were detected in the composition of fermentation broth

  7. Mathematical Modeling of the Three Phase Induction Motor Couple to DC Motor in Hybrid Electric Vehicle

    OpenAIRE

    Zulkarnain Lubis; A. N. Abdalla; Mortaza; Ruzlaini Ghon

    2009-01-01

    Problem statement: With emphasis on a cleaner environment and efficient operation, vehicles today rely more and more heavily on electrical power generation for success. Approach: Mathematical modeling the components of the HEV as the three phase induction motor couple to DC motor in hybrid electric vehicle was introduced. The controller of Induction Motor (IM) was designed based on input-output feedback linearization technique. It allowed greater electrical generation capacity and the fuel ec...

  8. UHF RFID Antenna: Printed Dipole Antenna with a CPS Matching Circuit and Inductively Coupled Feed

    OpenAIRE

    Nenad Popović

    2011-01-01

    This paper presents simulated (WIPL‐D pro) and measured results of a UHF RFID antenna realized with a dipole matched to a CPS (Coplanar Stripline) and inductively coupled with a small rectangular loop. Such a design enables achieving and controlling high values of the inductive reactance that is necessary for obtaining good match of the antenna to an Application Specific Integrated Circuit (ASIC) chip. The antenna is characterized by a simple and robust design, which results in low‐cost re...

  9. Plasmoids and the E-to-H transition in an inductively coupled plasma

    OpenAIRE

    McCarter, Angus J.

    2005-01-01

    An Inductively Coupled Plasma (ICP) exhibits two distinct modes of operation. A low input power capacitive E-mode, and a high input power inductive H-mode. The gas initially breaks down m the E-mode, switching to H-mode as input power is increased above a certain threshold. This transition between the E and H modes is observed by a dramatic increase in light output from the plasma, and a ‘glitch3 in the antenna current as the load characteristics of the plasma change from capacitive to induct...

  10. Determination of Oxidized Phosphatidylcholines by Hydrophilic Interaction Liquid Chromatography Coupled to Fourier Transform Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Pia Sala

    2015-04-01

    Full Text Available A novel liquid chromatography-mass spectrometry (LC-MS approach for analysis of oxidized phosphatidylcholines by an Orbitrap Fourier Transform mass spectrometer in positive electrospray ionization (ESI coupled to hydrophilic interaction liquid chromatography (HILIC was developed. This method depends on three selectivity criteria for separation and identification: retention time, exact mass at a resolution of 100,000 and collision induced dissociation (CID fragment spectra in a linear ion trap. The process of chromatography development showed the best separation properties with a silica-based Kinetex column. This type of chromatography was able to separate all major lipid classes expected in mammalian samples, yielding increased sensitivity of oxidized phosphatidylcholines over reversed phase chromatography. Identification of molecular species was achieved by exact mass on intact molecular ions and CID tandem mass spectra containing characteristic fragments. Due to a lack of commercially available standards, method development was performed with copper induced oxidation products of palmitoyl-arachidonoyl-phosphatidylcholine, which resulted in a plethora of lipid species oxidized at the arachidonoyl moiety. Validation of the method was done with copper oxidized human low-density lipoprotein (LDL prepared by ultracentrifugation. In these LDL samples we could identify 46 oxidized molecular phosphatidylcholine species out of 99 possible candidates.

  11. New approach to the calculation of relative sensitivity factors in inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    The relative sensitivity factors (RSFs) of 68 elements including alkali, alkaline earth, rare earth, and transition elements, Cd, B, In, Te, I in the analysis by inductively coupled plasma mass spectrometry were determined. The ionization process in an inductively coupled plasma was found to be only approximately described by the Saha-Eggert equation. A relationship between the RSFs and the absolute electronegativities of atoms of the elements was found. This factor has the strongest effect on the accuracy of calculations of RSFs for chemically active elements. The average relative systematic error of calculations of RSFs with consideration for absolute electronegativity was reduced to 0.30

  12. Separation, detection and characterization of nanomaterials in municipal wastewaters using hydrodynamic chromatography coupled to ICPMS and single particle ICPMS.

    Science.gov (United States)

    Proulx, Kim; Hadioui, Madjid; Wilkinson, Kevin J

    2016-07-01

    Engineered nanoparticles (ENP) are increasingly being incorporated into consumer products and reaching the environment at a growing rate. Unfortunately, few analytical techniques are available that allow the detection of ENP in complex environmental matrices. The major limitations with existing techniques are their relatively high detection limits and their inability to distinguish ENP from other chemical forms (e.g. ions, dissolved) or from natural colloids. Of the matrices that are considered to be a priority for method development, ENP are predicted to be found at relatively high concentrations in wastewaters and wastewater biosolids. In this paper, we demonstrate the capability of hydrodynamic chromatography (HDC) coupled to inductively coupled plasma mass spectrometry (ICPMS), in its classical and single particle modes (SP ICPMS), to identify ENP in wastewater influents and effluents. The paper first focuses on the detection of standard silver nanoparticles (Ag NP) and their mixtures, showing that significant dissolution of the Ag NP was likely to occur. For the Ag NP, detection limits of 0.03 μg L(-1) were found for the HDC ICPMS whereas 0.1 μg L(-1) was determined for the HDC SP ICPMS (based on results for the 80 nm Ag NP). In the second part of the paper, HDC ICPMS and HDC SP ICPMS were performed on some unspiked natural samples (wastewaters, river water). While nanosilver was below detection limits, it was possible to identify some (likely natural) Cu nanoparticles using the developed separation technology. PMID:26970748

  13. Characterization of an inductively coupled plasma source with convergent nozzle

    Science.gov (United States)

    Dropmann, Michael; Clements, Kathryn; Edgren, Josh; Laufer, Rene; Herdrich, Georg; Matthews, Lorin; Hyde, Truell

    2015-11-01

    The inductively heated plasma generator (IPG6-B) located in the CASPER labs at Baylor University has recently been characterized for both air, nitrogen and helium. A primary area of research within the intended scope of the instrument is the analysis of material degradation under high heat fluxes such as those imposed by a plasma during atmospheric entry of a spacecraft and at the divertor within various fusion experiment. In order to achieve higher flow velocities and respectively higher heat fluxes, a new exit flange has been designed to allow the installation of nozzles with varying geometries at the exit of the plasma generator. This paper will discuss characterization of the plasma generator for a convergent nozzle accelerating the plasma jet to supersonic velocity. The diagnostics employed include a cavity calorimeter to measure the total plasma power, a Pitot probe to measure stagnation pressure and a heat flux probe to measure the local heat flux. Radial profiles of stagnation pressure and heat flux allowing the determination of the local plasma enthalpy in the plasma jet will be presented. Support from the NSF and the DOE (award numbers PHY-1262031 and PHY-1414523) is gratefully acknowledged.

  14. Macroscopic quantum effects in capacitively- and inductively-coupled intrinsic Josephson junctions

    Science.gov (United States)

    Koyama, T.; Machida, M.

    2009-03-01

    A theory for macroscopic quantum tunneling (MQT) in intrinsic Josephson junction stacks is formulated. Both capacitive and inductive couplings between junctions are taken into account. We calculate the escape rate in the switching to the first resistive branch in the quantum regime. It is shown that the enhancement of the escape rate is caused mainly by the capacitive coupling between junctions in IJJ's with small in-plane area of ~ 1μm2.

  15. Mapping of lead, magnesium and copper accumulation in plant tissues by laser-induced breakdown spectroscopy and laser-ablation inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Kaiser, J. [Institute of Physical Engineering, Faculty of Mechanical Engineering, Brno University of Technology, Technicka 2896/2, 616 69 Brno (Czech Republic)], E-mail: kaiser@fme.vutbr.cz; Galiova, M.; Novotny, K.; Cervenka, R. [Department of Chemistry, Faculty of Science, Masaryk University, Kotlarska 2, 611 37 Brno (Czech Republic); Reale, L. [Faculty of Sciences, University of L' Aquila, Via Vetoio (Coppito 1), 67010 L' Aquila (Italy); Novotny, J.; Liska, M.; Samek, O. [Institute of Physical Engineering, Faculty of Mechanical Engineering, Brno University of Technology, Technicka 2896/2, 616 69 Brno (Czech Republic); Kanicky, V.; Hrdlicka, A. [Department of Chemistry, Faculty of Science, Masaryk University, Kotlarska 2, 611 37 Brno (Czech Republic); Stejskal, K.; Adam, V.; Kizek, R. [Department of Chemistry and Biochemistry, Faculty of Agronomy, Mendel University of Agriculture and Forestry, Zemedelska 1, 613 00 Brno (Czech Republic)

    2009-01-15

    Laser-Induced Breakdown Spectroscopy (LIBS) and Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) were utilized for mapping the accumulation of Pb, Mg and Cu with a resolution up to 200 {mu}m in a up to cm x cm area of sunflower (Helianthus annuus L.) leaves. The results obtained by LIBS and LA-ICP-MS are compared with the outcomes from Atomic Absorption Spectrometry (AAS) and Thin-Layer Chromatography (TLC). It is shown that laser-ablation based analytical methods can substitute or supplement these techniques mainly in the cases when a fast multi-elemental mapping of a large sample area is needed.

  16. Mapping of lead, magnesium and copper accumulation in plant tissues by laser-induced breakdown spectroscopy and laser-ablation inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Kaiser, J.; Galiová, M.; Novotný, K.; Červenka, R.; Reale, L.; Novotný, J.; Liška, M.; Samek, O.; Kanický, V.; Hrdlička, A.; Stejskal, K.; Adam, V.; Kizek, R.

    2009-01-01

    Laser-Induced Breakdown Spectroscopy (LIBS) and Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) were utilized for mapping the accumulation of Pb, Mg and Cu with a resolution up to 200 μm in a up to cm × cm area of sunflower ( Helianthus annuus L.) leaves. The results obtained by LIBS and LA-ICP-MS are compared with the outcomes from Atomic Absorption Spectrometry (AAS) and Thin-Layer Chromatography (TLC). It is shown that laser-ablation based analytical methods can substitute or supplement these techniques mainly in the cases when a fast multi-elemental mapping of a large sample area is needed.

  17. Mapping of lead, magnesium and copper accumulation in plant tissues by laser-induced breakdown spectroscopy and laser-ablation inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Laser-Induced Breakdown Spectroscopy (LIBS) and Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) were utilized for mapping the accumulation of Pb, Mg and Cu with a resolution up to 200 μm in a up to cm x cm area of sunflower (Helianthus annuus L.) leaves. The results obtained by LIBS and LA-ICP-MS are compared with the outcomes from Atomic Absorption Spectrometry (AAS) and Thin-Layer Chromatography (TLC). It is shown that laser-ablation based analytical methods can substitute or supplement these techniques mainly in the cases when a fast multi-elemental mapping of a large sample area is needed

  18. Implementation of Inductive Magnetosphere-Ionosphere Coupling and its Effects on Global MHD Magnetospheric Simulations

    Science.gov (United States)

    Xi, S.; Lotko, W.; Zhang, B.; Brambles, O.; Wiltberger, M. J.; Lyon, J.; Merkin, V. G.

    2010-12-01

    In global modeling, magnetosphere-ionosphere (MI) coupling physically connects a global magnetospheric (GM) model and a global ionospheric-thermospheric (GIT) model. The field-aligned current from the GM model and the conductance distributions from the GIT model are used in a Poisson equation derived from the ionospheric Ohm's law combined with current continuity to determine the electrostatic potential in the ionosphere. In current GM models, this electrostatic potential is mapped to the inner boundary of the GM simulation to determine electrostatic boundary conditions on the electric field and MHD velocity there. Inductive effects and the finite Alfven transit time between the low-altitude GM boundary and the high-altitude GIT boundary (MI gap region) are neglected in this formulation of MI coupling. Using fields and currents derived from Lyon-Fedder-Mobarry GM simulations, and conductance distributions derived from its standalone empirical conductance model in the MI coupling Poisson equation, we have computed the fast Fourier transform of the electrostatic field at the low-altitude LFM simulation boundary as described above, and the FFT of the inductive electric field at the boundary under the assumption that μ 0 Σ P vA ≤ 1, where Σ P is the ionospheric Pedersen conductance and vA is the smallest value of the Alfven speed in the MI gap region. In this regime, the complete electric field at the low-altitude simulation boundary includes the usual mapped electrostatic field with an inductive addition for which the finite Alfven transit time and the diversion of field-aligned into polarization currents in the gap region are negligible (Lotko, 2004). By comparing the boundary-averaged spectra of the electrostatic and so-determined inductive fields, we confirm that the purely electrostatic formulation of MI coupling is valid when the MHD state varies on times scales exceeding about 200 s. For faster MHD time variations, the inductive electric field is shown to

  19. 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...

  20. Determination of Arsenic in Sinus Wash and Tap Water by Inductively Coupled Plasma-Mass Spectrometry

    Science.gov (United States)

    Donnell, Anna M.; Nahan, Keaton; Holloway, Dawone; Vonderheide, Anne P.

    2016-01-01

    Arsenic is a toxic element to which humans are primarily exposed through food and water; it occurs as a result of human activities and naturally from the earth's crust. An experiment was developed for a senior level analytical laboratory utilizing an Inductively Coupled Plasma-Mass Spectrometer (ICP-MS) for the analysis of arsenic in household…

  1. Thorium determination in thorotrast patient organs using inductively coupled plasma mass spectrometry and imaging plate autoradiography

    International Nuclear Information System (INIS)

    In this study inductively coupled plasma mass spectrometry (ICP-MS) have been used for the determination of Th in liver and spleen collected from autopsy subjects in Thorotrast patients to obtain useful information for dosimetry. The applicability of an imaging plate autoradiography technique for the determination of thorium distributions in organs to obtain information related to microdosimetry has also been evaluated

  2. Simultaneous multielement analysis of rock samples by inductively coupled plasma mass spectrometry using discrete microsampling technique

    International Nuclear Information System (INIS)

    Simultaneous multielement analysis of geological standard rock samples (JG-1 and JB-2) has been successfully performed by inductively coupled plasma mass spectrometry using a discrete microsampling technique. In this technique only 100 μl sample solution was used for simultaneous determination of 5-10 elements in solution. (author)

  3. Improvement of Uniformity of Inductively Coupled Plasma with a Cone Spiral Antenna

    Institute of Scientific and Technical Information of China (English)

    LI Lin-Sen; XU Xu; LIU Feng; ZHOU Qian-Hong; NIE Zong-Fu; LIANG Yi-Zi; LIANG Rong-Qing

    2008-01-01

    Uniformity of inductively coupled plasma (ICP) is improved with a cone spiral antenna in our experiment. Performance of the ICP with a new type of antenna is experimentally investigated, The results indicate that the uniformity of plasma density in the radial direction is obviously improved as compared to the ICP with a planar spiral antenna. Performance of ICP is analysed with the experimental results.

  4. INDUCTIVELY COUPLED ARGON PLASMA AS AN ION SOURCE FOR MASS SPECTROMETRIC DETERMINATION OF TRACE ELEMENTS

    Science.gov (United States)

    Solution aerosols are injected into an inductively coupled argon plasma (ICP) to generate a relatively high number density of positive ions derived from elemental constituents. A small fraction of these ions is extracted through a sampling orifice into a differentially pumped vac...

  5. Polymerization by plasma of trichloroethylene by means of resistive and inductive coupling

    International Nuclear Information System (INIS)

    It was carried out the polymerization for plasma of the trichloroethylene by means of two types of coupling, resistive and inductive with the objective of studying the structure, morphology and the electric properties of the polymers obtained under these conditions. The structure and morphology of the polymers were studied by means of EDS and FT-IR spectroscopies. (Author)

  6. Inductively coupled plasma-atomic emission spectroscopy: The determination of trace impurities in uranium hexafluoride

    Science.gov (United States)

    Floyd, M. A.; Morrow, R. W.; Farrar, R. B.

    An analytical method has been developed for the determination of trace impurities in high-purity uranium hexafluoride using liquid-liquid extraction of the uranium from the trace impurities followed by analysis with inductively coupled plasma-atomic emission spectroscopy. Detection limits, accuracy, and precision data are presented.

  7. Stationary phase modulation in liquid chromatography through the serial coupling of columns: A review.

    Science.gov (United States)

    Alvarez-Segura, T; Torres-Lapasió, J R; Ortiz-Bolsico, C; García-Alvarez-Coque, M C

    2016-06-01

    Liquid chromatography with single columns often does not succeed in the analysis of complex samples, in terms of resolution and analysis time. A relatively simple solution to enhance chromatographic resolution is the modulation of the stationary phase through the serial coupling of columns. This can be implemented with any type of column using compatible elution conditions and conventional instruments. This review describes the key features of column coupling and published procedures, where two or more columns were coupled in series to solve separation problems. In all reports, the authors could not resolve their samples with single columns, whereas significant enhancement in chromatographic performance was obtained when the columns were combined. Particularly interesting is the reduction in the analysis time in the isocratic mode, which alleviates the "general elution problem" of liquid chromatography, and may represent a stimulus for the proposal of new procedures, especially in combination with mass spectrometric, electrochemical and refractometric detection. Developments proposed to make the serial coupling of columns useful in routine and research laboratories are outlined, including optimisation strategies that facilitate the selection of the appropriate column combination and elution conditions (solvent content, flow rate or temperature) in both isocratic and gradient modes. The availability of zero dead volume couplers, able to connect standard columns, and the commercialisation of short columns with multiple lengths, have expanded the possibilities of success. PMID:27155298

  8. Inductively coupled plasma and ion sources: History and state-of-the-art

    International Nuclear Information System (INIS)

    Over 100 years ago Hittorf first generated an electrodeless ''ring'' discharge by electromagnetic induction and began a 40 year controversy as to the true physical origin of such a discharge. Even Tesla advocated that these plasmas were merely the result of large electrostatic potential differences rather than electric fields induced by high frequency currents. Through clever experiments using crude spark gaps and leyden jars, the inductive nature of the discharge was confirmed in the late 1920's by MacKinnon, thus supporting the theories and experiments of Sir J.J. Thomson, perhaps the most staunch advocate of the induction mechanism. Today the authors routinely exploit the intense plasmas which are generated by induction. In this talk, the characteristics of inductively coupled plasma (ICP) and ion sources will be reviewed and future applications of intense plasma sources will be discussed. The inductively coupled plasma is Joule heated at moderate gas pressures, but the electromagnetic field penetration of these dense plasmas is limited by the plasma skin depth, typically a few millimeters to a few centimeters. The induction plasma is thus edge heated, a fact that constrains uniformity over large areas if helical induction coils are used. Flat, spiral coils may be used to improve uniformity by driving the plasma using a planar geometry. Issues of dimensional and frequency scaling will be discussed as they apply to large diameter sources. Ion beams extracted from ICPs are used for many applications including space propulsion, high power neutral beams, and materials processing. Broad ion beam (∼10 cm) current densities in excess of 100 mA-cm2 at 100 keV are obtained in pulsed mode operation. Recently, however, more consumer-oriented applications of less intense ICPs are emerging

  9. Assessment of pesticide residues in some fruits using gas chromatography coupled with micro electron capture detector

    International Nuclear Information System (INIS)

    A very sensitive analytical method for the determination of 26 pesticides in some fruits based on solid phase extraction (SPE) cleanup was developed using gas chromatography (GC) coupled with micro electron capture detector (mu ECD). The identity of the pesticides was confirmed by gas chromatography mass spectroscopy (GC-MS) using selected ion monitoring (SIM) mode. Ethyl acetate was used as a solvent for the extraction of pesticide residues with assistance of sonication. For cleanup an octadecyl, C18 SPE column was used. A linear response of mu ECD was observed for all pesticides with good correlation coefficients (>0.9992). Proposed method was successfully applied for the determination of pesticide residues in the orange, apple, and grape fruits. Average recoveries achieved for all of the pesticides at fortification levels of 0.05, 1.0 and 2.0 mu g g/sup -1/ in analyzed fruits were above 90% with relative standard deviations (RSD) less than 6%. (author)

  10. Use of a parallel path nebulizer for capillary-based microseparation techniques coupled with an inductively coupled plasma mass spectrometer for speciation measurements

    International Nuclear Information System (INIS)

    A low flow, parallel path Mira Mist CE nebulizer designed for capillary electrophoresis (CE) was evaluated as a function of make-up solution flow rate, composition, and concentration, as well as the nebulizer gas flow rate. This research was conducted in support of a project related to the separation and quantification of cobalamin (vitamin B-12) species using microseparation techniques combined with inductively coupled plasma mass spectrometry (ICP-MS) detection. As such, Co signals were monitored during the nebulizer characterization process. Transient effects in the ICP were studied to evaluate the suitability of using gradients for microseparations and the benefit of using methanol for the make-up solution was demonstrated. Co signal response changed significantly as a function of changing methanol concentrations of the make-up solution and maximum signal enhancement was seen at 20% methanol with a 15 μl/min flow rate. Evaluation of the effect of changing the nebulizer gas flow rates showed that argon flows from 0.8 to 1.2 l/min were equally effective. The Mira Mist CE parallel path nebulizer was then evaluated for interfacing capillary microseparation techniques including capillary electrophoresis (CE) and micro high performance liquid chromatography (μHPLC) to inductively coupled plasma mass spectrometry (ICP-MS). A mixture of four cobalamin species standards (cyanocobalamin, hydroxocobalamin, methylcobalamin, and 5' deoxyadenosylcobalamin) and the corrinoid analogue cobinamide dicyanide were successfully separated using both CE-ICP-MS and μHPLC-ICP-MS using the parallel path nebulizer with a make-up solution containing 20% methanol with a flow rate of 15 μl/min

  11. Use of a parallel path nebulizer for capillary-based microseparation techniques coupled with an inductively coupled plasma mass spectrometer for speciation measurements

    Science.gov (United States)

    Yanes, Enrique G.; Miller-Ihli, Nancy J.

    2004-06-01

    A low flow, parallel path Mira Mist CE nebulizer designed for capillary electrophoresis (CE) was evaluated as a function of make-up solution flow rate, composition, and concentration, as well as the nebulizer gas flow rate. This research was conducted in support of a project related to the separation and quantification of cobalamin (vitamin B-12) species using microseparation techniques combined with inductively coupled plasma mass spectrometry (ICP-MS) detection. As such, Co signals were monitored during the nebulizer characterization process. Transient effects in the ICP were studied to evaluate the suitability of using gradients for microseparations and the benefit of using methanol for the make-up solution was demonstrated. Co signal response changed significantly as a function of changing methanol concentrations of the make-up solution and maximum signal enhancement was seen at 20% methanol with a 15 μl/min flow rate. Evaluation of the effect of changing the nebulizer gas flow rates showed that argon flows from 0.8 to 1.2 l/min were equally effective. The Mira Mist CE parallel path nebulizer was then evaluated for interfacing capillary microseparation techniques including capillary electrophoresis (CE) and micro high performance liquid chromatography (μHPLC) to inductively coupled plasma mass spectrometry (ICP-MS). A mixture of four cobalamin species standards (cyanocobalamin, hydroxocobalamin, methylcobalamin, and 5' deoxyadenosylcobalamin) and the corrinoid analogue cobinamide dicyanide were successfully separated using both CE-ICP-MS and μHPLC-ICP-MS using the parallel path nebulizer with a make-up solution containing 20% methanol with a flow rate of 15 μl/min.

  12. Use of a parallel path nebulizer for capillary-based microseparation techniques coupled with an inductively coupled plasma mass spectrometer for speciation measurements

    Energy Technology Data Exchange (ETDEWEB)

    Yanes, Enrique G. E-mail: yanes@bhnrc.usda.gov; Miller-Ihli, Nancy J. E-mail: miller-ihli@bhnrc.usda.gov

    2004-06-18

    A low flow, parallel path Mira Mist CE nebulizer designed for capillary electrophoresis (CE) was evaluated as a function of make-up solution flow rate, composition, and concentration, as well as the nebulizer gas flow rate. This research was conducted in support of a project related to the separation and quantification of cobalamin (vitamin B-12) species using microseparation techniques combined with inductively coupled plasma mass spectrometry (ICP-MS) detection. As such, Co signals were monitored during the nebulizer characterization process. Transient effects in the ICP were studied to evaluate the suitability of using gradients for microseparations and the benefit of using methanol for the make-up solution was demonstrated. Co signal response changed significantly as a function of changing methanol concentrations of the make-up solution and maximum signal enhancement was seen at 20% methanol with a 15 {mu}l/min flow rate. Evaluation of the effect of changing the nebulizer gas flow rates showed that argon flows from 0.8 to 1.2 l/min were equally effective. The Mira Mist CE parallel path nebulizer was then evaluated for interfacing capillary microseparation techniques including capillary electrophoresis (CE) and micro high performance liquid chromatography ({mu}HPLC) to inductively coupled plasma mass spectrometry (ICP-MS). A mixture of four cobalamin species standards (cyanocobalamin, hydroxocobalamin, methylcobalamin, and 5' deoxyadenosylcobalamin) and the corrinoid analogue cobinamide dicyanide were successfully separated using both CE-ICP-MS and {mu}HPLC-ICP-MS using the parallel path nebulizer with a make-up solution containing 20% methanol with a flow rate of 15 {mu}l/min.

  13. Mathematical modeling of intrinsic Josephson junctions with capacitive and inductive couplings

    Science.gov (United States)

    Rahmonov, I. R.; Shukrinov, Yu M.; Zemlyanaya, E. V.; Sarhadov, I.; Andreeva, O.

    2012-11-01

    We investigate the current voltage characteristics (CVC) of intrinsic Josephson junctions (IJJ) with two types of couplings between junctions: capacitive and inductive. The IJJ model is described by a system of coupled sine-Gordon equations which is solved numerically by the 4th order Runge-Kutta method. The method of numerical simulation and numerical results are presented. The magnetic field distribution is calculated as the function of coordinate and time at different values of the bias current. The influence of model parameters on the CVC is studied. The behavior of the IJJ in dependence on coupling parameters is discussed.

  14. A fully analytic treatment of resonant inductive coupling in the far field

    International Nuclear Information System (INIS)

    For the application of resonant inductive coupling for wireless power transfer, fabrication of flat spiral coils using ribbon wire allows for analytic expressions of the capacitance and inductance of the coils and therefore the resonant frequency. The expressions can also be used in an approximate way for the analysis of coils constructed from cylindrical wire. Ribbon wire constructed from both standard metals as well as high temperature superconducting material is commercially available, so using these derived expressions as a basis, a fully analytic treatment is presented that allows for design trades to be made for hybrid designs incorporating either technology. The model is then extended to analyze the performance of the technology as applied to inductively coupled communications, which has been demonstrated as having an advantage in circumstances where radiated signals would suffer unacceptable levels of attenuation. - Highlights: ► An analytic framework finds power and efficiency for resonant inductive coupling. ► The framework supports superconducting, resistive and dielectric elements. ► Maximum power transfer occurs at an efficiency of 50% when in close proximity. ► A 100 turn superconducting design achieves 10% efficiency out to 280 coil radii. ► The system response to narrow band amplitude modulation is modeled and presented.

  15. Systematic evaluation of matrix effects in hydrophilic interaction chromatography versus reversed phase liquid chromatography coupled to mass spectrometry.

    Science.gov (United States)

    Periat, Aurélie; Kohler, Isabelle; Thomas, Aurélien; Nicoli, Raul; Boccard, Julien; Veuthey, Jean-Luc; Schappler, Julie; Guillarme, Davy

    2016-03-25

    Reversed phase liquid chromatography (RPLC) coupled to mass spectrometry (MS) is the gold standard technique in bioanalysis. However, hydrophilic interaction chromatography (HILIC) could represent a viable alternative to RPLC for the analysis of polar and/or ionizable compounds, as it often provides higher MS sensitivity and alternative selectivity. Nevertheless, this technique can be also prone to matrix effects (ME). ME are one of the major issues in quantitative LC-MS bioanalysis. To ensure acceptable method performance (i.e., trueness and precision), a careful evaluation and minimization of ME is required. In the present study, the incidence of ME in HILIC-MS/MS and RPLC-MS/MS was compared for plasma and urine samples using two representative sets of 38 pharmaceutical compounds and 40 doping agents, respectively. The optimal generic chromatographic conditions in terms of selectivity with respect to interfering compounds were established in both chromatographic modes by testing three different stationary phases in each mode with different mobile phase pH. A second step involved the assessment of ME in RPLC and HILIC under the best generic conditions, using the post-extraction addition method. Biological samples were prepared using two different sample pre-treatments, i.e., a non-selective sample clean-up procedure (protein precipitation and simple dilution for plasma and urine samples, respectively) and a selective sample preparation, i.e., solid phase extraction for both matrices. The non-selective pretreatments led to significantly less ME in RPLC vs. HILIC conditions regardless of the matrix. On the contrary, HILIC appeared as a valuable alternative to RPLC for plasma and urine samples treated by a selective sample preparation. Indeed, in the case of selective sample preparation, the compounds influenced by ME were different in HILIC and RPLC, and lower and similar ME occurrence was generally observed in RPLC vs. HILIC for urine and plasma samples

  16. Multi-element analysis using inductively coupled plasma mass spectrometry and inductively coupled plasma atomic emission spectroscopy for provenancing of animals at the continental scale.

    Science.gov (United States)

    Kreitals, Natasha M; Watling, R John

    2014-11-01

    Chemical signatures within the environment vary between regions as a result of climatological, geochemical and anthropogenic influences. These variations are incorporated into the region's geology, soils, water and vegetation; ultimately making their way through the food chain to higher level organisms. Because the variation in chemical signatures between areas is significant, a specific knowledge of differences in elemental distribution patterns between, and within populations, could prove beneficial for provenancing animals or animal related products when applied to indigenous and feral faunal populations. The domestic pig (Sus scrofa domestica) was used as an investigative model to determine the feasibility of using a chemical traceability method for the provenance determination of animal tissue. Samples of pig muscle, tongue, stomach, heart, liver and kidney were collected from known farming areas around Australia. Samples were digested in 1:3 H2O2:HNO3 and their elemental composition determined using solution based Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Pigs from different growing regions in Australia could be distinguished based on the chemical signature of each individual tissue type. Discrimination was possible at a region, state and population level. This investigation demonstrates the potential for multi-element analysis of low genetic variation native and feral species of forensic relevance. PMID:25240220

  17. Immobilized Metal Affinity Chromatography Coupled to Multiple Reaction Monitoring Enables Reproducible Quantification of Phospho-signaling.

    Science.gov (United States)

    Kennedy, Jacob J; Yan, Ping; Zhao, Lei; Ivey, Richard G; Voytovich, Uliana J; Moore, Heather D; Lin, Chenwei; Pogosova-Agadjanyan, Era L; Stirewalt, Derek L; Reding, Kerryn W; Whiteaker, Jeffrey R; Paulovich, Amanda G

    2016-02-01

    A major goal in cell signaling research is the quantification of phosphorylation pharmacodynamics following perturbations. Traditional methods of studying cellular phospho-signaling measure one analyte at a time with poor standardization, rendering them inadequate for interrogating network biology and contributing to the irreproducibility of preclinical research. In this study, we test the feasibility of circumventing these issues by coupling immobilized metal affinity chromatography (IMAC)-based enrichment of phosphopeptides with targeted, multiple reaction monitoring (MRM) mass spectrometry to achieve precise, specific, standardized, multiplex quantification of phospho-signaling responses. A multiplex immobilized metal affinity chromatography- multiple reaction monitoring assay targeting phospho-analytes responsive to DNA damage was configured, analytically characterized, and deployed to generate phospho-pharmacodynamic curves from primary and immortalized human cells experiencing genotoxic stress. The multiplexed assays demonstrated linear ranges of ≥3 orders of magnitude, median lower limit of quantification of 0.64 fmol on column, median intra-assay variability of 9.3%, median inter-assay variability of 12.7%, and median total CV of 16.0%. The multiplex immobilized metal affinity chromatography- multiple reaction monitoring assay enabled robust quantification of 107 DNA damage-responsive phosphosites from human cells following DNA damage. The assays have been made publicly available as a resource to the community. The approach is generally applicable, enabling wide interrogation of signaling networks. PMID:26621847

  18. Thin layer chromatography coupled to paper spray ionization mass spectrometry for cocaine and its adulterants analysis.

    Science.gov (United States)

    De Carvalho, Thays C; Tosato, Flavia; Souza, Lindamara M; Santos, Heloa; Merlo, Bianca B; Ortiz, Rafael S; Rodrigues, Rayza R T; Filgueiras, Paulo R; França, Hildegardo S; Augusti, Rodinei; Romão, Wanderson; Vaz, Boniek G

    2016-05-01

    Thin layer chromatography (TLC) is a simple and inexpensive type of chromatography that is extensively used in forensic laboratories for drugs of abuse analysis. In this work, TLC is optimized to analyze cocaine and its adulterants (caffeine, benzocaine, lidocaine and phenacetin) in which the sensitivity (visual determination of LOD from 0.5 to 14mgmL(-1)) and the selectivity (from the study of three different eluents: CHCl3:CH3OH:HCOOHglacial (75:20:5v%), (C2H5)2O:CHCl3 (50:50v%) and CH3OH:NH4OH (100:1.5v%)) were evaluated. Aiming to improve these figures of merit, the TLC spots were identified and quantified (linearity with R(2)>0.98) by the paper spray ionization mass spectrometry (PS-MS), reaching now lower LOD values (>1.0μgmL(-1)). The method developed in this work open up perspective of enhancing the reliability of traditional and routine TLC analysis employed in the criminal expertise units. Higher sensitivity, selectivity and rapidity can be provided in forensic reports, besides the possibility of quantitative analysis. Due to the great simplicity, the PS(+)-MS technique can also be coupled directly to other separation techniques such as the paper chromatography and can still be used in analyses of LSD blotter, documents and synthetic drugs. PMID:26970868

  19. Mathematical Modeling of the Three Phase Induction Motor Couple to DC Motor in Hybrid Electric Vehicle

    Directory of Open Access Journals (Sweden)

    Zulkarnain Lubis

    2009-01-01

    Full Text Available Problem statement: With emphasis on a cleaner environment and efficient operation, vehicles today rely more and more heavily on electrical power generation for success. Approach: Mathematical modeling the components of the HEV as the three phase induction motor couple to DC motor in hybrid electric vehicle was introduced. The controller of Induction Motor (IM was designed based on input-output feedback linearization technique. It allowed greater electrical generation capacity and the fuel economy and emissions benefits of hybrid electric automotive propulsion. Results: A typical series hybrid electric vehicle was modeled and investigated. Conclusion: Various tests, such as acceleration traversing ramp and fuel consumption and emission were performed on the proposed model of 3 phase induction motor coupler DC motor in electric hybrid vehicles drive.

  20. Indirect hydrogen analysis by gas chromatography coupled to mass spectrometry (GC-MS).

    Science.gov (United States)

    Varlet, V; Smith, F; Augsburger, M

    2013-08-01

    Gas chromatography (GC) is an analytical tool very useful to investigate the composition of gaseous mixtures. The different gases are separated by specific columns but, if hydrogen (H2 ) is present in the sample, its detection can be performed by a thermal conductivity detector or a helium ionization detector. Indeed, coupled to GC, no other detector can perform this detection except the expensive atomic emission detector. Based on the detection and analysis of H2 isotopes by low-pressure chemical ionization mass spectrometry (MS), a new method for H2 detection by GC coupled to MS with an electron ionization ion source and a quadrupole analyser is presented. The presence of H2 in a gaseous mixture could easily be put in evidence by the monitoring of the molecular ion of the protonated carrier gas. PMID:23893637

  1. The population distribution of argon atoms in Paschen 1s levels in an inductively coupled plasma

    International Nuclear Information System (INIS)

    The population distribution of argon atoms in Paschen 1s levels in inductively coupled plasmas is investigated using a collisional-radiative model and the optical emission spectroscopy method. The modelling results of population densities are in good agreement with the experimental ones. According to this model, the population distribution of 1s levels is affected mainly by the electron impact transfer and the resonance radiation processes. As a result, a simple relationship on the population ratio of 1s4 and 1s5 is obtained. From this relationship, three kinetic regimes with different electron densities and discharge pressures are identified, which can be used to characterize the population distribution of argon 1s levels in inductively coupled plasmas.

  2. Determination of trace impurities in uranium hexafluoride using inductively coupled plasma-atomic emission spectroscopy

    International Nuclear Information System (INIS)

    A procedure has been developed to determine 30 trace elements in high-purity uranium hexafluoride (UF6) using inductively coupled plasma-atomic emission spectroscopy. The analytical method consists of a liquid-liquid extraction of the uranium from the trace impurities with a tri-(2-ethyl-hexyl)-phosphate (TEHP)-hexane mixture. A computer-controlled scanning monochromator system interfaced to an inductively coupled plasma (ICP) is then used to determine the levels of 30 trace elements present in the UF6. A single sample dissolution procedure is used for all elements investigated. This preliminary report details experimental work done to date as part of a countinuing program to determine metallic impurities in uranium by ICP

  3. Study on spatial distribution of plasma parameters in a magnetized inductively coupled plasma

    Energy Technology Data Exchange (ETDEWEB)

    Cheong, Hee-Woon; Lee, Woohyun; Kim, Ji-Won; Whang, Ki-Woong, E-mail: kwhang@snu.ac.kr [Plasma Laboratory, Inter-University Semiconductor Research Center, Department of Electrical and Computer Engineering, Seoul National University, Seoul 151-742 (Korea, Republic of); Kim, Hyuk [Samsung Electronics Co., Banwol-dong, Hwaseong 445-701 (Korea, Republic of); Park, Wanjae [Tokyo Electron Miyagi Ltd., Taiwa-cho, Kurokawa-gun, Miyagi 981-3629 (Japan)

    2015-07-15

    Spatial distributions of various plasma parameters such as plasma density, electron temperature, and radical density in an inductively coupled plasma (ICP) and a magnetized inductively coupled plasma (M-ICP) were investigated and compared. Electron temperature in between the rf window and the substrate holder of M-ICP was higher than that of ICP, whereas the one just above the substrate holder of M-ICP was similar to that of ICP when a weak (<8 G) magnetic field was employed. As a result, radical densities in M-ICP were higher than those in ICP and the etch rate of oxide in M-ICP was faster than that in ICP without severe electron charging in 90 nm high aspect ratio contact hole etch.

  4. Considerations about the detection efficiency in inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Experimental investigations of analyte atomization, ionization and diffusion processes in the inductively coupled plasma applying single droplet introduction and optical emission spectroscopy provide hints how to improve the detection efficiency of inductively coupled plasma mass spectrometry. It is discussed how the flow, amount and type of injector gas, the size of droplets injected, the analyte mass, and the sampler interface of the mass spectrometer determine the position of analyte atomization and ionization as well as the magnitude of radial analyte ion diffusion at the interface of the mass spectrometer applied. - Highlights: ► Parameters determining analyte atomization and ionization in ICP's are discussed. ► Dependence of analyte diffusion on experimental conditions is described. ► Actions for improving the detection efficiency of ICP-MS are highlighted.

  5. Trace element analysis of samples by inductively coupled plasma mass spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    This paper reports the capability of inductively coupled plasma mass spectrometry (ICP-MS) for trace elements determination in several types of sample. Sample preparation, standardization and detection including effect of chemical and instrumental interferences were discussed. The analytical results of water sample from UN GEMS/Water PE from an inter-comparison study and lichens (IAEA 338 and quality control material) from a proficiency test were presented. (Author)

  6. Copper Determination in Gunshot Residue by Cyclic Voltammetric and Inductive Coupled Plasma-Optical Emission Spectroscopy

    OpenAIRE

    Mohd Hashim Nurul’Afiqah Hashimah; Mohd Zain Zainiharyati; Jaafar Mohd Zuli

    2016-01-01

    Analysis of gunshot residue (GSR) is a crucial evidences for a forensic analyst in the fastest way. GSR analysis insists a suitable method provides a relatively simple, rapid and precise information on the spot at the crime scene. Therefore, the analysis of Cu(II) in GSR using cyclic voltammetry (CV) on screen printed carbon electrode (SPCE) is a better choice compared to previous alternative methods such as Inductive Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) those required a lon...

  7. OPTIMAL CONTROL OF A NONLINEAR COUPLED ELECTROMAGNETIC INDUCTION HEATING SYSTEM WITH POINTWISE STATE CONSTRAINTS

    OpenAIRE

    Irwin Yousept

    2010-01-01

    An optimal control problem arising in the context of 3D electromagnetic induction heating is investigated. The state equation is given by a quasilinear stationary heat equation coupled with a semilinear time harmonic eddy current equation. The temperature-dependent electrical conductivity and the presence of pointwise inequality state-constraints represent the main challenge of the paper. In the first part of the paper, the existence and regularity of the state are addressed. The second part ...

  8. Computational Finite Element Software Assisted Development of a 3D Inductively Coupled Power Transfer System

    OpenAIRE

    Pratik Raval; Dariusz Kacprzak; Aiguo Patrick Hu

    2014-01-01

    To date inductively coupled power transfer (ICPT) systems have already found many practical applications including battery charging pads. In fact, current charging platforms tend to largely support only one- or two-dimensional planar movement in load. This paper proposes a new concept of extending the aspect ratios of the operating power transfer volume of ICPT systems to support arbitrary three dimensional load movements with respect to the primary coils. This is done by use of modern finite...

  9. On frequency optimization of assymetric resonant inductive coupling wireless power transfer links

    OpenAIRE

    Egidos, Nuria; Bou, Elisenda; Sedwick, Raymond; Alarcón Cot, Eduardo José

    2014-01-01

    Resonant Inductive Coupling Wireless Power Transfer (RIC-WPT) is a leading field of research due to the growing number of applications that can benefit from this technology: from biomedical implants to consumer electronics, fractionated spacecraft and electric vehicles amongst others. However, current applications are limited to symetric point-to-point-links. New challenges and applications of RIC-WPT emphasize the necessity to explore, predict and optimize the behavior of these links for dif...

  10. TRACE ELEMENTS ANALYSIS IN PAPER USING INDUCTIVELY COUPLED PLASMA - MASS SPECTROMETRY (ICP - MS)

    OpenAIRE

    ABOUL-ENEIN, Y; TANASE, I. Gh.; UDRISTIOIU, Florin Mihai; BUNACIU, Andrei A.

    2012-01-01

    The forensic examination and dating of documents is important in our society, because documents are used throughout our lives to record everything we do. The analysis of questioned documents therefore involves different types of analysis including comparison of the handwriting, ink, typescript or print, as well as physical and chemical characterization of the paper itself. Inductively coupled plasma mass spectrometry (ICP-MS) has already successfully been applied to applications in geology, f...

  11. Wave Energy Conversion: Direct Coupled Point Absorber in Heave with Induction Machine as Power Take Off

    OpenAIRE

    Skjervheim, Ottar

    2007-01-01

    In the area of offshore renewable, wave energy can give great contribution. There has been research for developing wave energy converters since the late eighteenth century when the first patent was applied for in 1799 [1], without any remarkable breakthrough. This master thesis will discuss the topic of wave energy conversion by a point absorber in heave with a directly coupled induction machine power take off. A wave to wire approach has been attempted in this thesis. The tool needed is a h...

  12. Ion balance in waters through inductively coupled plasma optical emission spectrometry

    OpenAIRE

    Sánchez Rodríguez, Carlos; Maestre Pérez, Salvador; Prats Moya, Soledad; Todolí Torró, José Luis

    2014-01-01

    Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) has been employed to carry out the determination of both major anions and cations in water samples. The anion quantification has been performed by means of a new automatic accessory. In this device chloride has been determined by continuously adding a silver nitrate solution. As a result solid silver chloride particles are formed and retained on a nylon filter inserted in the line. The emission intensity is read at a silver ch...

  13. Atomic Mineral Characteristics of Indonesian Osteoporosis by High-Resolution Inductively Coupled Plasma Mass Spectrometry

    OpenAIRE

    Zairin Noor; Sutiman Bambang Sumitro; Mohammad Hidayat; Agus Hadian Rahim; Akhmad Sabarudin; Tomonari Umemura

    2012-01-01

    Clinical research indicates that negative calcium balance is associated with low bone mass, rapid bone loss, and high fracture rates. However, some studies revealed that not only calcium is involved in bone strengthening as risk factor of fracture osteoporosis. Thus, in this report, the difference of metallic and nonmetallic elements in osteoporosis and normal bones was studied by high-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS). The influence of these elements on bone...

  14. Plutonium age dating (production date measurement) by inductively coupled plasma mass spectrometry

    OpenAIRE

    Varga, Zsolt; Nicholl, Adrian; Wallenius, Maria; Mayer, Klaus

    2015-01-01

    This paper describes rapid methods for the determination of the production date (age dating) of plutonium (Pu) materials by inductively coupled plasma mass spectrometry (ICP-MS) for nuclear forensic and safeguards purposes. One of the presented methods is a rapid, direct measurement without chemical separation using 235U/239Pu and 236U/240Pu chronometers. The other method comprises a straightforward extraction chromatographic separation, followed by ICP-MS measurement for the 234U/238Pu, 235U...

  15. Determination of Trace Elements in Ice Core Samples by Laser Ablation Inductively Coupled Plasma Mass Spectrometry

    OpenAIRE

    Reinhardt, Heiko; Kriews, Michael; Schrems, Otto; Lüdke, C.; Hoffmann, E; Skole, J.

    2001-01-01

    The snow and iceshields of the polar regions serve as a climate archiveand deliver a useful insight back to about 250.000 years of earth climatehistory1,2. The aim of our investigation reported here was to establisha new method for the determination of trace elements in ice cores frompolar regions with Laserablation Inductively Coupled Plasma MassSpectrometry (LA-ICP-MS)3. Primarily, the construction of a cryogeniclaserablation chamber and the optimization of the analysis system forthe sample...

  16. 87Sr/86Sr measurements on marine sediments by inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    The application of inductively coupled plasma-mass spectrometry (ICP-MS) is documented for the study of the strontium isotopic composition (87Sr/86Sr) in geological samples, i.e. in the marine lithic fraction of core sediments. Methods for the determination of the isotopic composition, its accuracy and precision are reported. The results obtained simultaneously on 11 samples by both ICP-MS and thermal ionization mass spectrometry (TIMS) reveal a very good correlation (r2 = 0.955). (orig.)

  17. Development of analytical methods for multiplex bio-assay with inductively coupled plasma mass spectrometry

    OpenAIRE

    Ornatsky, Olga I.; Kinach, Robert; Bandura, Dmitry R.; Lou, Xudong; Tanner, Scott D; Baranov, Vladimir I.; Nitz, Mark; Mitchell A. Winnik

    2008-01-01

    Advances in the development of highly multiplexed bio-analytical assays with inductively coupled plasma mass spectrometry (ICP-MS) detection are discussed. Use of novel reagents specifically designed for immunological methods utilizing elemental analysis is presented. The major steps of method development, including selection of elements for tags, validation of tagged reagents, and examples of multiplexed assays, are considered in detail. The paper further describes experimental protocols for...

  18. Iron-Isotopic Fractionation Studies Using Multiple Collector Inductively Coupled Plasma Mass Spectrometry

    Science.gov (United States)

    Anbar, A. D.; Zhang, C.; Barling, J.; Roe, J. E.; Nealson, K. H.

    1999-01-01

    The importance of Fe biogeochemistry has stimulated interest in Fe isotope fractionation. Recent studies using thermal ionization mass spectrometry (TIMS) and a "double spike" demonstrate the existence of biogenic Fe isotope effects. Here, we assess the utility of multiple-collector inductively-coupled plasma mass spectrometry(MC-ICP-MS) with a desolvating sample introduction system for Fe isotope studies, and present data on Fe biominerals produced by a thermophilic bacterium. Additional information is contained in the original extended abstract.

  19. Determination of trace elements in petroleum products by inductively coupled plasma techniques: A critical review

    OpenAIRE

    Sánchez Romero, Raquel; Todolí Torró, José Luis; Lienemann, Charles Philippe; Mermet, Jean Michel

    2013-01-01

    The fundamentals, applications and latter developments of petroleum products analysis through inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are revisited in the present bibliographic survey. Sample preparation procedures for the direct analysis of fuels by using liquid sample introduction systems are critically reviewed and compared. The most employed methods are sample dilution, emulsion or micro-emulsion preparation and sample decompositio...

  20. Determination of uranium and thorium isotope ratios by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Measurements conditions were selected and a procedure was proposed for determining the 234U/238U and 230Th/232Th isotope ratios using an ELEMENT single-channel double-focusing inductively coupled plasma mass spectrometer. The procedure was tested in analyzing bottom sediments from Lake Baikal with the extraction preconcentration of uranium and thorium. The accuracy of the procedure was verified using certified reference materials and a model solution by comparing the results obtained with the data of α spectrometry

  1. Applications of inductively coupled plasma mass spectrometry to the production control of aerospace and nuclear materials

    International Nuclear Information System (INIS)

    Inductively coupled plasma source mass spectrometry (ICP-MS) has proved to be a useful practical tool in a high-volume quality control laboratory. The application of this technique to materials produced for the aerospace and nuclear industries is discussed. Techniques employed for uranium isotope ratio determination and elemental determination of gadolinium, samarium and thorium in hafnium and zirconium alloys are described. Strategies employed for a semi-quantitative survey analysis for a wide range of elements are also presented. (author)

  2. Photon noise limited radiation detection with lens-antenna coupled Microwave Kinetic Inductance Detectors

    OpenAIRE

    Yates, S J C; Baselmans, J. J. A.; Endo, A; Janssen, R. M. J.; Ferrari, L; Diener, P.; Baryshev, A.M.

    2011-01-01

    Microwave kinetic inductance detectors (MKIDs) have shown great potential for sub-mm instrumentation because of the high scalability of the technology. Here, we demonstrate for the first time in the sub-mm band (0.1–2 mm) a photon noise limited performance of a small antenna coupled MKID detector array and we describe the relation between photon noise and MKID intrinsic generation-recombination noise. Additionally, we use the observed photon noise to measure the optical efficiency of detector...

  3. Integrated CFD Model for Nanoparticle Production in Inductively Coupled Plasma Reactor: Implementation and Application

    OpenAIRE

    Benros Santos Lopes, Silvania

    2016-01-01

    Nanoparticles represent a very exciting new area of research. Their small size, ranging from several nanometers to tens of nanometers, is responsible for many changes in the structural, thermal, electromagnetic, optical and mechanical properties in comparison with the bulk solid of the same materials. However, promoting the use of such material requires well-controlled synthesis techniques to be developed. Inductively coupled thermal plasma (ICTP) reactors have been shown to offer unique adva...

  4. Plasma Diagnostics and Plasma-Surface Interactions in Inductively Coupled Plasmas

    OpenAIRE

    Titus, Monica Joy

    2010-01-01

    The semiconductor industry's continued trend of manufacturing device features on the nanometer scale requires increased plasma processing control and improved understanding of plasma characteristics and plasma-surface interactions. This dissertation presents a series of experimental results for focus studies conducted in an inductively coupled plasma (ICP) system. First novel "on-wafer" diagnostic tools are characterized and related to plasma characteristics. Second, plasma-polymer interactio...

  5. Quantum Fluctuations of Mesoscopic Damped Circuit Involving Capacitance-Inductance Coupling at a Finite Temperature

    Science.gov (United States)

    Xu, Xing-Lei; Xu, Shi-Min; Li, Hong-Qi

    2008-06-01

    The quantization of mesoscopic damped circuit involving capacitance-inductance coupling is proposed by the method of thrice linear transformation and damped harmonic oscillator quantization. The quantum fluctuations of the charges and current of each loop are calculated by thermo-field dynamics (TFD) in thermal vacuum state, thermal coherent state and thermal squeezed state, respectively. It is shown that the quantum fluctuations of the charges and current not only depend on circuit inherent parameter and coupled magnitude, but also rely on squeezed coefficients, squeezed angle, environmental temperature and damped resistance. And, because of influence of environmental temperature and damped resistance, the quantum fluctuations increase with increasing temperature and decrease with prolonging time.

  6. Determination of trace elements in petroleum products by inductively coupled plasma techniques: A critical review

    International Nuclear Information System (INIS)

    The fundamentals, applications and latter developments of petroleum products analysis through inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are revisited in the present bibliographic survey. Sample preparation procedures for the direct analysis of fuels by using liquid sample introduction systems are critically reviewed and compared. The most employed methods are sample dilution, emulsion or micro-emulsion preparation and sample decomposition. The first one is the most widely employed due to its simplicity. Once the sample has been prepared, an organic matrix is usually present. The performance of the sample introduction system (i.e., nebulizer and spray chamber) depends strongly upon the nature and properties of the solution finally obtained. Many different devices have been assayed and the obtained results are shown. Additionally, samples can be introduced into the plasma by using an electrothermal vaporization (ETV) device or a laser ablation system (LA). The recent results published in the literature showing the feasibility, advantages and drawbacks of latter alternatives are also described. Therefore, the main goal of the review is the discussion of the different approaches developed for the analysis of crude oil and its derivates by inductively coupled plasma (ICP) techniques. - Highlights: • Analysis of petroleum products by inductively coupled plasma techniques is revisited. • Fundamental studies are included together with reports dealing with applications. • Conventional and non-conventional sample introduction methods are considered. • Sample preparation methods are critically compared and described

  7. Thermochemical Nonequilibrium 2D Modeling of Nitrogen Inductively Coupled Plasma Flow

    Science.gov (United States)

    Yu, Minghao; Yusuke, Takahashi; Hisashi, Kihara; Ken-ichi, Abe; Kazuhiko, Yamada; Takashi, Abe; Satoshi, Miyatani

    2015-09-01

    Two-dimensional (2D) numerical simulations of thermochemical nonequilibrium inductively coupled plasma (ICP) flows inside a 10-kW inductively coupled plasma wind tunnel (ICPWT) were carried out with nitrogen as the working gas. Compressible axisymmetric Navier-Stokes (N-S) equations coupled with magnetic vector potential equations were solved. A four-temperature model including an improved electron-vibration relaxation time was used to model the internal energy exchange between electron and heavy particles. The third-order accuracy electron transport properties (3rd AETP) were applied to the simulations. A hybrid chemical kinetic model was adopted to model the chemical nonequilibrium process. The flow characteristics such as thermal nonequilibrium, inductive discharge, effects of Lorentz force were made clear through the present study. It was clarified that the thermal nonequilibrium model played an important role in properly predicting the temperature field. The prediction accuracy can be improved by applying the 3rd AETP to the simulation for this ICPWT. supported by Grant-in-Aid for Scientific Research (No. 23560954), sponsored by the Japan Society for the Promotion of Science

  8. Determination of trace elements in petroleum products by inductively coupled plasma techniques: A critical review

    Energy Technology Data Exchange (ETDEWEB)

    Sánchez, Raquel [Department of Analytical Chemistry, Nutrition and Food Sciences, P.O. Box 99, 03080, Alicante (Spain); Todolí, José Luis, E-mail: jose.todoli@ua.es [Department of Analytical Chemistry, Nutrition and Food Sciences, P.O. Box 99, 03080, Alicante (Spain); Lienemann, Charles-Philippe [IFP Energies Nouvelles, Rond-point de l' échangeur de Solaize, BP 3, F-69360 Solaize (France); Mermet, Jean-Michel [Spectroscopy Forever, 01390 Tramoyes (France)

    2013-10-01

    The fundamentals, applications and latter developments of petroleum products analysis through inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are revisited in the present bibliographic survey. Sample preparation procedures for the direct analysis of fuels by using liquid sample introduction systems are critically reviewed and compared. The most employed methods are sample dilution, emulsion or micro-emulsion preparation and sample decomposition. The first one is the most widely employed due to its simplicity. Once the sample has been prepared, an organic matrix is usually present. The performance of the sample introduction system (i.e., nebulizer and spray chamber) depends strongly upon the nature and properties of the solution finally obtained. Many different devices have been assayed and the obtained results are shown. Additionally, samples can be introduced into the plasma by using an electrothermal vaporization (ETV) device or a laser ablation system (LA). The recent results published in the literature showing the feasibility, advantages and drawbacks of latter alternatives are also described. Therefore, the main goal of the review is the discussion of the different approaches developed for the analysis of crude oil and its derivates by inductively coupled plasma (ICP) techniques. - Highlights: • Analysis of petroleum products by inductively coupled plasma techniques is revisited. • Fundamental studies are included together with reports dealing with applications. • Conventional and non-conventional sample introduction methods are considered. • Sample preparation methods are critically compared and described.

  9. Development and application of liquid chromatography coupled to isotope ratio mass spectrometry

    International Nuclear Information System (INIS)

    Stable isotope analysis has found widespread applications in various disciplines such as archaeology, geochemistry, biology, food authenticity, and forensic science. Coupling chromatography to isotope ratio mass spectrometry for compound-specific isotope analysis (CSIA) is a trend, as it provides several advantages over bulk isotope analysis, e.g., relatively simple sample preparation, the ability to measure individual compounds in a complex mixture in one run, and the reduced sample size required for precise isotope analysis. Gas chromatography coupled to isotope ratio mass spectrometry (GC/IRMS) has been well-established for compound-specific isotope analysis of volatile organic compounds within the last two decades. However, an interface combining liquid chromatography with isotope ratio mass spectrometry (LC/IRMS) was not commercially available until 2004. The current design of the interface requires using a carbon-free eluent in chromatographic separation. This requirement limits the application of the most frequently used reversed-phase liquid chromatography in CSIA, because the elution strength of water at room temperature is too low to serve as mobile phase in reversed-phase separations. In order to increase the elution strength of water, we propose using high temperature water for chromatographic elution. The polarity of water decreases with an increase of temperature, yielding increased elution strength in reversed-phase columns. Therefore, high temperature water can be used as eluent instead of organic solvent for combining reversed-phase liquid chromatography with isotope ratio mass spectrometry (RPLC/IRMS). Additionally, temperature gradients can replace organic solvent gradients to increase chromatographic resolution. This is very important for LC/IRMS analysis, as precise isotope analysis requires baseline separation of analytes. In this thesis, high-temperature reversed-phase liquid chromatography was coupled to, and for the first time carefully

  10. Development and application of liquid chromatography coupled to isotope ratio mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Lijun

    2014-02-19

    Stable isotope analysis has found widespread applications in various disciplines such as archaeology, geochemistry, biology, food authenticity, and forensic science. Coupling chromatography to isotope ratio mass spectrometry for compound-specific isotope analysis (CSIA) is a trend, as it provides several advantages over bulk isotope analysis, e.g., relatively simple sample preparation, the ability to measure individual compounds in a complex mixture in one run, and the reduced sample size required for precise isotope analysis. Gas chromatography coupled to isotope ratio mass spectrometry (GC/IRMS) has been well-established for compound-specific isotope analysis of volatile organic compounds within the last two decades. However, an interface combining liquid chromatography with isotope ratio mass spectrometry (LC/IRMS) was not commercially available until 2004. The current design of the interface requires using a carbon-free eluent in chromatographic separation. This requirement limits the application of the most frequently used reversed-phase liquid chromatography in CSIA, because the elution strength of water at room temperature is too low to serve as mobile phase in reversed-phase separations. In order to increase the elution strength of water, we propose using high temperature water for chromatographic elution. The polarity of water decreases with an increase of temperature, yielding increased elution strength in reversed-phase columns. Therefore, high temperature water can be used as eluent instead of organic solvent for combining reversed-phase liquid chromatography with isotope ratio mass spectrometry (RPLC/IRMS). Additionally, temperature gradients can replace organic solvent gradients to increase chromatographic resolution. This is very important for LC/IRMS analysis, as precise isotope analysis requires baseline separation of analytes. In this thesis, high-temperature reversed-phase liquid chromatography was coupled to, and for the first time carefully

  11. Development and characterization of induction heating electrothermal vaporization (IH-ETV) sample introduction for inductively coupled plasma spectrometry

    Science.gov (United States)

    Rybak, Michael E.; Salin, Eric D.

    2001-03-01

    A general study of performance attributes was conducted for a prototypical electrothermal vaporization (ETV) sample introduction system, in which induction heating (IH) was used to facilitate the drying, pyrolysis, and vaporization of samples from long, undercut graphite cup probes in a radio-frequency (RF) induction field. In the first part of this study, experiments were carried out to determine the heating characteristics and temperature control aspects of an IH-ETV arrangement. Using a remote-sensing infrared thermocouple, it was determined that a 3/8-inch (9.53-mm) outer diameter graphite cup sample probe could be heated to a maximum temperature of 1860°C in the induction field of the IH-ETV under full forward power (1.5 kW). The IH-ETV device was found to have a rapid heating response (1/ e time-constant of 2.0±0.2 s) that was independent of the initial/final temperatures chosen. Linear temperature control was possible by regulating either the DC voltage applied to the plate or the current flowing to the grid of the RF generator oscillator tube. The second part of this work consisted of studies to establish benchmarks, such as limits of detection (LOD) with inductively coupled plasma optical emission spectrometry (ICP-OES) and transport efficiency for analyte vaporization under several x-Ar mixed gas atmospheres [where x=15% N 2, 10% O 2, HCl (sparged), or 15% SF 6 (v/v)]. In general, reproducible transient signals with evolution times of 5-15 s were seen for the vaporization of most elements studied, with peak area intensity and reproducibility generally being the best with SF 6-Ar. A 10-fold increase in transport efficiency was seen for refractory carbide-forming analytes (Cr, V) when vaporization was conducted in a halogenous ( x=HCl, SF 6) versus non-halogenous ( x=N 2, O 2) environment, with a two-fold improvement being observed for most other non-refractory elements (Cd, Cu, Fe, Mn, Ni, Pb, Zn). The transport of arsenic proved to be a special case

  12. Induction

    DEFF Research Database (Denmark)

    Sprogøe, Jonas; Elkjaer, Bente

    2010-01-01

    The purpose of this paper is to explore how induction of newcomers can be understood as both organizational renewal and the maintenance of status quo, and to develop ways of describing this in terms of learning.......The purpose of this paper is to explore how induction of newcomers can be understood as both organizational renewal and the maintenance of status quo, and to develop ways of describing this in terms of learning....

  13. Determination of selenomethionine, selenocysteine, and inorganic selenium in eggs by HPLC-inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lipiec, Elzbieta; Siara, Grzegorz [CNRS/UPPA, Laboratoire de Chimie Analytique Bio-Inorganique et Environnement, Pau (France); Warsaw University of Technology, Warsaw (Poland); Bierla, Katarzyna; Ouerdane, Laurent; Szpunar, Joanna [CNRS/UPPA, Laboratoire de Chimie Analytique Bio-Inorganique et Environnement, Pau (France)

    2010-05-15

    A method for the simultaneous determination of selenomethionine (SeMet), selenocysteine (SeCys), and selenite [Se(IV)] in chicken eggs was developed. A sample preparation protocol including defatting, protein denaturation, and carbamidomethylation was optimized in order to achieve complete protein digestion and to avoid SeCys losses. Quantification was carried out by reversed-phase HPLC-inductively coupled plasma mass spectrometry (ICP MS) after quantitative isolation of the selenium-containing fraction by size-exclusion liquid chromatography. The detection limits were 0.06, 0.003, and 0.01 {mu}g g{sup -1} (dry weight) for SeCys, Se(IV) and SeMet, respectively, and the precision was 5-10%. The end products of carbamidomethylation of the different selenium species were identified for the first time by electrospray QTOF MS after custom-designed 2D HPLC purification. Differences in selenium speciation in egg yolk and white were highlighted, the yolk containing more SeCys and the white more SeMet. An insight into selenium bioaccessibility in eggs was obtained by digestion with simulated gastric and gastrointestinal juices and size-exclusion HPLC-ICP MS. (orig.)

  14. RAPID DETERMINATION OF 237 NP AND PU ISOTOPES IN WATER BY INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY AND ALPHA SPECTROMETRY

    Energy Technology Data Exchange (ETDEWEB)

    Maxwell, S.; Jones, V.; Culligan, B.; Nichols, S.; Noyes, G.

    2010-06-23

    A new method that allows rapid preconcentration and separation of plutonium and neptunium in water samples was developed for the measurement of {sup 237}Np and Pu isotopes by inductively-coupled plasma mass spectrometry (ICP-MS) and alpha spectrometry; a hybrid approach. {sup 238}U can interfere with {sup 239}Pu measurement by ICP-MS as {sup 238}UH{sup +} mass overlap and {sup 237}Np via peak tailing. The method provide enhanced removal of uranium by separating Pu and Np initially on TEVA Resin, then moving Pu to DGA resin for additional removal of uranium. The decontamination factor for uranium from Pu is almost 100,000 and the decontamination factor for U from Np is greater than 10,000. This method uses stacked extraction chromatography cartridges and vacuum box technology to facilitate rapid separations. Preconcentration is performed using a streamlined calcium phosphate precipitation method. Purified solutions are split between ICP-MS and alpha spectrometry so that long and short-lived Pu isotopes can be measured successfully. The method allows for simultaneous extraction of 20 samples (including QC samples) in 4 to 6 hours, and can also be used for emergency response. {sup 239}Pu, {sup 242}Pu and {sup 237}Np were measured by ICP-MS, while {sup 236}Pu, {sup 238}Pu, and {sup 239}Pu were measured by alpha spectrometry.

  15. Coupling Charge Reduction Mass Spectrometry to Liquid Chromatography for Complex Mixture Analysis.

    Science.gov (United States)

    Stutzman, John R; Crowe, Matthew C; Alexander, James N; Bell, Bruce M; Dunkle, Melissa N

    2016-04-01

    Electrospray ionization (ESI) of solution mixtures often generates complex mass spectra, even following liquid chromatography (LC), due to analyte multiple charging. Multiple charge state distributions can lead to isobaric interferences, mass spectral congestion, and ambiguous ion identification. As a consequence, data interpretation increases in complexity. Several charge reduction mass spectrometry (MS) approaches have been previously developed to reduce the average charge state of gaseous ions; however, all of these techniques have been restricted to direct infusion MS. In this study, synthetic polyols and surfactants separated by liquid chromatography and ionized by positive mode ESI have been subjected to polonium-210 α-particle radiation to reduce the average charge state to singly charged cations prior to mass analysis. LC/MS analysis of 5000 molecular weight poly(ethylene glycol) (PEG5000) generated an average charge state of 5.88+; whereupon, liquid chromatography/electrospray ionization/charge reduction/mass spectrometry (LC/CR/MS) analysis of PEG 5000 generated an average charge state of 1.00+. The PEG5000 results demonstrated a decrease in spectral complexity and enabled facile interpretation. Other complex solution mixtures representing specific MS challenges (i.e., competitive ionization and isobaric ion overlap) were explored and analyzed with LC/CR/MS to demonstrate the benefits of coupling LC to CR/MS. For example, polyol information related to initiator, identity/relative amount of monomer, and estimated molecular weight was characterized in random and triblock ethylene oxide/propylene oxide polyols using LC/CR/MS. LC/CR/MS is a new analytical technique for the analysis of complex mixtures. PMID:26971559

  16. Effect of coupling currents on the dynamic inductance during fast transient in superconducting magnets

    Science.gov (United States)

    Marinozzi, V.; Sorbi, M.; Manfreda, G.; Bellina, F.; Bajas, H.; Chlachidze, G.

    2015-03-01

    We present electromagnetic models aiming to calculate the variation of the inductance in a magnet due to dynamic effects such as the variation of magnetization or the coupling with eddy currents. The models are studied with special regard to the calculation of the inductance in superconducting magnets which are affected by interfilament coupling currents. The developed models have been compared with experimental data coming from tests of prototype Nb3Sn magnets designed for the new generation of accelerators. This work is relevant for the quench protection study of superconducting magnets: quench is an unwanted event, when part of the magnet becomes resistive; in these cases, the current should be discharged as fast as possible, in order to maintain the resistive zone temperature under a safe limit. The magnet inductance is therefore a relevant term for the description of the current discharge, especially for the high-field new generation superconducting magnets for accelerators, and this work shows how to calculate the correct value during rapid current changes, providing a mean for simulations of the reached temperature.

  17. Specific Aspects Regarding Coupled Numerical Modeling of Inverter and Load Equipments in an Induction Heating Installation

    Directory of Open Access Journals (Sweden)

    Claudiu MICH-VANCEA

    2008-05-01

    Full Text Available The most propitious projection of inductiveelectrothermic installation requires a deep study ofcoupled electrothermic and circuits problems; thereforethe present paper follows the same line. Research inspecific literature have emphasized that induction heatinghas a much higher efficiency if the supply of the charge(inductor – piece is done at frequencies other thatindustrial one. [1]. Due to material alter depending ontemperature and, implicitly, the variation of the electricalparameters of the heating installation it is necessary totackle the projection of these inductive electrothermicinstallation projected through coupled numericalmodeling of the inverter circuit and of the heatingthrough induction process. The paper presents thenumerical modeling of the continuous current –alternating current conversion bridge (inverter withelements of static switch – over, the type of commandsignal (PWM of elements of static switch of power, thenumerical modeling of the heating throughelectromagnetic induction process and aspects ofcorrelation regarding the functioning/ working of theinstallation depending on the parameters of the load. Theparameters get modified due to material alter dependingon temperature during the heating process.

  18. Assessment of Pesticide Residues in Some Fruits Using Gas Chromatography Coupled with Micro Electron Capture Detector

    Directory of Open Access Journals (Sweden)

    M. I. Bhanger

    2011-12-01

    Full Text Available A very sensitive analytical method for the determination of 26 pesticides in some fruits based on solid phase extraction (SPE cleanup was developed using gas chromatography (GC coupled with micro electron capture detector (μECD. The identity of the pesticides was confirmed by gas chromatography mass spectroscopy (GC-MS using selected ion monitoring (SIM mode. Ethyl acetate was used as a solvent for the extraction of pesticide residues with assistance of sonication. For cleanup an octadecyl, C18 SPE column was used. A linear response of μECD was observed for all pesticides with good correlation coefficients (>0.9992. Proposed method was successfully applied for the determination of pesticide residues in the orange, apple, and grape fruits. Average recoveries achieved for all of the pesticides at fortification levels of 0.05, 1.0 and 2.0 μg g-1 in analyzed fruits were above 90% with relative standard deviations (RSD less than 6

  19. Fast separation of triterpenoid saponins using supercritical fluid chromatography coupled with single quadrupole mass spectrometry.

    Science.gov (United States)

    Huang, Yang; Zhang, Tingting; Zhou, Haibo; Feng, Ying; Fan, Chunlin; Chen, Weijia; Crommen, Jacques; Jiang, Zhengjin

    2016-03-20

    Triterpenoid saponins (TSs) are the most important components of some traditional Chinese medicines (TCMs) and have exhibited valuable pharmacological properties. In this study, a rapid and efficient method was developed for the separation of kudinosides, stauntosides and ginsenosides using supercritical fluid chromatography coupled with single quadrupole mass spectrometry (SFC-MS). The separation conditions for the selected TSs were carefully optimized after the initial screening of eight stationary phases. The best compromise for all compounds in terms of chromatographic performance and MS sensitivity was obtained when water (5-10%) and formic acid (0.05%) were added to the supercritical carbon dioxide/MeOH mobile phase. Beside the composition of the mobile phase, the nature of the make-up solvent for interfacing SFC with MS was also evaluated. Compared to reversed phase liquid chromatography, the SFC approach showed higher resolution and shorter running time. The developed SFC-MS methods were successfully applied to the separation and identification of TSs present in Ilex latifolia Thunb., Panax quinquefolius L. and Panax ginseng C.A. Meyer. These results suggest that this SFC-MS approach could be employed as a useful tool for the quality assessment of natural products containing TSs as active components. PMID:26773536

  20. ANALYSIS OF PENTACHLOROPHENOL IN WATER BY PURGE AND TRAP CONCENTRATOR COUPLED TO GAS CHROMATOGRAPHY

    Institute of Scientific and Technical Information of China (English)

    HuixiaLan; YuancaiChen; ZhonghaoChen

    2004-01-01

    It is convenient and time saving to analyze pentachlorophenol (PCP) in water by purge and trap concentrator coupled to gas chromatography that avoids employing a great deal of organic solvent. In this paper, the appropriate purge and trap conditions of PCP are determined: the trapped sorbent is TenaxGC; the purge gas is pure nitrogen and purge flow is 40ml/min; the purge time is 30min. A series of standard PCP water samples 5, 10, 50, 100, 200, 400, 800, 1000ppb are analyzed in order to obtain standard curve, and the linear regressive equation obtained is Y=109.65X-687.72, which correlation coefficient r is 0.9949. The precision of the method is determined with 0.5ppb PCP water sample, and the standard deviation measured is 3%. The detection limit for PCP is 0.2ppb.

  1. ANALYSIS OF PENTACHLOROPHENOL IN WATER BY PURGE AND TRAP CONCENTRATOR COUPLED TOGAS CHROMATOGRAPHY

    Institute of Scientific and Technical Information of China (English)

    Huixia Lan; Yuancai Chen; Zhonghao Chen

    2004-01-01

    It is convenient and time saving to analyze pentachlorophenol (PCP) in water by purge and trap concentrator coupled to gas chromatography that avoids employing a great deal of organic solvent: In this paper, the appropriate purge and trap conditions of PCP are determined: the trapped sorbent is TenaxGC; the purge gas is pure nitrogen and purge flow is 40ml/min; the purge time is 30min. A series of standard PCP water samples 5, 10, 50, 100, 200,400, 800, 1000ppb are analyzed in order to obtain standard curve, and the linear regressive equation obtained is Y=109.65X-687.72, which correlation coefficient r is 0.9949. The precision of the method is determined with 0.5ppb PCP water sample, and the standard deviation measured is 3%. The detection limit for PCP is 0.2ppb.

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

    International Nuclear Information System (INIS)

    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

  3. Diagnosis of propionic acidemia by gas chromatography coupled to mass spectrometry in a case analysis

    International Nuclear Information System (INIS)

    Propionic acidemia is an inherited metabolic disease caused by a deficiency in the propionyl-CoA carboxilase, a biotin-dependent mitochondrial enzyme. The disorder is a clinically heterogeneous disease and one of the most frequently occurring organic acidurias. We report the first Cuban case with a severe form of propionic acidemia followed by acidosis and death. The diagnosis was carried out by gas chromatography coupled to mass spectrometry. Our aim is to highlight the importance of organic acids urine analysis as part of the first laboratory tests in undiagnosed seriously ill children. The definitive diagnosis is important as it serves as a clear guideline to establish a suitable treatment and allows geneticists to provide patients with a proper genetic counseling

  4. Preparation of inulin-type fructooligosaccharides using fast protein liquid chromatography coupled with refractive index detection.

    Science.gov (United States)

    Li, J; Cheong, K L; Zhao, J; Hu, D J; Chen, X Q; Qiao, C F; Zhang, Q W; Chen, Y W; Li, S P

    2013-09-20

    A fast protein liquid chromatography coupled with refractive index detection (FPLC-RID) method was firstly developed for preparation and purification of fructooligosaccharides with different degree of polymerization from burdock, Arctium lappa. After extraction with 60% ethanol and decolorization with MCI gel CHP20P, total fructooligosaccharides were purified on Bio-Gel P-2 column eluted with water at the flow rate of 0.3 ml/min, which was the optimized conditions. The obtained fructooligosaccharides with degree of polymerization of 3-9 were identified based on their methylation analysis, MS and NMR data. This method has the advantages of high automation, good recovery and easy performance, which could be used for preparation of FOS from other sources, as well as other targeted compounds without UV absorbance. PMID:23962565

  5. Determination of organic and inorganic mercury species in Sungai Kinta, Perak by reversed-phase high performance liquid chromatography (HPLC) on-line coupled with ICP-MS

    International Nuclear Information System (INIS)

    This paper describes a simple method for mercury speciation in river water samples of Sungai Kinta, Perak. Separation and measurement were done by high-performance liquid chromatography on-line with inductively coupled plasma mass spectrometry (HPLC/ ICP-MS). Separation of mercury species was accomplished within 6 minutes on an AQ C18 4.6 mm i.d x 150 mm, 5 μm reversed phase column with 0.1 % (w/ v) L-cysteine as mobile phase. Under the optimum instrumental conditions, recoveries of 101-104 % for MeHg+ and 96 - 104 % for Hg2+ were obtained with experimental detection limits of 1ngL-1 for inorganic mercury and 1.5 μgL-1 for organic mercury. (author)

  6. Ion Flux and Ion Energy Distributions in an Inductively Coupled GEC Rf Refererence Cell in Chlorine

    Science.gov (United States)

    Radovanov, Svetlana; Forrister, Ray; Anderson, Harold

    1996-10-01

    Ion flux and energy distribution measurements in pure chlorine were performed in an inductively coupled Gaseous Electronics Reference Cell 13.56 MHz radiofrequency discharge . Measurements were made using miniaturized gridded energy analyzer. This detector was developed at the University of New Mexico, based on earlier design of the small size energy analyzers at MIT. The detector was mounted on a 12 inch water cooled carrier to suppress probe heating. The probe could be radially moved in the discharge cell to monitor the radial uniformity of the plasma. In addition, the detector was protected with a ceramic coating to supress for the electron saturation current of unshielded probe areas. The measurements were done in the "bright " mode dominated by inductive coupling at different pressures and powers. The radial variation of the ion flux in pure chlorine and argon show similar strongly nonuniform profile. As expected, absolute ion flux values in chlorine are substantially decreased compared to pure argon discharge. The spatial nonuniformity across the 16 cm diameter surface of the grounded electrode is in agreement with the Langmuir probe measurements done by Miller and MIT measurements in pure argon. The ion energy distribution functions (IEDs) measured exhibit a complex structure indicative of both light Cl^+ and heavier Cl_2^+ ions. The IEDs in chlorine are much broder than those measured in pure argon plasma. The radial profile of IEDs found in the GEC/ICP chlorine discharge indicate large changes are occuring in the nature of power coupling to the discharge moving center to edge.

  7. 3D-PIC simulation of an inductively coupled ion source

    Science.gov (United States)

    Henrich, Robert; Muehlich, Nina Sarah; Becker, Michael; Heiliger, Christian

    2015-09-01

    Inductively coupled ion sources are applied to a wide range of plasma applications, especially surface modifications. The knowledge of the behavior and precise information of the plasma parameters are of main importance. These values are tedious to measure without influencing the discharge. By applying our fully three-dimensional PlasmaPIC tool we are able to reach these plasma parameters with a spatial and temporal resolution which is quite hard to achieve experimentally. PlasmaPIC is used for modeling discharges in arbitrary geometries without limitations to any symmetry. By this means we are able to demonstrate that the plasma density has an irrotational character. Furthermore, we will show the dependence of the plasma parameters of different working conditions. We will show that for gridded inductively coupled ion sources the neutral gas pressure inside the discharge chamber depends on the extraction of ions. This effect is considered in PlasmaPIC by a self-consistent coupling of the neutral gas simulation and the plasma simulation whereas the neutral gas distribution is calculated using the direct simulation Monte Carlo method (DSMC). This work has been supported by the ``Bundesministerium fuer Wirtschaft und Energie.'' Grant 50RS1507.

  8. Direct solid soil analysis by laser ablation inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Determination of heavy metals in soils by inductively coupled plasma atomic emission spectrometry (ICP-AES) usually involves the time-consuming step of preparing a solution of the solid that is then nebulized into the plasma. According to regulations, digestion by aqua regia(hydrochloric acid + nitric acid, 3 + 1) should be carried out although it is known that this method is incomplete for silicate soils. The problem can be eliminated by introducing the solid directly into the plasma using the laser ablation technique for sampling. Results are described for a study of laser ablation using a Q-switched Nd: YAG laser coupled with a new échelle spectrometer which has a multichannel solid-state detector. The laser pulses were focused onto the solid surface of pressed soil samples to generate an aerosol which is entrained in a flowing Ar stream, transported through a tube and then introduced directly into the inductively coupled plasma. Some characteristics of the preparation technique, the selection of an internal standard and homogeneity tests of the elemental distribution are reported along with a comparison and evaluation of three methods of calibration. The criteria used to measure the performance of laser ablation ICP-AES are the relative standard deviations obtained of 4.9–12.7% and the accuracy, 0.3–12.4% for Fe, Mn, Cu, Pb, Cr, Zn and Ni

  9. Online Coupling of Flow-Field Flow Fractionation and Single Particle Inductively Coupled Plasma-Mass Spectrometry: Characterization of Nanoparticle Surface Coating Thickness and Aggregation State

    Science.gov (United States)

    Surface coating thickness and aggregation state have strong influence on the environmental fate, transport, and toxicity of engineered nanomaterials. In this study, flow-field flow fractionation coupled on-line with single particle inductively coupled plasma-mass spectrometry i...

  10. The Tuned Substrate Self-bias in a Radio-frequency Inductively Coupled Plasma

    Institute of Scientific and Technical Information of China (English)

    丁振峰; 霍伟刚; 王友年

    2004-01-01

    The radio frequency (rf) self-bias of the substrate in a rf inductively coupled plasma is controlled by means of varying the impedance of an external LC network inserted between the substrate and the ground. Experimental studies were done on the relations of the tuned substrate self-bias with varying discharge and external circuit parameters. Under a certain discharge gas pressure, the curves of tuned substrate self-bias Vtsb versus tuning capacitance Ct demonstrate jumps and hysteresises when rf discharge power is higher than a threshold. The hysteresis loop in terms of ACtcrit1 (= Ccrit1 - Ccrit2, here, Ccrit1, Ccrit2 are critical capacitance magnitudes under which the tuned substrate self-bias jumps) decreases with increasing rf discharge power, while the maximum | Vtsbimn | is achieved in the middle discharge-power region. Under a constant discharge power |Vtsb min|, Ctcrit1 and Ctcrit2 achieve their minimums in the middle gas-pressure region.When the tuning capacitance is pre-set at a lower value, Vtsb varies slightly with gas-flow rate;in the case of tuning capacitance sufficiently approaching CtcritX, Vtdb undergoes the jump and hysteresis with the changing gas-flow rate. By inserting a resistor R into the external network,the characteristics of Vtsb - Ct curves are changed with the reduced quality factor Q depending on resistance values. Based on inductive- and capacitive-coupling characteristics of inductively coupled plasma, the dependence of a plasma sheath on plasma parameters, and the impedance properties of the substrate branch, the observed results can be qualitatively interpreted.

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

    International Nuclear Information System (INIS)

    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

  12. EVALUATION OF CORROSION OF ENGINEERING CERAMICS BY ATOMIC EMISSION SPECTROMETRY IN INDUCTIVELY COUPLED PLASMA

    OpenAIRE

    DAGMAR GALUSKOVÁ; DUŠAN GALUSEK; PAVOL ŠAJGALÍK

    2014-01-01

    An analytical method has been developed and verified, facilitating chemical analysis of saline aqueous solutions from corrosion tests of two types of engineering ceramics, i.e. polycrystalline alumina, and silicon nitride. The method is capable of providing complementary information related to mechanisms of corrosion and kinetics of dissolution of the two main components of the ceramics, i.e. Al in α-Al2O3, and Si in Si3N4. A radially viewed inductively coupled plasma atomic emission spectros...

  13. Photon noise limited radiation detection with lens-antenna coupled Microwave Kinetic Inductance Detectors

    CERN Document Server

    Yates, S J C; Endo, A; Janssen, R M J; Ferrari, L; Diener, P; Baryshev, A M

    2011-01-01

    Microwave Kinetic Inductance Detectors (MKIDs) have shown great potential for sub-mm instrumentation because of the high scalability of the technology. Here we demonstrate for the first time in the sub-mm band (0.1...2 mm) a photon noise limited performance of a small antenna coupled MKID detector array and we describe the relation between photon noise and MKID intrinsic generation-recombination noise. Additionally we use the observed photon noise to measure the optical efficiency of detectors to be 0.8+-0.2.

  14. Construction of Larger Area Density-Uniform Plasma with Collisional Inductively Coupled Plasma Cells

    Institute of Scientific and Technical Information of China (English)

    OUYANG Liang; LIU Wandong; BAI Xiaoyan; CHEN Zhipeng; WANG Huihui; LI LUO Chen; JI Liangliang; HU Bei

    2007-01-01

    The plasma density and electron temperature of a multi-source plasma system composed of several collisional inductively coupled plasma (ICP) cells were measured by a double-probe. The discharges of the ICP cells were shown to be independent of each other. Furthermore, the total plasma density at simultaneous multi-cell discharge was observed to be approximately equal to the summation of the plasma density when the cells discharge separately. Based on the linear summation phenomenon, it was shown that a larger area plasma with a uniform density and temperature profile could be constructed with multi-collisional ICP cells.

  15. Surface Modification of Nanometre Silicon Carbide Powder with Polystyrene by Inductively Coupled Plasma

    Institute of Scientific and Technical Information of China (English)

    WEI Gang; MENG Yuedong; ZHONG Shaofeng; LIU Feng; JIANG Zhongqing; SHU Xingsheng; REN Zhaoxing; WANG Xiangke

    2008-01-01

    An investigation was made into polystyrene (PS) grafted onto nanometre sili-con carbide (SIC) particles. In our experiment, the grafting polymerization reaction was in-duced by a radio frequency (RF) inductively coupled plasma (ICP) treatment of the nanome-tre powder. FTIR (Fourier transform infrared spectrum) and XPS (X-ray photoelectron spec-troscopy) results reveal that PS is grafted onto the surface of silicon carbide powder. An analysis is presented on the effectiveness of this approach as a function of plasma operating variables including the plasma treating power, treating time, and grafting reaction temperature and time.

  16. Inductively coupled plasma-atomic emission spectrometry (ICP-AES) in support of nuclear waste management

    International Nuclear Information System (INIS)

    Simulated complex nuclear waste solutions are characterized by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AEC). The system uses and ICP source focused on both a polychromator and a computer-controlled scanning monochromator for intensity measurements. This instrumentation allows for simultaneous and sequential measurements of liquid extraction distribution coefficients needed in the development of process flow sheets for component separations. A large number of elements are determined rapidly with adequate sensitivity and accuracy. The focus of this investigation centers on the analysis of nuclear fission products. 13 references, 13 tables

  17. Hard-Coupled Nonlinear Model of Induction Heating of Nonmagnetic Cylindrical Billets In Rotation

    Czech Academy of Sciences Publication Activity Database

    Karban, P.; Mach, F.; Doležel, Ivo

    Funchal - Madeira: A.P.D.E.E. Associação Portuguesa para a Promoção e Desenvolvimento da Engenharia Electrotécnica, 2011 - (Antunes, C.; Wiak, S.), s. 1-8 ISBN 978-972-8822-24-8. [International Symposium on Electromagnetic Fields in Mechatronics, Electrical and Electronic Engineering, ISEF2011 /15./. Funchal - Madeira (PT), 01.09.2011-03.09.2011] R&D Projects: GA ČR(CZ) GAP102/11/0498 Institutional research plan: CEZ:AV0Z20570509 Keywords : induction heating * hard-coupled model * magnetic field Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering http://www.apdee.org

  18. Hard-Coupled Modeling of Induction Shrink Fit of Gas-Turbine Active Wheel

    Czech Academy of Sciences Publication Activity Database

    Kotlan, V.; Karban, P.; Ulrych, B.; Doležel, Ivo; Kůs, Pavel

    Heidelberg: Springer, 2012 - (Kyamakya, K.; Halang, W.; Mathis, W.; Chedjou, J.; Li, Z.), s. 287-301. (Studies in Computational Intelligence. 459). ISBN 978-3-642-34559-3 R&D Projects: GA ČR(CZ) GAP102/11/0498; GA ČR GA102/09/1305 Institutional research plan: CEZ:AV0Z20570509 Keywords : induction shrink fit * finite element methods of higher order of accuracy * coupled problem Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering http://www.springer.com/series/7092

  19. Effect of neutral gas heating in argon radio frequency inductively coupled plasma

    International Nuclear Information System (INIS)

    Heating of neutral gas in inductively coupled plasma (ICP) is known to result in neutral gas depletion. In this work, this effect is considered in the simulation of the magnetic field distribution of a 13.56 MHz planar coil ICP. Measured electron temperatures and densities at argon pressures of 0.03, 0.07 and 0.2 mbar were used in the simulation whilst neutral gas temperatures were heuristically fitted. The simulated results showed reasonable agreement with the measured magnetic field profile. (author)

  20. Analysis of neodymium oxide for rare earth impurities by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    A procedure for the determination of the rare earths elements in neodymium oxide with purity grade above 99% by inductively coupled plasma optical emission spectrometry is described. Determination limits were 0,005% for the elements Eu, Dy, Gd, Tb, Ho and Y and 0,01% for Sm and La. The precision of the method was evaluated through the relative standard deviation (RSD) for individual rare earth elements. The values lies in the range of 3 -7% for most of them but lanthanum, has shown 13% RSD. (author)

  1. Inductively Coupled Plasma Optical-Emission Spectroscopy Determination of Major and Minor Elements in Vinegar

    Directory of Open Access Journals (Sweden)

    Arzu AKPINAR-BAYIZIT

    2010-12-01

    Full Text Available This study characterizes the mineral content of vinegar samples. The concentrations of Na, K, Ca, Mg and P (major elements as well as Fe, Mn, Sn, Cu, Ni, Zn, Pb and Cd (minor elements were determined in 35 commercial vinegar samples using inductively coupled plasma optical-emission spectrometry (ICP-OES. The elements with the highest concentrations were K, Na, Ca, Mg and P. The concentrations of heavy metals in the vinegar samples, including Cd, Ni, Sn and Pb, were not considered a health risk.

  2. Electron Temperature Control in Inductively Coupled Nitrogen Plasmas by Adding Argon/Helium

    Institute of Scientific and Technical Information of China (English)

    康正德; 蒲以康

    2002-01-01

    A new technique, adding argon or helium into nitrogen plasma, has been used to regulate the electron temperature in an inductively coupled plasma. The electron temperature is determined by analysing the intensity ratio of two nitrogen spectrum lines. The results show that, when the total pressure is 0.7Pa, the electron temperature increases with the increase of the He partial pressure in He/N2 plasma, but the electron temperature decreases with the increase of the Ar partial pressure in Ar/N2 plasma. The regulation effect of electron temperature is weaker in higher pressure N2/He plasma of 2.6Pa.

  3. Characterization of silicon isotropic etch by inductively coupled plasma etcher for microneedle array fabrication

    International Nuclear Information System (INIS)

    This work investigates the isotropic etching properties in inductively coupled plasma (ICP) etcher for microneedle arrays fabrication. The effects of process variables including powers, gas and pressure on needle structure generation are characterized by factorial design of experiment (DOE). The experimental responses of vertical etching depth, lateral etching length, ratio of vertical etching depth to lateral etching length and photoresist etching rate are reported. The relevance of the etching variables is also presented. The obtained etching behaviours for microneedle structure generation will be applied to develop recipes to fabricate microneedles in designed dimensions

  4. Considerations for the installation of an inductively coupled plasma for the analysis of radioactive samples

    International Nuclear Information System (INIS)

    The sensitivity, dynamic range, and sample through-put rate attributes of the inductively coupled plasma (ICP) call for its consideration as the instrument of choice for the multielement analysis of radioactive samples. Based on our experience in handling radioactive materials, considerations are presented concerning safety of the operator, modularity of the ICP-atomic emission spectrometer systems, reduction of the complex actinide spectra, atomization systems, drain and recovery systems, aerosol containment, heat dissipation, radiolysis effects of sample on dry-box environment, and liquid and solid sampling

  5. Surface Modification of Nanometre Silicon Carbide Powder with Polystyrene by Inductively Coupled Plasma

    International Nuclear Information System (INIS)

    An investigation was made into polystyrene (PS) grafted onto nanometre silicon carbide (SiC) particles. In our experiment, the grafting polymerization reaction was induced by a radio frequency (RF) inductively coupled plasma (ICP) treatment of the nanometre powder. FTIR (Fourier transform infrared spectrum) and XPS (X-ray photoelectron spectroscopy) results reveal that PS is grafted onto the surface of silicon carbide powder. An analysis is presented on the effectiveness of this approach as a function of plasma operating variables including the plasma treating power, treating time, and grafting reaction temperature and time.

  6. Surface Modification of Nanometre Silicon Carbide Powder with Polystyrene by Inductively Coupled Plasma

    Science.gov (United States)

    Wei, Gang; Meng, Yuedong; Zhong, Shaofeng; Liu, Feng; Jiang, Zhongqing; Shu, Xingsheng; Ren, Zhaoxing; Wang, Xiangke

    2008-02-01

    An investigation was made into polystyrene (PS) grafted onto nanometre silicon carbide (SiC) particles. In our experiment, the grafting polymerization reaction was induced by a radio frequency (RF) inductively coupled plasma (ICP) treatment of the nanometre powder. FTIR (Fourier transform infrared spectrum) and XPS (X-ray photoelectron spectroscopy) results reveal that PS is grafted onto the surface of silicon carbide powder. An analysis is presented on the effectiveness of this approach as a function of plasma operating variables including the plasma treating power, treating time, and grafting reaction temperature and time.

  7. Concentrations of Th and U in human tissues determined by inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    In about 20 specimens of untreated human soft tissues, Th and U, were analyzed by inductively coupled plasma-mass spectrometry (ICP-MS). The concentration values obtained, particularly in the case of U, tended to be lower than reported ones. In order to investigate the source of the discrepancy, human tissue samples (treated for preservation), which had been analyzed for U in the previous study by fission tracks, were analyzed again by ICP-MS. This demonstrated the difference may be a reflection of the variance between treated and untreated samples. The problems involved in the analysis and the sample treatment are discussed. (author)

  8. Determination of thorium and uranium in total diet samples by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    The Th and U contents in total diet samples were determined by inductively coupled plasma mass spectrometry (ICP-MS). The internal standardization method was adopted to compensate for non-spectral interferences arising from matrix elements in the sample solutions. Concentration levels of the order of pg ml-1 of Th and U in the total diet sample were determined easily and rapidly by using Bi as an internal standard. The mean concentrations and standard deviations of Th and U in the total diet samples were found to be 25 ± 12 and 44 ± 20 ng g-1 of ash, respectively (for n = 62). (author)

  9. Production date determination of uranium-oxide materials by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    The paper describes analytical methods developed for the production date determination of uranium-based nuclear materials by the measurement of 230Th/234U isotope ratio. An improved sample preparation method for the destructive analysis involving extraction chromatographic separation with TEVATM resin was applied prior to the measurement by isotope dilution inductively coupled plasma sector field mass spectrometry (ICP-SFMS). The results obtained were compared with the direct, quasi-non-destructive measurement using laser ablation ICP-SFMS technique for age determination. The advantages and limitations of both methods are discussed

  10. Photon noise limited radiation detection with lens-antenna coupled microwave kinetic inductance detectors

    International Nuclear Information System (INIS)

    Microwave kinetic inductance detectors (MKIDs) have shown great potential for sub-mm instrumentation because of the high scalability of the technology. Here, we demonstrate for the first time in the sub-mm band (0.1-2 mm) a photon noise limited performance of a small antenna coupled MKID detector array and we describe the relation between photon noise and MKID intrinsic generation-recombination noise. Additionally, we use the observed photon noise to measure the optical efficiency of detectors to be 0.8 ± 0.2.

  11. Neptunium determination by inductively coupled plasma mass spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    The determination of neptunium-237 (237Np) traditionally has been performed by alpha spectrometry or neutron activation analysis. These methods are labor intensive and require several days for completion. Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is a possible alternative for 237Np determinations. This paper describes the analytical method developed for samples that have significant levels of uranium present. The lower reporting limits achievable by ICP-MS are competitive with the counting methods, but the real advantage for this laboratory lies in the lower cost and faster turnaround time provided by ICP-MS. (author)

  12. Application of Inductively Coupled Wireless Radio Frequency Probe to Knee Joint in Magnetic Resonance Image

    Directory of Open Access Journals (Sweden)

    Yuki Katayama

    2009-10-01

    Full Text Available An inductively coupled wireless coil for a radio frequency (RF probe has been designed and applied to a human knee joint to improve the signal to noise ratio (SNR in a magnetic resonance image (MRI. A birdcage type of a primary coil and a Helmholtz type of a wireless secondary coil have been manufactured. The coils were applied to a human knee with a 3 T MRI system. SNR was calculated both in the proton density image and in the T2 weighted image of MRI. The experimental results show that the designed coils are effective to increase SNR in the human knee MRI.

  13. Argon metastable state densities in inductively coupled plasma in mixtures of Ar and O2

    International Nuclear Information System (INIS)

    We have measured the densities of 1s5 and 1s3 argon metastables as a function of the abundance of molecular oxygen in an inductively coupled plasma (ICP) in mixtures of Ar and O2. Laser absorption spectroscopy was used to determine the densities of the metastables. It was found that even small abundances of oxygen lead to large increases in metastable density, mostly due to the reduction in the electron number density, since electron-induced quenching determines the metastable density. At abundances higher than 7% to 15% for powers between 50 and 150 W, quenching by oxygen molecules begins to dominate and the metastable density drops again.

  14. Fabrication of lithographically defined optical coupling facets for silicon-on-insulator waveguides by inductively coupled plasma etching

    International Nuclear Information System (INIS)

    We present a technique to lithographically define and fabricate all required optical facets on a silicon-on-insulator photonic integrated circuit by an inductively coupled plasma etch process. This technique offers 1 μm positioning accuracy of the facets at any location within the chip and eliminates the need of polishing. Facet fabrication consists of two separate steps to ensure sidewall verticality and minimize attack on the end surfaces of the waveguides. Protection of the waveguides by a thermally evaporated aluminum layer before the 40-70 μm deep optical facet etching has been proven essential in assuring the facet smoothness and integrity. Both scanning electron microscopy analysis and optical measurement results show that the quality of the facets prepared by this technique is comparable to the conventional facets prepared by polishing

  15. Review of online coupling of sample preparation techniques with liquid chromatography.

    Science.gov (United States)

    Pan, Jialiang; Zhang, Chengjiang; Zhang, Zhuomin; Li, Gongke

    2014-03-01

    Sample preparation is still considered as the bottleneck of the whole analytical procedure, and efforts has been conducted towards the automation, improvement of sensitivity and accuracy, and low comsuption of organic solvents. Development of online sample preparation techniques (SP) coupled with liquid chromatography (LC) is a promising way to achieve these goals, which has attracted great attention. This article reviews the recent advances on the online SP-LC techniques. Various online SP techniques have been described and summarized, including solid-phase-based extraction, liquid-phase-based extraction assisted with membrane, microwave assisted extraction, ultrasonic assisted extraction, accelerated solvent extraction and supercritical fluids extraction. Specially, the coupling approaches of online SP-LC systems and the corresponding interfaces have been discussed and reviewed in detail, such as online injector, autosampler combined with transport unit, desorption chamber and column switching. Typical applications of the online SP-LC techniques have been summarized. Then the problems and expected trends in this field are attempted to be discussed and proposed in order to encourage the further development of online SP-LC techniques. PMID:24560367

  16. On-line concentration sample stacking coupled with water-in-oil microemulsion electrokinetic chromatography.

    Science.gov (United States)

    Huang, Hsi-Ya; Liu, Wan-Ling; Singco, Brenda; Hsieh, Shih-Huan; Shih, Yung-Han

    2011-10-21

    This study describes for the first time, the ability of a normal stacking mode (NSM) on-line concentration step coupled with water-in-oil (W/O) microemulsion electrokinetic chromatography (MEEKC), using six common penicillin antibiotics (oxacillin, penicillin V, penicillin G, nafcillin, ampicillin, and amoxicillin) as test analytes. Optimization of penicillin separation in the conventional W/O MEEKC system demonstrated that change in the type and concentration of the oil phase (1-butanol) and column temperature had a pronounced effect on the separation. With the subsequent development of the NSM coupled with W/O MEEKC, improved separation and detection sensitivities were observed when an organic solvent plug (1-propanol; 1.04 cm) was placed between the W/O microemulsion and the sample solutions. This could be attributed to the solution viscosity difference between the aqueous sample zone and the organic solvent plug causing the penicillin to be stacked in this 1-propanol plug. The optimal NSM W/O MEEKC provided about 12-fold increase in detection sensitivity compared with conventional sample injection (50 mbar, 3 s). Finally, this proposed method was successfully applied in the analyses of several food samples (porcine organs) spiked with penicillin. PMID:21689819

  17. SPECIATION OF SELENIUM(IV) AND SELENIUM(VI) USING COUPLED ION CHROMATOGRAPHY: HYDRIDE GENERATION ATOMIC ABSORPTION SPECTROMETRY

    Science.gov (United States)

    A simple method was developed to speciate inorganic selenium in the microgram per liter range using coupled ion chromatography-hydride generation atomic absorption spectrometry. Because of the differences in toxicity and adsorption behavior, determination of the redox states selenite, Se(IV), and s...

  18. Multivariate analysis of progressive thermal desorption coupled gas chromatography-mass spectrometry.

    Energy Technology Data Exchange (ETDEWEB)

    Van Benthem, Mark Hilary; Mowry, Curtis Dale; Kotula, Paul Gabriel; Borek, Theodore Thaddeus, III

    2010-09-01

    Thermal decomposition of poly dimethyl siloxane compounds, Sylgard{reg_sign} 184 and 186, were examined using thermal desorption coupled gas chromatography-mass spectrometry (TD/GC-MS) and multivariate analysis. This work describes a method of producing multiway data using a stepped thermal desorption. The technique involves sequentially heating a sample of the material of interest with subsequent analysis in a commercial GC/MS system. The decomposition chromatograms were analyzed using multivariate analysis tools including principal component analysis (PCA), factor rotation employing the varimax criterion, and multivariate curve resolution. The results of the analysis show seven components related to offgassing of various fractions of siloxanes that vary as a function of temperature. Thermal desorption coupled with gas chromatography-mass spectrometry (TD/GC-MS) is a powerful analytical technique for analyzing chemical mixtures. It has great potential in numerous analytic areas including materials analysis, sports medicine, in the detection of designer drugs; and biological research for metabolomics. Data analysis is complicated, far from automated and can result in high false positive or false negative rates. We have demonstrated a step-wise TD/GC-MS technique that removes more volatile compounds from a sample before extracting the less volatile compounds. This creates an additional dimension of separation before the GC column, while simultaneously generating three-way data. Sandia's proven multivariate analysis methods, when applied to these data, have several advantages over current commercial options. It also has demonstrated potential for success in finding and enabling identification of trace compounds. Several challenges remain, however, including understanding the sources of noise in the data, outlier detection, improving the data pretreatment and analysis methods, developing a software tool for ease of use by the chemist, and demonstrating our belief

  19. State-space modeling of the radio frequency inductively-coupled plasma generator

    International Nuclear Information System (INIS)

    Computational fluid dynamics models of RF-ICP are useful in understanding the basic transport phenomenon in an ICP torch under a wide variety of operating conditions. However, these models lack the ability to evaluate the effects of the plasma condition on the RF generator. In this paper, simulation of an induction plasma generator has been done using state space modelling by considering inductively coupled plasma as a part of RF network .The time dependent response of the RF-ICP generator circuit to given input excitation has been computed by extracting the circuit's state-space variables and their constraint matrices. MATLAB 7.1 software has been used to solve the state equations. The values of RF coil current, frequency and plasma power has been measured experimentally also at different plate bias voltage. The simulated model is able to predict RF coil current, frequency, plasma power, overall efficiency of the generator. The simulated and measured values are in agreement with each other. This model can prove useful as a design tool for the Induction plasma generator.

  20. State-space modeling of the radio frequency inductively-coupled plasma generator

    Energy Technology Data Exchange (ETDEWEB)

    Dewangan, Rakesh Kumar; Punjabi, Sangeeta B; Mangalvedekar, H A; Lande, B K [Electrical Engineering Department, V J T I, Mumbai-400019 (India); Joshi, N K; Barve, D N, E-mail: ham.vjti@gmail.co [Laser and Plasma Technology Division, BARC, Mumbai-400085 (India)

    2010-02-01

    Computational fluid dynamics models of RF-ICP are useful in understanding the basic transport phenomenon in an ICP torch under a wide variety of operating conditions. However, these models lack the ability to evaluate the effects of the plasma condition on the RF generator. In this paper, simulation of an induction plasma generator has been done using state space modelling by considering inductively coupled plasma as a part of RF network .The time dependent response of the RF-ICP generator circuit to given input excitation has been computed by extracting the circuit's state-space variables and their constraint matrices. MATLAB 7.1 software has been used to solve the state equations. The values of RF coil current, frequency and plasma power has been measured experimentally also at different plate bias voltage. The simulated model is able to predict RF coil current, frequency, plasma power, overall efficiency of the generator. The simulated and measured values are in agreement with each other. This model can prove useful as a design tool for the Induction plasma generator.

  1. On-line coupled high performance liquid chromatography-gas chromatography for the analysis of contamination by mineral oil. Part 1: method of analysis.

    Science.gov (United States)

    Biedermann, Maurus; Grob, Koni

    2012-09-14

    For the analysis of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH), on-line coupled high performance liquid chromatography-gas chromatography-flame ionization detection (HPLC-GC-FID) offers important advantages: it separates MOSH and MOAH in robust manner, enables direct injection of large aliquots of raw extracts (resulting in a low detection limit), avoids contamination of the sample during preparation and is fully automated. This review starts with an overview of the technology, particularly the fundamentals of introducing large volumes of solvent into GC, and their implementation into various transfer techniques. The main part deals with the concepts of MOSH and MOAH analysis, with a thorough discussion of the choices made. It is followed by a description of the method. Finally auxiliary tools are summarized to remove interfering components, enrich the sample in case of a high fat content and obtain additional information about the MOSH and MOAH composition. PMID:22770383

  2. Comparison of standard and reaction cell inductively coupled plasma mass spectrometry in the determination of chromium and selenium species by HPLC-ICP-MS

    International Nuclear Information System (INIS)

    Elemental speciation is becoming a common analytical procedure for geochemical investigations. The various redox species of environmentally relevant metals can have vastly different biogeochemical properties, including sorption, solubility, bioavailability, and toxicity. The use of high performance liquid chromatography (HPLC) coupled to elemental specific detectors, such as inductively coupled plasma mass spectrometry (ICP-MS), has become one of the most important speciation methods employed. This is due to the separation versatility of HPLC and the sensitive and selective detection capabilities of ICP-MS. The current study compares standard mode ICP-MS to recently developed reaction cell (RC) ICP-MS, which has the ability to remove or reduce many common polyatomic interferences that can limit the ability of ICP-MS to quantitate certain analytes in complex matrices. Determination of chromium and selenium redox species is achieved using ion-exchange chromatography with elemental detection by standard and RC-ICP-MS, using various chromium and selenium isotopes. In this study, method performance and detection limits for the various permutations of the method (isotope monitored or ICP-MS detection mode) were found to be comparable and generally less than 1 μg L-1. The method was tested on synthetic laboratory samples, surface water, groundwater, and municipal tap water matrices

  3. Comparison of standard and reaction cell inductively coupled plasma mass spectrometry in the determination of chromium and selenium species by HPLC-ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Bednar, A.J. [U.S. Army Engineer Research and Development Center, Environmental Laboratory, 3909 Halls Ferry Rd., Vicksburg, MS 39180 (United States)], E-mail: Anthony.J.Bednar@erdc.usace.army.mil; Kirgan, R.A.; Jones, W.T. [U.S. Army Engineer Research and Development Center, Environmental Laboratory, 3909 Halls Ferry Rd., Vicksburg, MS 39180 (United States)

    2009-01-19

    Elemental speciation is becoming a common analytical procedure for geochemical investigations. The various redox species of environmentally relevant metals can have vastly different biogeochemical properties, including sorption, solubility, bioavailability, and toxicity. The use of high performance liquid chromatography (HPLC) coupled to elemental specific detectors, such as inductively coupled plasma mass spectrometry (ICP-MS), has become one of the most important speciation methods employed. This is due to the separation versatility of HPLC and the sensitive and selective detection capabilities of ICP-MS. The current study compares standard mode ICP-MS to recently developed reaction cell (RC) ICP-MS, which has the ability to remove or reduce many common polyatomic interferences that can limit the ability of ICP-MS to quantitate certain analytes in complex matrices. Determination of chromium and selenium redox species is achieved using ion-exchange chromatography with elemental detection by standard and RC-ICP-MS, using various chromium and selenium isotopes. In this study, method performance and detection limits for the various permutations of the method (isotope monitored or ICP-MS detection mode) were found to be comparable and generally less than 1 {mu}g L{sup -1}. The method was tested on synthetic laboratory samples, surface water, groundwater, and municipal tap water matrices.

  4. Excellent Silicon Surface Passivation Achieved by Industrial Inductively Coupled Plasma Deposited Hydrogenated Intrinsic Amorphous Silicon Suboxide

    Directory of Open Access Journals (Sweden)

    Jia Ge

    2014-01-01

    Full Text Available We present an alternative method of depositing a high-quality passivation film for heterojunction silicon wafer solar cells, in this paper. The deposition of hydrogenated intrinsic amorphous silicon suboxide is accomplished by decomposing hydrogen, silane, and carbon dioxide in an industrial remote inductively coupled plasma platform. Through the investigation on CO2 partial pressure and process temperature, excellent surface passivation quality and optical properties are achieved. It is found that the hydrogen content in the film is much higher than what is commonly reported in intrinsic amorphous silicon due to oxygen incorporation. The observed slow depletion of hydrogen with increasing temperature greatly enhances its process window as well. The effective lifetime of symmetrically passivated samples under the optimal condition exceeds 4.7 ms on planar n-type Czochralski silicon wafers with a resistivity of 1 Ωcm, which is equivalent to an effective surface recombination velocity of less than 1.7 cms−1 and an implied open-circuit voltage (Voc of 741 mV. A comparison with several high quality passivation schemes for solar cells reveals that the developed inductively coupled plasma deposited films show excellent passivation quality. The excellent optical property and resistance to degradation make it an excellent substitute for industrial heterojunction silicon solar cell production.

  5. Ion flux and ion distribution function measurements in synchronously pulsed inductively coupled plasmas

    Energy Technology Data Exchange (ETDEWEB)

    Brihoum, Melisa; Cunge, Gilles; Darnon, Maxime; Joubert, Olivier [Laboratoire des Technologies de la Microelectronique CNRS, Grenoble Cedex 9, Isere 38054 (France); Gahan, David [Impedans Ltd., Dublin 17 (Ireland); Braithwaite, Nicholas St. J. [Department of Physical Sciences, Open University, Walton Hall, Milton Keynes MK7 6AA (United Kingdom)

    2013-03-15

    Changes in the ion flux and the time-averaged ion distribution functions are reported for pulsed, inductively coupled RF plasmas (ICPs) operated over a range of duty cycles. For helium and argon plasmas, the ion flux increases rapidly after the start of the RF pulse and after about 50 {mu}s reaches the same steady state value as that in continuous ICPs. Therefore, when the plasma is pulsed at 1 kHz, the ion flux during the pulse has a value that is almost independent of the duty cycle. By contrast, in molecular electronegative chlorine/chlorosilane plasmas, the ion flux during the pulse reaches a steady state value that depends strongly on the duty cycle. This is because both the plasma chemistry and the electronegativity depend on the duty cycle. As a result, the ion flux is 15 times smaller in a pulsed 10% duty cycle plasma than in the continuous wave (CW) plasma. The consequence is that for a given synchronous RF biasing of a wafer-chuck, the ion energy is much higher in the pulsed plasma than it is in the CW plasma of chlorine/chlorosilane. Under these conditions, the wafer is bombarded by a low flux of very energetic ions, very much as it would in a low density, capacitively coupled plasma. Therefore, one can extend the operating range of ICPs through synchronous pulsing of the inductive excitation and capacitive chuck-bias, offering new means by which to control plasma etching.

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

    International Nuclear Information System (INIS)

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

  7. Ion flux and ion distribution function measurements in synchronously pulsed inductively coupled plasmas

    International Nuclear Information System (INIS)

    Changes in the ion flux and the time-averaged ion distribution functions are reported for pulsed, inductively coupled RF plasmas (ICPs) operated over a range of duty cycles. For helium and argon plasmas, the ion flux increases rapidly after the start of the RF pulse and after about 50 μs reaches the same steady state value as that in continuous ICPs. Therefore, when the plasma is pulsed at 1 kHz, the ion flux during the pulse has a value that is almost independent of the duty cycle. By contrast, in molecular electronegative chlorine/chlorosilane plasmas, the ion flux during the pulse reaches a steady state value that depends strongly on the duty cycle. This is because both the plasma chemistry and the electronegativity depend on the duty cycle. As a result, the ion flux is 15 times smaller in a pulsed 10% duty cycle plasma than in the continuous wave (CW) plasma. The consequence is that for a given synchronous RF biasing of a wafer-chuck, the ion energy is much higher in the pulsed plasma than it is in the CW plasma of chlorine/chlorosilane. Under these conditions, the wafer is bombarded by a low flux of very energetic ions, very much as it would in a low density, capacitively coupled plasma. Therefore, one can extend the operating range of ICPs through synchronous pulsing of the inductive excitation and capacitive chuck-bias, offering new means by which to control plasma etching.

  8. Lithium Iron Phosphate Powders and Coatings Obtained by Means of Inductively Coupled Thermal Plasma

    Science.gov (United States)

    Major, K.; Veilleux, J.; Brisard, G.

    2016-01-01

    Lithium-ion batteries have high energy efficiency and good cycling life and are considered as one of the best energy storage device for hybrid and/or electrical vehicle. Still, several problems must be solved prior to a broad adoption by the automotive industry: energy density, safety, and costs. To enhance both energy density and safety, the current study aims at depositing binder-free cathode materials using inductively coupled thermal plasma. In a first step, lithium iron phosphate (LiFePO4) powders are synthesized in an inductively coupled thermal plasma reactor and dispersed in a conventional polyvinylidene fluoride (PVDF) binder. Then, binder-free LiFePO4 coatings are directly deposited onto nickel current collectors by solution precursor plasma spraying (SPPS). The morphology, microstructure, and composition of the synthesized LiFePO4 powders and coatings are fully characterized by electronic microscopy, x-ray diffraction, and x-ray photoelectron spectroscopy (XPS). Quantifying Li with XPS requires the substitution of iron with manganese in the SPPS precursors (LiMPO4, where M = Fe or Mn). The plasma-derived cathodes (with and without PVDF binder) are assembled in button cells and tested. Under optimized plasma conditions, cyclic voltammetry shows that the electrochemical reversibility of plasma-derived cathodes is improved over that of conventional sol-gel-derived LiFePO4 cathodes.

  9. Determination of the rare-earth elements in geological materials by inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Lichte, F.E.; Meier, A.L.; Crock, J.G.

    1987-01-01

    A method of analysis of geological materials for the determination of the rare-earth elements using the Inductively coupled plasma mass spectrometric technique (ICP-MS) has been developed. Instrumental parameters and factors affecting analytical results have been first studied and then optimized. Samples are analyzed directly following an acid digestion, without the need for separation or preconcentration with limits of detection of 2-11 ng/g, precision of ?? 2.5% relative standard deviation, and accuracy comparable to inductively coupled plasma emission spectrometry and instrumental neutron activation analysis. A commercially available ICP-MS instrument is used with modifications to the sample introduction system, torch, and sampler orifice to reduce the effects of high salt content of sample solutions prepared from geologic materials. Corrections for isobaric interferences from oxide ions and other diatomic and triatomic ions are made mathematically. Special internal standard procedures are used to compensate for drift in metahmetal oxide ratios and sensitivity. Reference standard values are used to verify the accuracy and utility of the method.

  10. Applications of inductively coupled plasma-mass spectrometry to radionuclide determinations

    International Nuclear Information System (INIS)

    The symposium, Applications of Inductively Coupled-Mass Spectrometry to Radionuclide Determinations, was held in Gatlinburg, Tennessee on 13--14 October 1994. Despite the fact that the United States Department of Energy (DOE) is changing the mission of many facilities from defense-related nuclear materials production to site remediation and monitoring, the need to fully characterize wastes and environmental samples, combined with the need to monitor worker radiation exposure by means of internal dosimetry, continues to increase the demand for radioisotope determinations. Active nuclear facilities in the United States and elsewhere are strongly emphasizing these determinations, and they are concurrently demanding better and faster analysis techniques to assure the quality of the materials that they supply for nuclear energy production and other nuclear technologies. Many alternatives to radiometry are being studied, however, one of the most promising techniques for radionuclide determinations appears to be inductively coupled plasma - mass spectrometry (ICP-MS). The symposium was a continuation of work started by the Plasma Spectroscopy task group of ASTM Subcommittee C26.05 on Nuclear Fuel Cycle Test Methods, but the DOE Office of Transportation, Emergency Management, and Analytical Services (EM-76) was involved in the genesis of the symposium. Papers covered applications in nuclear material production, high-level waste characterization, environmental monitoring and waste management, and internal dosimetry and health protection. Eleven papers have been processed separately for inclusion on the data base

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

    International Nuclear Information System (INIS)

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

  12. Inductively coupled plasma etching of BZN thin films in SF6/Ar plasmas

    Science.gov (United States)

    Wang, Gang; Li, Ping; Zhang, Guojun; Li, Wei; Dai, Liping; Jiang, Jing

    2013-03-01

    Etching mechanisms and characteristics of bismuth zinc niobate (BZN) thin films were investigated in inductively coupled SF6/Ar plasmas. The influences of various etching parameters including the gas flow ratio, process pressure, and ICP power on the etching results were analyzed. It is found that the chemical etching with F radicals was more effective than the physical sputtering etching with Ar ions for the inductively coupled plasma etching of BZN thin films. The mechanism of ion assisted chemical etching of BZN thin films in SF6/Ar plasmas was proposed. A maximum etch rate of approximately 43.15 nm/min for the BZN thin film was obtained at the optimum etching conditions: 3/2 for the SF6/Ar gas flow ratio, 10 mTorr for the process pressure, and 600 W for the ICP power. The surface morphology of the etched BZN thin film was observed, where was smooth and clean and no post-etch residues were remained.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-09-01

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

  14. Trace determination of Pu by LIF in an inductively coupled plasma

    International Nuclear Information System (INIS)

    Inductively Coupled Plasma/Emission Spectrometry (ICP/ES) technique is largely used in the nuclear industry as an elementary analytical technique. Nevertheless, when the sample to analyse presents elements with a lot of emission spectral lines, spectral interferences lead to limited sensitivity. This is the case for Pu determination in presence of large U concentration. In pure aqueous solution, the limit of detection (LOD) for Pu is 10 μg/1. In presence of U, the LOD is determined by a ratio U/Pu = 1000. Pulsed Laser Induced Fluorescence (LIF) spectrometry is known to be a very selective technique when associated with an Inductively Coupled Plasma source. The absolute sensitivity is better by 2 or 3 orders of magnitude; its principle is based on selective excitation of the ionic species in the plasma followed by fluorescence radiation detection of these species; this radiation being practically free from spectral interferences, it is possible to improve the relative LOD. In this presentation, experimental results performed at Cogema/Marcoule laboratory are presented. After the experimental set-up description, first results of LIF are shown: - very good selectivity is effectively obtained, - a series of analytical results obtained with excitation scanning from the visible to the U.V. show that sensitivity of LIF technique is strictly related to the spectroscopic scheme

  15. Inductively coupled plasma-mass spectrometry: an initial assessment of the VG isotopes Plasmaquad

    International Nuclear Information System (INIS)

    The Chemical Analysis Group has been approached by a British Scientific instrument maker regarding the possibility of the group participating in a Department of Trade and Industry sponsored scheme whereby we would have a 12 month period to assess the advantages and disadvantages of a new analytical technique, Inductively Coupled Plasma-Mass Spectrometry. This report details our initial assessment of the instrument, carried out in order to decide whether to participate in the scheme. We have attempted to discover whether the instrument meets the claims made of it in advertising literature, and have attempted to compare the technique with another, proven technique, Inductively Coupled Plasma - Optical Emission Spectroscopy. The Plasmaquad offers excellent sensitivity for almost all of the elements of the periodic table, giving a distinct improvement over the Chemical Analysis Group's present capabilities for many elements. The isotope ratio measuring ability is important, as the Group has no such capability at the moment and a demand for this type of measurement is foreseen. Our conclusions, while inevitably somewhat subjective, form the basis for recommending Harwell to participate in the scheme. (author)

  16. Inductively coupled hydrogen plasma processing of AZO thin films for heterojunction solar cell applications

    International Nuclear Information System (INIS)

    Highlights: • A high-density plasma reactor of inductively coupled plasma source is used in this work. • The conductivity and transmittance can be enhanced simultaneously in the hydrogen process. • The formation of additional donors and passivation due to the hydrogen plasma processing. • The photovoltaic improvement due to the improved AZO layer and hetero-interface quality in the solar cells. - Abstract: Al-doped ZnO (AZO) thin films deposited by means of RF magnetron sputtering were processed in a low frequency inductively coupled plasma of H2, aiming at heterojunction (HJ) solar cell applications. A variety of characterization results show that the hydrogen plasma processing exerts a significant influence on the microstructures, electrical and optical properties of the AZO films. The incorporation of hydrogen under the optimum treatment simultaneously promoted the transmittance and conductivity due to the hydrogen associated passivation effect on the native defects and the formation of shallow donors in the films, respectively. A p-type c-Si based HJ solar cell with a front AZO contact was also treated in as-generated non-equilibrium hydrogen plasma and the photovoltaic performance of the solar cell was prominently improved. The underlying mechanism was discussed in terms of the beneficial impacts of high-density hydrogen plasma on the properties of AZO itself and the hetero-interfaces involved in the HJ structure (interface defect and energy band configuration)

  17. Inductively coupled hydrogen plasma processing of AZO thin films for heterojunction solar cell applications

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, H.P. [State Key Laboratory of Electronic Thin Films and Integrated Devices, School of Energy Science and Engineering, University of Electronic Science and Technology of China, 2006 Xiyuan Ave, West High-Tech Zone, Chengdu, Sichuan 611731 (China); Plasma Sources and Application Center, NIE, and Institute of Advanced Studies, Nanyang Technological University, 637616 Singapore (Singapore); Xu, S., E-mail: shuyan.xu@nie.edu.sg [Plasma Sources and Application Center, NIE, and Institute of Advanced Studies, Nanyang Technological University, 637616 Singapore (Singapore); Zhao, Z. [School of Microelectronics and Solid-state electronics, University of Electronic Science and Technology of China, No.4, Section 2, North Jianshe Rd, Chengdu 610054 (China); Xiang, Y., E-mail: Xiang@uestc.edu.cn [State Key Laboratory of Electronic Thin Films and Integrated Devices, School of Energy Science and Engineering, University of Electronic Science and Technology of China, 2006 Xiyuan Ave, West High-Tech Zone, Chengdu, Sichuan 611731 (China); Institute of Electronic and Information Engineering in Dongguan,UESTC, Dongguan 523808, Guangdong (China)

    2014-10-15

    Highlights: • A high-density plasma reactor of inductively coupled plasma source is used in this work. • The conductivity and transmittance can be enhanced simultaneously in the hydrogen process. • The formation of additional donors and passivation due to the hydrogen plasma processing. • The photovoltaic improvement due to the improved AZO layer and hetero-interface quality in the solar cells. - Abstract: Al-doped ZnO (AZO) thin films deposited by means of RF magnetron sputtering were processed in a low frequency inductively coupled plasma of H{sub 2}, aiming at heterojunction (HJ) solar cell applications. A variety of characterization results show that the hydrogen plasma processing exerts a significant influence on the microstructures, electrical and optical properties of the AZO films. The incorporation of hydrogen under the optimum treatment simultaneously promoted the transmittance and conductivity due to the hydrogen associated passivation effect on the native defects and the formation of shallow donors in the films, respectively. A p-type c-Si based HJ solar cell with a front AZO contact was also treated in as-generated non-equilibrium hydrogen plasma and the photovoltaic performance of the solar cell was prominently improved. The underlying mechanism was discussed in terms of the beneficial impacts of high-density hydrogen plasma on the properties of AZO itself and the hetero-interfaces involved in the HJ structure (interface defect and energy band configuration)

  18. Determination of cadmium and zinc isotope ratios in sheep's blood and organ tissue by electrothermal vaporization inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    A method is described for the determination of Cd and Zn isotope ratios in sheep's blood and organ tissue. Samples were digested with nitric acid using a microwave oven. Cadmium and Zn were separated from matrix components using adsorption chromatography prior to isotope ratio measurement by electrothermal vaporization inductively coupled plasma mass spectrometry. A concentration factor of 35 was achieved. Limits of detection for the determination of Cd and Zn in blood were 0.34 and 0.40 pg g-1, respectively. Cadmium isotope ratios (111Cd: 106Cd; 111Cd: 110Cd) were determined with a precision of 2-3% for both peak height and area count measurements. Zinc isotope ratios (68Zn: 67Zn; 68Zn: 66Zn) were determined with a precision of 2% for peak height measurements and 1% for peak area count measurements. (Author)

  19. Biomonitoring of hair samples by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS)

    Science.gov (United States)

    Sela, H.; Karpas, Z.; Zoriy, M.; Pickhardt, C.; Becker, J. S.

    2007-03-01

    An analytical method for determining essential elements (Zn, Fe and Cu) and toxic elements (Cr, Pb and U) on single hair strands by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-SFMS) using a double focusing sector field mass spectrometer was developed. Results obtained directly using LA-ICP-SFMS of hair were compared with those measured by inductively coupled plasma quadrupole mass spectrometry (ICP-QMS) of solutions of digested hair samples and the analytical methods were found to agree well. Different quantification strategies for trace element determination in hair samples such as external calibration, standard addition and isotope dilution were compared and demonstrated for uranium. For uranium determination in powdered hair by LA-ICP-MS solution-based calibration was applied by coupling the laser ablation chamber to an ultrasonic nebulizer. The significance of single hair analysis by LA-ICP-SFMS was demonstrated by a case study of a person who changed living environment. Differences in the uranium content observed along the single hair strand correlated with the changes in the level of uranium in drinking water. The uranium concentration in a single hair decreased from 212 to 18 ng g-1 with a change in the uranium concentration in drinking water from 2000 to 30 ng l-1. In addition, measurements of uranium isotope ratios showed a natural isotopic composition throughout the whole period in the drinking water, as well as in the hair samples. This paper demonstrates the potential use of laser ablation ICP-MS to provide measurements on a single hair strand and its potential to become a very powerful tool in hair analysis for biological monitoring.

  20. Determination of Vitamin C (Ascorbic Acid Using High Performance Liquid Chromatography Coupled with Electrochemical Detection

    Directory of Open Access Journals (Sweden)

    Ondrej Zitka

    2008-11-01

    Full Text Available Vitamin C (ascorbic acid, ascorbate, AA is a water soluble organic compound that participates in many biological processes. The main aim of this paper was to utilize two electrochemical detectors (amperometric – Coulouchem III and coulometric – CoulArray coupled with flow injection analysis for the detection of ascorbic acid. Primarily, we optimized the experimental conditions. The optimized conditions were as follows: detector potential 100 mV, temperature 25 °C, mobile phase 0.09% TFA:ACN, 3:97 (v/v and flow rate 0.13 mL·min-1. The tangents of the calibration curves were 0.3788 for the coulometric method and 0.0136 for the amperometric one. The tangent of the calibration curve measured by the coulometric detector was almost 30 times higher than the tangent measured by the amperometric detector. Consequently, we coupled a CoulArray electrochemical detector with high performance liquid chromatography and estimated the detection limit for AA as 90 nM (450 fmol per 5 μL injection. The method was used for the determination of vitamin C in a pharmaceutical preparations (98 ± 2 mg per tablet, in oranges (Citrus aurantium (varied from 30 to 56 mg/100 g fresh weight, in apples (Malus sp. (varied from 11 to 19 mg/100 g fresh weight, and in human blood serum (varied from 38 to 78 μM. The recoveries were also determined.

  1. Headspace in-tube microextraction coupled with micellar electrokinetic chromatography of neutral aromatic compounds.

    Science.gov (United States)

    Cho, Sung Min; Park, Bum Su; Jung, Woo Sung; Lee, Sang Won; Jung, Yunhwan; Chung, Doo Soo

    2016-02-01

    Headspace (HS) extraction can be carried out easily and aptly via single drop microextraction coupled with capillary electrophoresis (CE). However, one drawback is the difficulty of keeping the single drop stably at the capillary tip. To solve this problem, we have recently demonstrated HS in-tube microextraction (ITME) of acidic compounds such as chlrophenols in an acidic sample using a basic run buffer plug in the separation capillary for CE as an acceptor phase. In this report, an organic acceptor plug in a capillary was used to extract neutral organic volatile pollutants such as BTEX (benzene, toluene, ethylbenzene, and m-xylene). After extraction, the analytes enriched in the organic acceptor plug were analyzed with micellar electrokinetic chromatography (MEKC). The enrichment factors for BTEX in a standard solution were up to 350 under an optimal condition of 25°C for 20 min. As an application, BTEX spiked into bottled water were analyzed with HS-ITME-MEKC, and the enrichment factors for BTEX were up to 320. The limits of detections were 1-4 ppb, which are at least 200 times lower than the US Environmental Protection Agency guidelines for drinking water, except benzene. The entire procedure of HS-ITME-MEKC was carried out automatically using a commercial CE instrument. PMID:26653509

  2. Direct coupling of packed column supercritical fluid chromatography to continuous corona discharge ion mobility spectrometry.

    Science.gov (United States)

    Rahmanian, A; Ghaziaskar, H S; Khayamian, T

    2013-01-11

    In this study, packed column supercritical fluid chromatography (SFC) was directly coupled to a continuous corona discharge (CD) ion mobility spectrometer (IMS) with several modifications. The main advantage of the developed detector is its capability to introduce full column effluent up to 2000 mL min(-1) CO(2) gas directly into the IMS cell relative to 40 mL min(-1) CO(2) gas as a maximum tolerance, reported for the previous IMS detectors. This achievement was made possible because of using corona discharge instead of (63)Ni as an ionization source and locating the inlet and outlet of the CO(2) gas in the counter electrode of the CD in opposite direction. In addition, a heated interface was placed between back pressure regulator (BPR) and the IMS cell to heat the output of the BPR for introducing sample as the gas phase into the IMS cell. Furthermore, a make-up methanol flow was introduced between the column outlet and BPR to provide a more uniform flow through the BPR and also to prevent freezing and deposition of the analytes in the BPR. The performance of the SFC-CD-IMS was evaluated by analysis of testosterone, medroxyprogesterone, caffeine, and theophylline as test compounds and figures of merit for these compounds have been calculated. PMID:23261285

  3. Application of a particle separation device to reduce inductively coupled plasma-enhanced elemental fractionation in laser ablation-inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    The particle size distribution of laser ablation aerosols are a function of the wavelength, the energy density and the pulse duration of the laser, as well as the sample matrix and the gas environment. Further the size of the particles affects the vaporization and ionization efficiency in the inductively coupled plasma (ICP). Some matrices produce large particles, which are not completely vaporized and ionized in the ICP. The previous work has shown that analytical results such as matrix-independent calibration, accuracy and precision can be significantly influenced by the particle sizes of the particles. To minimize the particle size related incomplete conversion of the sample to ions in the ICP a particle separation device was developed, which allows effective particle separation using centrifugal forces in a thin coiled tube. In this device, the particle cut-off size is varied by changing the number of turns in the coil, as well as by changing the gas flow and the tube diameter. The interaction of the laser with the different samples leads to varying particle size distributions. When carrying out quantitative analysis with non-matrix matched calibration reference materials, it was shown that different particle cut-off sizes were required depending on the ICP conditions and the instrument used for analysis. Various sample materials were investigated in this study to demonstrate the applicability of the device. For silicate matrices, the capability of the ICP to produce ions was significantly reduced for particles larger than 0.5 μm, and was dependent on the element monitored. To reduce memory effects caused by the separated particles, a washout procedure was developed, which additionally allowed the analysis of the trapped particles. These results clearly demonstrate the very important particle size dependent ICP-MS signal response and the potential of the described particle size based separator for the reduction of ICP induced elemental fractionation

  4. Coupling an induction motor type generator to ac power lines. [making windmill generators compatible with public power lines

    Science.gov (United States)

    Nola, F. J. (Inventor)

    1984-01-01

    A system for coupling an induction motor type generator to an A.C. power line includes an electronic switch means that is controlled by a control system and is regulated to turn on at a relatively late point in each half cycle of its operation. The energizing power supplied by the line to the induction motor type generator is decreased and the net power delivered to the line is increased.

  5. Multi-element analysis of Macedonian wines by inductively coupled plasma–mass spectrometry (ICP–MS) and inductively coupled plasma–optical emission spectrometry (IP–OES) for regional classification

    OpenAIRE

    Ivanova, Violeta; Wiltsche, Helmar; Stafilov, Trajče; Stefova, Marina; Motter, Herber; Lankmayr, Ernst

    2013-01-01

    Major, minor, and trace elements in wines from the Republic of Macedonia were determined in this study. Both inductively coupled plasma–mass spectrometry (ICP-MS) and inductively coupled plasma– optical emission spectrometry (ICP-OES) were used for accurate determination of the concentration of 42 elements (Ag, Al, Au, B, Ba, Be, Bi, Ca, Cd, Ce, Co, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Ho, La, Lu, Mg, Mn, Mo, Na, Nd, Ni, P, Pb, Pr, S, Sm, Tb, Ti, Tl, Tm, U, V, Yb, Zn, Zr) in 25 Macedonian white, r...

  6. Metabolite Profile of Salidroside in Rats by Ultraperformance Liquid Chromatography Coupled with Quadrupole Time-of-Flight Mass Spectrometry and High-Performance Liquid Chromatography Coupled with Quadrupole-Linear Ion Trap Mass Spectrometry.

    Science.gov (United States)

    Hu, Zhiwei; Wang, Ziming; Liu, Yong; Wu, Yan; Han, Xuejiao; Zheng, Jian; Yan, Xiufeng; Wang, Yang

    2015-10-21

    In the present work, the salidroside metabolite profile in rat urine was investigated, and subsequently the metabolic pathways of salidroside were proposed. After administrations of salidroside at an oral dose of 100 or 500 mg/kg, rat urine samples were collected and pretreated with methanol to precipitate the proteins. The pretreated samples were analyzed by an Acquity ultraperformance liquid chromatography (UPLC) coupled with an HSS T3 column and detected by quadrupole time-of-flight mass spectrometry (Q-TOF-MS) or high-performance liquid chromatography coupled with hybrid triple-quadrupole linear ion trap mass spectrometry (HPLC/Q-trap-MS). A total of eight metabolites were detected and identified on the basis of the characteristics of their protonated ions in the urine samples. The results elucidated that salidroside was metabolized via glucuronidation, sulfation, deglycosylation, hydroxylation, methylation, and dehydroxylation pathways in vivo. PMID:26461036

  7. Liquid chromatography-mass spectrometry coupling by the intermediary of a liquid micro chromatography-electro spray interface; Couplage chromatographie liquide-spectrometrie de masse par l`intermediaire d`une interface electrospray-microchromatographie liquide

    Energy Technology Data Exchange (ETDEWEB)

    Gillard Factor, C.

    1996-12-06

    The objective of this work is to realize a liquid chromatography- mass spectrometry coupling by the intermediary of an electro spray interface and the evaluation of performances of tis analytical tool to study pollutants in water, and more particularly pesticides whom maximum admissible concentration in a table water is 0.1{mu}g/l. This study has allowed to bring to the fore the interest of the ionization mode by electro spray in a LC/MS coupling to identify and quantify pesticides in the state of traces without treating the sample. Then, it was demonstrated the usefulness of this analytical tool to detect high molecular masses molecules. (N.C.)

  8. Sulfur analysis by inductively coupled plasma-mass spectrometry: A review

    Energy Technology Data Exchange (ETDEWEB)

    Giner Martínez-Sierra, J.; Galilea San Blas, O.; Marchante Gayón, J.M.; García Alonso, J.I., E-mail: jiga@uniovi.es

    2015-06-01

    In recent years the number of applications of sulfur (S) analysis using inductively coupled plasma mass spectrometry (ICP-MS) as detector has increased significantly. In this article we describe in some depth the application of ICP-MS for S analysis with emphasis placed on the sulfur-specific detection by hyphenated techniques such as LC, GC, CE and LA coupled on-line to ICP-MS. The different approaches available for sulfur isotope ratio measurements by ICP-MS are also detailed. Particular attention has been paid to the quantification of peptides/proteins and the analysis of metallopeptides/metalloproteins via sulfur by LC–ICP-MS. Likewise, the speciation analysis of metal-based pharmaceuticals and metallodrugs and non-metal selective detection of pharmaceuticals via S are highlighted. Labeling procedures for metabolic applications are also included. Finally, the measurement of natural variations in S isotope composition with multicollector ICP-MS instruments is also covered in this review. - Highlights: • Emphasis placed on the sulfur-specific detection by chromatographic techniques coupled on-line to ICP-MS. • Different instrumental approaches available for sulfur measurements by ICP-MS. • Quantification of proteins and the analysis of metalloproteins via sulfur by LC-ICP-MS. • Labelling procedures for metabolic applications are also included. • The measurement of natural variations in S isotope composition with multicollector ICP-MS.

  9. Sulfur analysis by inductively coupled plasma-mass spectrometry: A review

    International Nuclear Information System (INIS)

    In recent years the number of applications of sulfur (S) analysis using inductively coupled plasma mass spectrometry (ICP-MS) as detector has increased significantly. In this article we describe in some depth the application of ICP-MS for S analysis with emphasis placed on the sulfur-specific detection by hyphenated techniques such as LC, GC, CE and LA coupled on-line to ICP-MS. The different approaches available for sulfur isotope ratio measurements by ICP-MS are also detailed. Particular attention has been paid to the quantification of peptides/proteins and the analysis of metallopeptides/metalloproteins via sulfur by LC–ICP-MS. Likewise, the speciation analysis of metal-based pharmaceuticals and metallodrugs and non-metal selective detection of pharmaceuticals via S are highlighted. Labeling procedures for metabolic applications are also included. Finally, the measurement of natural variations in S isotope composition with multicollector ICP-MS instruments is also covered in this review. - Highlights: • Emphasis placed on the sulfur-specific detection by chromatographic techniques coupled on-line to ICP-MS. • Different instrumental approaches available for sulfur measurements by ICP-MS. • Quantification of proteins and the analysis of metalloproteins via sulfur by LC-ICP-MS. • Labelling procedures for metabolic applications are also included. • The measurement of natural variations in S isotope composition with multicollector ICP-MS

  10. Developments and trends in inductively coupled plasma mass spectrometry and its influence on the recent advances in trace element analysis

    International Nuclear Information System (INIS)

    A brief introduction to the various instrumental methods such as atomic absorption spectrometry, x-ray fluorescence spectrometry, neutron activation analysis, inductively coupled plasma atomic emission spectrometry, thermal ionization mass spectrometry, etc. are presented highlighting their relative merits and demerits. The history and developments of inductively coupled plasma mass spectrometry (ICP-MS) and its advantages and limitations over other multi-element instrumental techniques are reviewed. Extended capabilities by hyphenating ICP-MS to various other well-known sample introduction techniques such as flow-injection, electrothermal vaporization, chromatographic methods and laser ablation are discussed in brief. The recent development of high resolution multi-collector double-focusing magnetic mass spectrometer with inductively coupled plasma at atmospheric pressure as source is also discussed. Some of the areas where more developments can be expected in future are suggested. (author). 77 refs., 4 tabs., 3 figs

  11. Temperature-programmed high-performance liquid chromatography coupled to isotope ratio mass spectrometry.

    Science.gov (United States)

    Godin, Jean-Philippe; Hopfgartner, Gérard; Fay, Laurent

    2008-09-15

    The utility of liquid chromatography coupled to the isotope ratio mass spectrometry technique (LC-IRMS) has already been established through a variety of successful applications. However, the analytical constraint related to the use of aqueous mobile phases limits the LC separation mechanism. We report here a new strategy for high-precision (13)C isotopic analyses based on temperature-programmed LC-IRMS using aqueous mobile phases. Under these conditions, the isotopic precision and accuracy were studied. On one hand, experiments were carried out with phenolic acids using isothermal LC conditions at high temperature (170 degrees C); on the other hand, several experiments were performed by ramping the temperature, as conventionally used in a gas chromatography-based method with hydrosoluble fatty acids and pulses of CO 2 reference gas. In isothermal conditions at 170 degrees C, despite the increase of the CO 2 background, p-coumaric acid and its glucuronide conjugate gave reliable isotopic ratios compared to flow injection analysis-isotopic ratio mass spectrometry (FIA-IRMS) analyses (isotopic precision and accuracy are lower than 0.3 per thousand). On the opposite, for its sulfate conjugate, the isotopic accuracy is affected by its coelution with p-coumaric acid. Not surprisingly, this study also demonstrates that at high temperature (170 degrees C), a compound eluting with long residence time (i.e., ferulic acid) is degraded, affecting thus the delta (13)C (drift of 3 per thousand) and the peak area (compared to FIA-IRMS analysis at room temperature). Quantitation is also reported in isothermal conditions for p-coumaric acid in the range of 10-400 ng/mL and with benzoic acid as an internal standard. For temperature gradient LC-IRMS, in the area of the LC gradient (set up at 20 degrees C/min), the drift of the background observed produces a nonlinearity of SD (delta (13)C) approximately 0.01 per thousand/mV. To circumvent this drift, which impacts severely the

  12. Analytical Model and Optimized Design of Power Transmitting Coil for Inductively Coupled Endoscope Robot.

    Science.gov (United States)

    Ke, Quan; Luo, Weijie; Yan, Guozheng; Yang, Kai

    2016-04-01

    A wireless power transfer system based on the weakly inductive coupling makes it possible to provide the endoscope microrobot (EMR) with infinite power. To facilitate the patients' inspection with the EMR system, the diameter of the transmitting coil is enlarged to 69 cm. Due to the large transmitting range, a high quality factor of the Litz-wire transmitting coil is a necessity to ensure the intensity of magnetic field generated efficiently. Thus, this paper builds an analytical model of the transmitting coil, and then, optimizes the parameters of the coil by enlarging the quality factor. The lumped model of the transmitting coil includes three parameters: ac resistance, self-inductance, and stray capacitance. Based on the exact two-dimension solution, the accurate analytical expression of ac resistance is derived. Several transmitting coils of different specifications are utilized to verify this analytical expression, being in good agreements with the measured results except the coils with a large number of strands. Then, the quality factor of transmitting coils can be well predicted with the available analytical expressions of self- inductance and stray capacitance. Owing to the exact estimation of quality factor, the appropriate coil turns of the transmitting coil is set to 18-40 within the restrictions of transmitting circuit and human tissue issues. To supply enough energy for the next generation of the EMR equipped with a Ø9.5×10.1 mm receiving coil, the coil turns of the transmitting coil is optimally set to 28, which can transfer a maximum power of 750 mW with the remarkable delivering efficiency of 3.55%. PMID:26292335

  13. Quality assessment of traditional Chinese medicine herb couple by high-performance liquid chromatography and mass spectrometry combined with chemometrics.

    Science.gov (United States)

    Cheng, Tao-Fang; Jia, Yu-Ran; Zuo, Zheng; Dong, Xin; Zhou, Ping; Li, Ping; Li, Fei

    2016-04-01

    This study was designed to develop a simple, specific and reliable method to overall analyze the chemical constituents in clematidis radix et rhizome/notopterygii rhizome et radix herb couple using high-performance liquid chromatography coupled with tandem mass spectrometry and multiple chemometric analysis. First, the separation and qualitative analysis of herb couple was achieved on an Agilent Zorbax Eclipse Plus C18 column (250 mm × 4.6 mm, 5 μm), and 69 compounds were unambiguously or tentatively identified. Moreover, in quantitative analysis, eight ingredients including six coumarins and two triterpenoid sapogenins were quantified by high-performance liquid chromatography coupled with tandem mass spectrometry. In terms of good linearity (r(2) ≥ 0.9995) with a relatively wide concentration range, recovery (85.40-102.50%) and repeatability (0.99-4.45%), the validation results suggested the proposed method was reliable, and successfully used to analyze ten batches of herb couple samples. Then, hierarchical cluster analysis and principal component analysis were used to classify samples and search significant ingredients. The results showed that ten batches of herb couple samples were classified into three groups, and six compounds were found for its better quality control. PMID:26834048

  14. Bulk plasma fragmentation in a C4F8 inductively coupled plasma: A hybrid modeling study

    International Nuclear Information System (INIS)

    A hybrid model is used to investigate the fragmentation of C4F8 inductive discharges. Indeed, the resulting reactive species are crucial for the optimization of the Si-based etching process, since they determine the mechanisms of fluorination, polymerization, and sputtering. In this paper, we present the dissociation degree, the density ratio of F vs. CxFy (i.e., fluorocarbon (fc) neutrals), the neutral vs. positive ion density ratio, details on the neutral and ion components, and fractions of various fc neutrals (or ions) in the total fc neutral (or ion) density in a C4F8 inductively coupled plasma source, as well as the effect of pressure and power on these results. To analyze the fragmentation behavior, the electron density and temperature and electron energy probability function (EEPF) are investigated. Moreover, the main electron-impact generation sources for all considered neutrals and ions are determined from the complicated C4F8 reaction set used in the model. The C4F8 plasma fragmentation is explained, taking into account many factors, such as the EEPF characteristics, the dominance of primary and secondary processes, and the thresholds of dissociation and ionization. The simulation results are compared with experiments from literature, and reasonable agreement is obtained. Some discrepancies are observed, which can probably be attributed to the simplified polymer surface kinetics assumed in the model

  15. Characterization of stationary and pulsed inductively coupled RF discharges for plasma sterilization

    International Nuclear Information System (INIS)

    Sterilization of bio-medical materials using radio frequency (RF) excited inductively coupled plasmas (ICPs) has been investigated. A double ICP has been developed and studied for homogenous treatment of three-dimensional objects. Sterilization is achieved through a combination of ultraviolet light, ion bombardment and radical treatment. For temperature sensitive materials, the process temperature is a crucial parameter. Pulsing of the plasma reduces the time average heat strain and also provides additional control of the various sterilization mechanisms. Certain aspects of pulsed plasmas are, however, not yet fully understood. Phase resolved optical emission spectroscopy and time resolved ion energy analysis illustrate that a pulsed ICP ignites capacitively before reaching a stable inductive mode. Time resolved investigations of the post-discharge, after switching off the RF power, show that the plasma boundary sheath in front of a substrate does not fully collapse for the case of hydrogen discharges. This is explained by electron heating through super-elastic collisions with vibrationally excited hydrogen molecules

  16. Characterization of stationary and pulsed inductively coupled RF discharges for plasma sterilization

    Science.gov (United States)

    Gans, T.; Osiac, M.; O'Connell, D.; Kadetov, V. A.; Czarnetzki, U.; Schwarz-Selinger, T.; Halfmann, H.; Awakowicz, P.

    2005-05-01

    Sterilization of bio-medical materials using radio frequency (RF) excited inductively coupled plasmas (ICPs) has been investigated. A double ICP has been developed and studied for homogenous treatment of three-dimensional objects. Sterilization is achieved through a combination of ultraviolet light, ion bombardment and radical treatment. For temperature sensitive materials, the process temperature is a crucial parameter. Pulsing of the plasma reduces the time average heat strain and also provides additional control of the various sterilization mechanisms. Certain aspects of pulsed plasmas are, however, not yet fully understood. Phase resolved optical emission spectroscopy and time resolved ion energy analysis illustrate that a pulsed ICP ignites capacitively before reaching a stable inductive mode. Time resolved investigations of the post-discharge, after switching off the RF power, show that the plasma boundary sheath in front of a substrate does not fully collapse for the case of hydrogen discharges. This is explained by electron heating through super-elastic collisions with vibrationally excited hydrogen molecules.

  17. Spectroanalytical investigations on inductively coupled N2/Ar and Ar/Ar high frequency plasmas

    International Nuclear Information System (INIS)

    In order to improve the detection limits of trace elements in corrosion products of metallic materials, the inductively coupled plasma excitation source (ICP) was applied for spectroscopic analysis. Besides optimizing the working conditions for the mentioned materials, the fundamental research clearing the excitation processes in ICP was carried out. Basicly, two plasma systems were investigated: the nitrogen cooled N2/Ar- and pure Ar/Ar-plasma. The computed detection limits for 8 chosen elements are between 0.1 and 50 μg ml-1 in both plasmas. The advantage of ion lines was clearly present; in N2/Ar-plasma it was larger than in Ar/Ar-plasma. The excitation temperatures measured with help of ArI, FeI and ZnI lines rise with increasing power and decreasing distance from the induction coil. The distribution of Zn excitation temperature in N2/Ar-plasma as well as the measured N+2 rotational and CN vibrational temperatures indicate, that the toroidal structure of Ar/Ar-plasma is not analogue to the N2/Ar-plasma. The values of the various excitation temperatures (Ar, Fe, Zn) and the differences between the excitation, vibration, rotation and ionization temperatures (Tsub(i) > Tsub(n) = Tsub(vib) > Tsub(rot)) indicate an absence of thermal equilibrium in the concerned system. (orig.)

  18. Numerical Study of a System of Long Josephson Junctions with Inductive and Capacitive Couplings

    Science.gov (United States)

    Rahmonov, I. R.; Shukrinov, Yu. M.; Plecenik, A.; Zemlyanaya, E. V.; Bashashin, M. V.

    2016-02-01

    The phase dynamics of the stacked long Josephson junctions is investigated taking into account the inductive and capacitive couplings between junctions and the diffusion current. The simulation of the current-voltage characteristics is based on the numerical solution of a system of nonlinear partial differential equations by a fourth order Runge-Kutta method and finite-difference approximation. A parallel implementation is based on the MPI technique. The effectiveness of the MPI/C++ code is confirmed by calculations on the multi-processor cluster CICC (LIT JINR, Dubna). We demonstrate the appearance of the charge traveling wave (CTW) at the boundary of the zero field step. Based on this fact, we conclude that the CTW and the fluxons coexist.

  19. Three-dimensional discharge simulation of inductively coupled plasma (ICP) etching reactor

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    More and more importance has been attached to inductively coupled plasma (ICP) in semiconductor manufacture. For a deep understanding of the plasma discharge process in the etching reactor, this study made a three-dimensional simulation on the Ar plasma discharge process with the commercial software CFD-ACE, which is according to the real experiment conditions and data supplied by North Microelec-tronic Corporation. The error of the simulation results is in the range of ±20% with credibility. The numerical results show that the three-dimentional spatial distribu-tion of electron density is reduced from the chamber center to the wall. The distri-bution of electron density, electron temperature and power deposition is related to the shape and placement of the coil.

  20. Nonlinear electromagnetic fields in 0.5 MHz inductively coupled plasmas

    DEFF Research Database (Denmark)

    Ostrikov, K.N.; Tsakadze, E.L.; Xu, S.;

    2003-01-01

    the fundamental frequency harmonics only. After transition to higher-power (similar to1130 W) H-mode, the second-harmonic nonlinear azimuthal magnetic field B-phi(2omega) that is in 4-6 times larger than the fundamental frequency component B-phi(omega), has been observed. A simplified plasma fluid......Radial profiles of magnetic fields in the electrostatic (E) and electromagnetic (H) modes of low-frequency (similar to500 kHz) inductively coupled plasmas have been measured using miniature magnetic probes. In the low-power (similar to170 W) E-mode, the magnetic field pattern is purely linear, with...... model explaining the generation of the second harmonics of the azimuthal magnetic field in the plasma source is proposed. The nonlinear second harmonic poloidal (r-z) rf current generating the azimuthal magnetic field B-phi(2omega) is attributed to nonlinear interactions between the fundamental...

  1. Heat Transfer During Radio Frequency Inductively Coupled Plasma Deposition of Tungsten

    Institute of Scientific and Technical Information of China (English)

    JIANG Xianliang; M.I.BOULOS

    2007-01-01

    Particle melting and substrate temperature are important in controlling deposited density and residual stress in thermal plasma deposition of refractory materials.In this paper,both the heating and cooling behaviours of tungsten particles inside a radio frequency inductively coupled plasma(ICP)and the plasma heat flux to the substrate were investigated.The distribution of the plasma-generated heat on device,powder injection probe,deposition chamber,and substrate Was determined by measuring the water flow rate and the flow-in and flow-out water temperatures in the four parts.Substrate temperature Was measured by a two-colour pyrometer during the ICP deposition of tungsten.Experimental results show that the heat flux to the substrate accounts for about 20% of the total plasma energy,the substrate temperature can reach as high as 2100 K,and the heat loss by radiation is significant in the plasma deposition of tungsten.

  2. Isotope ratio determinations by inductively coupled plasma/mass spectrometry for zinc bioavailability studies

    International Nuclear Information System (INIS)

    A method is described for the measurement of 67Zn/68Zn and 70Zn/68Zn ratios by inductively coupled plasma/mass spectrometry with ultrasonic nebulization. The method provides sufficient accuracy and precision for zinc bioavailability studies that use samples of human feces or blood plasma. Extraction of zinc from ashed samples yields aqueous solutions sufficiently devoid of matrix ions that could affect count rates and isotope ratios. Effects of sodium matrix, zinc concentration, and instrumental parameters on the precision of isotope ratio determinations are documented. Additions of spikes enriched in 67Zn and 70Zn to natural-abundance fecal samples verify that ratios can be determined on solutions 30 μM in zinc (70Zn and to 84 atom% excess of 67Zn. (Auth.)

  3. OPTIMAL CONTROL OF A NONLINEAR COUPLED ELECTROMAGNETIC INDUCTION HEATING SYSTEM WITH POINTWISE STATE CONSTRAINTS

    Directory of Open Access Journals (Sweden)

    Irwin Yousept

    2010-07-01

    Full Text Available An optimal control problem arising in the context of 3D electromagnetic induction heating is investigated. The state equation is given by a quasilinear stationary heat equation coupled with a semilinear time harmonic eddy current equation. The temperature-dependent electrical conductivity and the presence of pointwise inequality state-constraints represent the main challenge of the paper. In the first part of the paper, the existence and regularity of the state are addressed. The second part of the paper deals with the analysis of the corresponding linearized equation. Some suffcient conditions are presented which guarantee thesolvability of the linearized system. The final part of the paper is concerned with the optimal control. The aim of the optimization is to find the optimal voltage such that a desired temperature can be achieved optimally. The corresponding first-order necessary optimality condition is presented.

  4. Real-time analysis of CuO by inductively coupled plasma emission without external calibration

    International Nuclear Information System (INIS)

    The study of a method, devoted to real-time detection of metallic pollutants present in stack gas, is investigated. This method is based on spectroanalysis using an inductively coupled plasma (ICP) emission system without external calibration. The fluidized bed technology is employed to inject metallic species into the ICP emission. The mass fluxes of copper oxide (CuO) are then determined by using the intensity ratios of the metallic element spectral lines with those of the plasma gas element (argon or dry air). These ratios and the plasma characteristics (atomic excitation temperature, degree of thermal disequilibrium θ=Te/Th) are inserted into a calculation code of plasma composition to determine the mass flux. The results are in good agreement using either argon plasma or dry air plasma. A study of the fluidized bed properties is made to compare our values with those resulting from the elutriation calculation of the copper oxide

  5. Plutonium age dating (production date measurement) by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    This paper describes rapid methods for the determination of the production date (age dating) of plutonium (Pu) materials by inductively coupled plasma mass spectrometry (ICP-MS) for nuclear forensic and safeguards purposes. One of the presented methods is a rapid, direct measurement without chemical separation using 235U/239Pu and 236U/240Pu chronometers. The other method comprises a straightforward extraction chromatographic separation, followed by ICP-MS measurement for the 234U/238Pu, 235U/239Pu, 236U/240Pu and 238U/242Pu chronometers. Age dating results of two plutonium certified reference materials (SRM 946 and 947, currently distributed as NBL CRM 136 and 137) are in good agreement with the archive purification dates. (author)

  6. Inductively coupled plasma mass spectrometry (ICP-MS) and its application in life sciences

    International Nuclear Information System (INIS)

    Inductively-coupled plasma mass spectrometry (ICP-MS) has made much progress since its birth in the late 1990s. The author will give a rather systematic overview on the use of this technique in new devices and technologies related to plasma source, sample-introducing device and detecting spectrometer etc. In this overview, an emphasis will be put on the evaluation of the ICP-MS technique in combination with a series of physical, chemical and biological techniques, such as laser ablation (LA), capillary electrophoresis (CE) and high performance liquid chromatograph (HPLC), along with their representative high accuracy and high sensitivity. Finally, comprehensive and fruitful applications of the ICP-MS and its combinative techniques in the detection of trace metallic elements and isotopes in complex biological and environmental samples will be revealed

  7. Computational Finite Element Software Assisted Development of a 3D Inductively Coupled Power Transfer System

    Directory of Open Access Journals (Sweden)

    Pratik Raval

    2014-02-01

    Full Text Available To date inductively coupled power transfer (ICPT systems have already found many practical applications including battery charging pads. In fact, current charging platforms tend to largely support only one- or two-dimensional planar movement in load. This paper proposes a new concept of extending the aspect ratios of the operating power transfer volume of ICPT systems to support arbitrary three dimensional load movements with respect to the primary coils. This is done by use of modern finite element method analysis software to propose the primary and secondary magnetic structures of such an ICPT system. Firstly, two primary magnetic structures are proposed based on contrasting modes of operation and different field directions. This includes a single-phase and multi-phase current model. Next, a secondary magnetic structure is customized to be compatible with both primary structures. The resulting system is shown to produce a 3D power transfer volume for battery cell charging applications.

  8. Inductively Coupled Plasma: Fundamental Particle Investigations with Laser Ablation and Applications in Magnetic Sector Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Saetveit, Nathan Joe [Iowa State Univ., Ames, IA (United States)

    2008-01-01

    Particle size effects and elemental fractionation in laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) are investigated with nanosecond and femtosecond laser ablation, differential mobility analysis, and magnetic sector ICP-MS. Laser pulse width was found to have a significant influence on the LA particle size distribution and the elemental composition of the aerosol and thus fractionation. Emission from individual particles from solution nebulization, glass, and a pressed powder pellet are observed with high speed digital photography. The presence of intact particles in an ICP is shown to be a likely source of fractionation. A technique for the online detection of stimulated elemental release from neural tissue using magnetic sector ICP-MS is described. Detection limits of 1 μg L-1 or better were found for P, Mn, Fe, Cu, and Zn in a 60 μL injection in a physiological saline matrix.

  9. The inductively coupled plasma as a source for the measurement of fundamental spectroscopic constants

    International Nuclear Information System (INIS)

    Inductively coupled plasmas (ICPs) are stable, robust sources for the generation of spectra from neutral and singly ionized atoms. They are used extensively for analytical spectrometry, but have seen limited use for the measurement of fundamental spectroscopic constants. Several properties of the ICP affect its suitability for such fundamental measurements. They include: spatial structure, spectral background, noise characteristics, electron densities and temperatures, and the state of equilibrium in the plasma. These properties are particularly sensitive to the means by which foreign atoms are introduced into the plasma. With some departures from the operating procedures normally used in analytical measurements, the ICP promise to be a useful source for the measurement of fundamental atomic constants. (orig.)

  10. Measurement of neutral gas temperature in a 13.56 MHz inductively coupled plasma

    Energy Technology Data Exchange (ETDEWEB)

    Jayapalan, Kanesh K.; Chin, Oi Hoong [Plasma Technology Research Centre, Department of Physics, University of Malaya, 50603 Kuala Lumpur (Malaysia)

    2015-04-24

    Measuring the temperature of neutrals in inductively coupled plasmas (ICP) is important as heating of neutral particles will influence plasma characteristics such as the spatial distributions of plasma density and electron temperature. Neutral gas temperatures were deduced using a non-invasive technique that combines gas actinometry, optical emission spectroscopy and simulation which is described here. Argon gas temperature in a 13.56 MHz ICP were found to fall within the range of 500 − 800 K for input power of 140 − 200 W and pressure of 0.05 − 0.2 mbar. Comparing spectrometers with 0.2 nm and 0.5 nm resolution, improved fitting sensitivity was observed for the 0.2 nm resolution.

  11. Sulphate analysis in uranium leach iron(III) chloride solutions by inductively coupled argon plasma spectrometry

    International Nuclear Information System (INIS)

    Inductively coupled Argon Plasma Spectrometry is used for the indirect determination of sulphate in iron(III) chloride leach solution of Elliot Lake uranium ores via addition of a known amount of barium ions and analyzing for excess of barium. The ore contains ∼ 7 wt% pyrite, FeS2, as the major mineral which oxidizes to generate sulphate during leaching with Fe(III). The effects of pH, the concentrations of Fe(III) and chloride ions and for presence of ethanol in the test samples on the accuracy of analysis are studied. It is found that unlike the Rhodizonate method, removal of iron(III) from or addition of ethanol to the test sample prior to analysis are not required. Linear calibration curves are obtained. (author)

  12. RF electric field penetration and power deposition into nonequilibrium planar-type inductively coupled plasmas

    Institute of Scientific and Technical Information of China (English)

    Mao Ming; Wang Shuai; Dai Zhong-Ling; Wang You-Nian

    2007-01-01

    The RF electric field penetration and the power deposition into planar-type inductively coupled plasmas in lowpressure discharges have been studied by means of a self-consistent model which consists of Maxwell equations combined with the kinetic equation of electrons. The Maxwell equations are solved based on the expansion of the Fourier-Bessel series for determining the RF electric field. Numerical results show the influence of a non-Maxwellian electron energy distribution on the RF electric field penetration and the power deposition for different coil currents. Moreover, the two-dimensional spatial profiles of RF electric field and power density are also shown for different numbers of RF coil turns.

  13. Improved etch characteristics of SiO2 by the enhanced inductively coupled plasma

    International Nuclear Information System (INIS)

    The generation of active species for silicon dioxide etch and the formation of passivation layers on Si or photoresist is important for etching contact holes of high aspect ratio in sub-half-micron technology. Some methods use a process gas with high C/F ratio chemistry, such as C4F8, and/or apply a pulsed plasma technique, or radical control by chamber-wall modification. As a simple novel method, enhanced inductively coupled plasma (E-ICP) is expected to control the plasma characteristics by changing its E-ICP frequency; we tested the feasibility of using E-ICP for the process of contact hole etching. Scanning electron microscope images of etched profiles for micropatterns of 1 and 0.3 μm are shown to compare to the results by CW-ICP, magnetized-ICP, and E-ICP

  14. Fabrication of resonator-quantum well infrared photodetector focal plane array by inductively coupled plasma etching

    Science.gov (United States)

    Sun, Jason; Choi, Kwong-Kit

    2016-02-01

    Inductively coupled plasma (ICP) etching has distinct advantages over reactive ion etching in that the etching rates are considerably higher, the uniformity is much better, and the sidewalls of the etched material are highly anisotropic due to the higher plasma density and lower operating pressure. Therefore, ICP etching is a promising process for pattern transfer required during microelectronic and optoelectronic fabrication. Resonator-quantum well infrared photodetectors (R-QWIPs) are the next generation of QWIP detectors that use resonances to increase the quantum efficiency (QE). To fabricate R-QWIP focal plane arrays (FPAs), two optimized ICP etching processes are developed. Using these etching techniques, we have fabricated R-QWIP FPAs of several different formats and pixel sizes with the required dimensions and completely removed the substrates of the FPAs. Their QE spectra were tested to be 30 to 40%. The operability and spectral nonuniformity of the FPA is ˜99.5 and 3%, respectively.

  15. Inductively coupled plasma-induced etch damage of GaN p-n junctions

    International Nuclear Information System (INIS)

    Plasma-induced etch damage can degrade the electrical and optical performance of III-V nitride electronic and photonic devices. We have investigated the etch-induced damage of an inductively coupled plasma (ICP) etch system on the electrical performance of mesa-isolated GaN pn-junction diodes. GaN positive-insulating-negative mesa diodes were formed by Cl2/BCl3/Ar ICP etching under different plasma conditions. The reverse leakage current in the mesa diodes showed a strong relationship to chamber pressure, ion energy, and plasma flux. Plasma induced damage was minimized at moderate flux conditions (≤500 W), pressures ≥2 mTorr, and at ion energies below approximately -275 V. (c) 2000 American Vacuum Society

  16. Anisotropic Ta2O5 waveguide etching using inductively coupled plasma etching

    International Nuclear Information System (INIS)

    Smooth and vertical sidewall profiles are required to create low loss rib and ridge waveguides for integrated optical device and solid state laser applications. In this work, inductively coupled plasma (ICP) etching processes are developed to produce high quality low loss tantalum pentoxide (Ta2O5) waveguides. A mixture of C4F8 and O2 gas are used in combination with chromium (Cr) hard mask for this purpose. In this paper, the authors make a detailed investigation of the etch process parameter window. Effects of process parameters such as ICP power, platen power, gas flow, and chamber pressure on etch rate and sidewall slope angle are investigated. Chamber pressure is found to be a particularly important factor, which can be used to tune the sidewall slope angle and so prevent undercut

  17. Horn-coupled, commercially-fabricated aluminum lumped-element kinetic inductance detectors for millimeter wavelengths

    Energy Technology Data Exchange (ETDEWEB)

    McCarrick, H., E-mail: hlm2124@columbia.edu; Flanigan, D.; Jones, G.; Johnson, B. R.; Araujo, D.; Limon, M.; Luu, V.; Miller, A. [Department of Physics, Columbia University, New York, New York 10025 (United States); Ade, P.; Doyle, S.; Tucker, C. [School of Physics and Astronomy, Cardiff University, Cardiff, Wales CF24 3AA (United Kingdom); Bradford, K.; Che, G. [Department of Physics, Arizona State University, Tempe, Arizona 85287 (United States); Cantor, R. [STAR Cryoelectronics, Santa Fe, New Mexico 87508 (United States); Day, P.; Leduc, H. [Jet Propulsion Laboratory, Caltech, Pasadena, California 91109 (United States); Mauskopf, P. [School of Physics and Astronomy, Cardiff University, Cardiff, Wales CF24 3AA (United Kingdom); Department of Physics and School of Earth and Space Exploration, Arizona State University, Tempe, Arizona 85287 (United States); Mroczkowski, T. [Naval Research Laboratory, Washington DC 20375 (United States); Zmuidzinas, J. [Jet Propulsion Laboratory, Caltech, Pasadena, California 91109 (United States); Department of Physics, Caltech, Pasadena, California 91125 (United States)

    2014-12-15

    We discuss the design, fabrication, and testing of prototype horn-coupled, lumped-element kinetic inductance detectors (LEKIDs) designed for cosmic microwave background studies. The LEKIDs are made from a thin aluminum film deposited on a silicon wafer and patterned using standard photolithographic techniques at STAR Cryoelectronics, a commercial device foundry. We fabricated 20-element arrays, optimized for a spectral band centered on 150 GHz, to test the sensitivity and yield of the devices as well as the multiplexing scheme. We characterized the detectors in two configurations. First, the detectors were tested in a dark environment with the horn apertures covered, and second, the horn apertures were pointed towards a beam-filling cryogenic blackbody load. These tests show that the multiplexing scheme is robust and scalable, the yield across multiple LEKID arrays is 91%, and the measured noise-equivalent temperatures for a 4 K optical load are in the range 26±6 μK√(s)

  18. Inductively coupled plasma induced deep levels in epitaxial n-GaAs

    International Nuclear Information System (INIS)

    The electronic properties of defects introduced by low energy inductively coupled Ar plasma etching of n-type (Si doped) GaAs were investigated by deep level transient spectroscopy (DLTS) and Laplace DLTS. Several prominent electron traps (Ec—0.046 eV, Ec—0.186 eV, Ec—0.314 eV. Ec—0.528 eV and Ec—0.605 eV) were detected. The metastable defect Ec—0.046 eV having a trap signature similar to E1 is observed for the first time. Ec—0.314 eV and Ec—0.605 eV are metastable and appear to be similar to the M3 and M4 defects present in dc H-plasma exposed GaAs.

  19. Effect of Skimmer Cone Material on the Spectra of Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    The inductively coupled plasma ion source for mass spectrometry is very sensitive for multielement analysis with detection limits down to sub part per trillion (ppt). Polyatomic ions which could be formed in the mass spectra may interfere in the analysis of some element. Experimental conditions have great influences on the formation of polyatomic ions. The present work demonstrates that the skimmer materials (Au, Ag, Ni, and Cu) are participating in the formation of polyatomic ions, meanwhile the sampler materials have no real effect. The mechanism of formation of polyatomic ions is explained. Heats of formation of polyatomic species formed from the skimmer materials such as: Au X, Ag X, Ni X and Cu X; where X= Ar, O, N, C and H are calculated by Gaussian program (G 94 W)

  20. Photoluminescence enhancement by inductively coupled argon plasma exposure for quantum-well intermixing

    International Nuclear Information System (INIS)

    The exposure of InGaAs/InGaAsP quantum-well (QW) structures to argon (Ar) plasma in an inductively coupled system has been studied. An increase in photoluminescence (PL) intensity without PL peak shift was observed for 5-min Ar plasma exposure compared to the as-grown sample. The exposure creates point defects, and upon rapid thermal annealing produces intermixing between barriers and QWs, resulting in the blueshift of QWs. A selective intermixing using a 200-nm-thick of SiO2 layer as an intermixing mask exhibited a differential band-gap blueshift of 86 nm, with a differential linewidth broadening of 0.3 nm between masked and unmasked section. The improvement of PL intensity in combination with selective intermixing process can pave the way for high-quality hybrid photonic and optoelectronic integrated circuits

  1. Multi-elemental analysis of aqueous geological samples by inductively coupled plasma-optical emission spectrometry

    Science.gov (United States)

    Todorov, Todor I.; Wolf, Ruth E.; Adams, Monique

    2014-01-01

    Typically, 27 major, minor, and trace elements are determined in natural waters, acid mine drainage, extraction fluids, and leachates of geological and environmental samples by inductively coupled plasma-optical emission spectrometry (ICP-OES). At the discretion of the analyst, additional elements may be determined after suitable method modifications and performance data are established. Samples are preserved in 1–2 percent nitric acid (HNO3) at sample collection or as soon as possible after collection. The aqueous samples are aspirated into the ICP-OES discharge, where the elemental emission signals are measured simultaneously for 27 elements. Calibration is performed with a series of matrix-matched, multi-element solution standards.

  2. A comprehensive study of different gases in inductively coupled plasma torch operating at one atmosphere

    Energy Technology Data Exchange (ETDEWEB)

    Punjabi, Sangeeta B. [Electrical Engineering Department, V. J.T.I, Matunga, Mumbai 400019 (India); Department of Physics, University of Mumbai, Kalina, Santacruz(E) 400098 (India); Joshi, N. K. [Faculty of Engineering and technology, MITS, lakshmangarh, (Sikar), Rajasthan 332311 (India); Mangalvedekar, H. A.; Lande, B. K. [Electrical Engineering Department, V. J.T.I, Matunga, Mumbai 400019 (India); Das, A. K. [Laser and Plasma Technology Division, BARC, Mumbai 400085 (India); Kothari, D. C. [Department of Physics, University of Mumbai, Kalina, Santacruz(E) 400098 (India)

    2012-01-15

    A numerical study is done to understand the possible operating regimes of RF-ICP torch (3 MHz, 50 kW) using different gases for plasma formation at atmospheric pressure. A two dimensional numerical simulation of RF-ICP torch using argon, nitrogen, oxygen, and air as plasma gas has been investigated using computational fluid dynamic (CFD) software fluent{sup (c)}. The operating parameters varied here are central gas flow, sheath gas flow, RF-power dissipated in plasma, and plasma gas. The temperature contours, flow field, axial, and radial velocity profiles were investigated under different operating conditions. The plasma resistance, inductance of the torch, and the heat distribution for various plasma gases have also been investigated. The plasma impedance of ICP torch varies with different operating parameters and plays an important role for RF oscillator design and power coupling. These studies will be useful to decide the design criteria for ICP torches required for different material processing applications.

  3. Evaluation of correction method for mass discrimination effect in multiple collector inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    This paper describes advances in isotopic measurements that have been made with an inductively coupled plasma source magnetic sector multiple collector mass spectrometer (MC-ICP-MS) and presents results of new experiments aimed at further evaluating the instrumental capability as well as the correction technique for the mass discrimination effects. The ability to correct for the mass discrimination effect using a second element of similar mass and very high sensitivity for elements that are otherwise difficult to ionize gives this instrument major advantages over other conventional techniques for isotopic measurements. The isotopic data obtained by MC-ICP-MS clearly demonstrate potential as a new technique to produce precise and reproducible isotopic data for the elements that are difficult to measure by thermal ionization mass spectrometry (TIMS). (author)

  4. A study of isotope ratio measurement by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    The measurement of isotopic ratios by inductively coupled plasma mass spectrometry (ICP-MS) has the benefits of ionising all metallic elements, simplifying sample preparation and reducing analysis time, when compared with thermal ionisation mass spectrometry (TIMS). However, the use of ICP-MS in isotopic ratio studies has been somewhat restricted by its failure to offer the precision and accuracy required by a variety of applications. The precision achievable by ICP-MS, typically 0.2 to 0.3% RSD, for isotopic ratios, has generally been regarded as being primarily limited by instrumental instability. An investigation of the sources of instrumental noise in ICP-MS has been undertaken, utilising noise spectral analysis as a diagnostic aid. Study of parametric variation upon noise production has identified the methods by which modulation of the ion signal occurs. Noise spectral analysis has allowed an understanding of the limitations imposed upon measurement precision by the various contributing noise sources to be established. (author)

  5. Stable isotope dilution analysis of hydrologic samples by inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Garbarino, J.R.; Taylor, H.E.

    1987-01-01

    Inductively coupled plasma mass spectrometry is employed in the determination of Ni, Cu, Sr, Cd, Ba, Ti, and Pb in nonsaline, natural water samples by stable isotope dilution analysis. Hydrologic samples were directly analyzed without any unusual pretreatment. Interference effects related to overlapping isobars, formation of metal oxide and multiply charged ions, and matrix composition were identified and suitable methods of correction evaluated. A comparability study snowed that single-element isotope dilution analysis was only marginally better than sequential multielement isotope dilution analysis. Accuracy and precision of the single-element method were determined on the basis of results obtained for standard reference materials. The instrumental technique was shown to be ideally suited for programs associated with certification of standard reference materials.

  6. Determination of elemental content off rocks by laser ablation inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Lichte, F.E.

    1995-01-01

    A new method of analysis for rocks and soils is presented using laser ablation inductively coupled plasma mass spectrometry. It is based on a lithium borate fusion and the free-running mode of a Nd/YAG laser. An Ar/N2 sample gas improves sensitivity 7 ?? for most elements. Sixty-three elements are characterized for the fusion, and 49 elements can be quantified. Internal standards and isotopic spikes ensure accurate results. Limits of detection are 0.01 ??g/g for many trace elements. Accuracy approaches 5% for all elements. A new quality assurance procedure is presented that uses fundamental parameters to test relative response factors for the calibration.

  7. Standard practice for alternate actinide calibration for inductively coupled plasma-mass spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2004-01-01

    1.1 This practice provides guidance for an alternate linear calibration for the determination of selected actinide isotopes in appropriately prepared aqueous solutions by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). This alternate calibration is mass bias adjusted using thorium-232 (232Th) and uranium-238 (238U) standards. One of the benefits of this standard practice is the ability to calibrate for the analysis of highly radioactive actinides using calibration standards at much lower specific activities. Environmental laboratories may find this standard practice useful if facilities are not available to handle the highly radioactive standards of the individual actinides of interest. 1.2 The instrument response for a series of determinations of known concentration of 232Th and 238U defines the mass versus response relationship. For each standard concentration, the slope of the line defined by 232Th and 238U is used to derive linear calibration curves for each mass of interest using interference equ...

  8. Ion kinetic energies in inductively coupled plasma/mass spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    Ion kinetic energies in an inductively coupled plasma/mass spectrometer (ICP-MS) system have been measured with the use of a retarding potential on the analyzing quadrupole. The energies differ markedly from those previously reported in the literature. This is attributed to the elimination of any arcing of the ICP to the sampling orifice or skimmer of the ICP-MS system. In the absence of secondary discharge effects, the ion energies increase with the mass of the ion and are consistent with those expected from molecular beam sampling from a plasma with a temperature of --5000 K and a potential of --2 V. Ion energies are found to be virtually independent of aerosol gas flow, plasma power, and sample matrix composition, allowing independent optimization of plasma parameters and ion optics

  9. Metal determination in samples of plants by high resolution inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    In the last years, the use of environmental monitoring to determine anthropogenic metal insertions in the environment has been widely discussed as an alternative method to the direct measurement of these emissions to the ecosystem. This paper describes the determination of several chemical elements present in pine needles samples, including thorium, uranium using the High Resolution inductively Coupled Plasma and rare earths, Mass Spectrometer (HR-ICP-MS). The method of internal standardization was used to compense the non-spectral interferences of the different elements present in sample solution matrix. The chemical element bismuth (Bi) was chosen to act as an internal standard. In order to determine the accuracy of the proposed method, certified samples of pine needles (Nation Bureau of Standards Standard Reference Material 1575) were analyzed. (author)

  10. Low-frequency, self-sustained oscillations in inductively coupled plasmas used for optical pumping

    Energy Technology Data Exchange (ETDEWEB)

    Coffer, J.; Encalada, N.; Huang, M.; Camparo, J. [Physical Sciences Laboratories, The Aerospace Corporation 2310, E. El Segundo Blvd., El Segundo, California 90245 (United States)

    2014-10-28

    We have investigated very low frequency, on the order of one hertz, self-pulsing in alkali-metal inductively-coupled plasmas (i.e., rf-discharge lamps). This self-pulsing has the potential to significantly vary signal-to-noise ratios and (via the ac-Stark shift) resonant frequencies in optically pumped atomic clocks and magnetometers (e.g., the atomic clocks now flying on GPS and Galileo global navigation system satellites). The phenomenon arises from a nonlinear interaction between the atomic physics of radiation trapping and the plasma's electrical nature. To explain the effect, we have developed an evaporation/condensation theory (EC theory) of the self-pulsing phenomenon.

  11. Inductively coupled plasma mass spectrometry with ambient helium surrounding ion source

    International Nuclear Information System (INIS)

    An enclosed device surrounding the argon inductively coupled plasma torch was fabricated to exclude air entrainment and attenuate background interferences. Helium was introduced into the enclosure, and ambient helium plasma was formed stably. Under cold plasma condition, we found that the spectral background decreased about 1 order of magnitude averagely compared with that in typical operation condition. For laser ablation with a Nd:YAG laser, the limits of detection of 28Si, 29Si, 31P, and 32S in an iron matrix were improved significantly; the linearity of their calibration curves was greatly improved as well compared with standard mode and cool mode ICP-MS with no ambient helium. The result indicates that polyatomic interferences from nitrogen, oxygen, hydrogen, carbon, etc. were effectively reduced in helium ambient ICP-MS.

  12. Pulsed radio-frequency discharge inductively coupled plasma mass spectrometry for oxide analysis

    Science.gov (United States)

    Li, Weifeng; Yin, Zhibin; Hang, Wei; Li, Bin; Huang, Benli

    2016-08-01

    A direct solid sampling technique has been developed based on a pulsed radio-frequency discharge (RFD) in mixture of N2 and Ar environment at atmospheric pressure. With an averaged input power of 65 W, a crater with the diameter of 80 μm and depth of 50 μm can be formed on sample surface after discharge for 1 min, suggesting the feasibility of the pulsed RFD for sampling nonconductive solids. Combined with inductively coupled plasma mass spectrometry (ICPMS), this technique allows to measure elemental composition of solids directly with relative standard deviation (RSD) of ~ 20%. Capability of quantitative analysis was demonstrated by the use of soil standards and artificial standards. Good calibration linearity and limits of detection (LODs) in range of 10- 8-10- 9 g/g were achieved for most elements.

  13. Modeling and simulation of ion-filtered inductively coupled plasma using argon plasma

    International Nuclear Information System (INIS)

    An ion-filtered inductively coupled plasma (IF-ICP) is proposed to reduce ion bombardment and provide high metastable species density for chemical vapor deposition. Argon plasma, which has simple reaction mechanism, is simulated to show the effects of ion filter. Compared to typical ICP, the maximum density of ions of IF-ICP is lower while that of metastable species is higher. The filter can absorb ions effectively and relatively small amount of metastable species, with the absorption coefficient proportional to its surface area. A proper gap between filter and substrate can achieve more metastable species and less ions on the substrate. The pressure and RF power need to be optimized based on the tradeoff between deposition rate and ion damage. The density of ions on the substrate can be reduced by two orders of magnitude while that of metastable species are maintained in the order of 1017 m-3 under the optimized conditions. (author)

  14. Effect of the electron energy distribution on total energy loss with argon in inductively coupled plasmas

    International Nuclear Information System (INIS)

    The total energy lost per electron-ion pair lost εT is investigated with the electron energy distribution function (EEDF). The EEDFs are measured at various argon powers in RF inductively coupled plasma, and the EEDFs show a depleted distribution (a discontinuity occurring at the minimum argon excitation threshold energy level) with the bulk temperature and the tail temperature. The total energy loss per electron-ion pair lost εT is calculated from a power balance model with the Maxwellian EEDFs and the depleted EEDFs and then compared with the measured εT from the floating probe. It is concluded that the small population of the depleted high energy electrons dramatically increases the collisional energy loss, and the calculated εT from the depleted EEDFs has a value that is similar to the measured εT

  15. Expressing self-absorption in the analytical function of inductively coupled plasma atomic emission spectrometry

    Science.gov (United States)

    Kántor, Tibor; Bartha, András

    2015-11-01

    The self-absorption of spectral lines was studied with up to date multi-element inductively coupled plasma atomic emission spectrometry (ICP-AES) instrumentation using radial and axial viewing of the plasma, as well, performing line peak height and line peak area measurements. Two resonance atomic and ionic lines of Cd and Mg were studied, the concentration range was extended up to 2000 mg/L. At the varying analyte concentration, constant matrix concentration of 10,000 mg/L Ca was ensured in the pneumatically nebulized solutions. The physical and the phenomenological formulation of the emission analytical function is overviewed and as the continuity of the earlier results the following equation is offered:

  16. Inductively coupled plasma optical emission spectroscopy determination of trace element composition of argan oil.

    Science.gov (United States)

    Gonzálvez, A; Ghanjaoui, M E; El Rhazi, M; de la Guardia, M

    2010-02-01

    A methodology based on inductively coupled plasma optical emission spectroscopy (ICP-OES) after microwave assisted acid digestion has been developed to determine the trace element content of Moroccan argan oil. Limit of detection values equal or lower than few mg/kg were obtained for all elements under study. To assure the accuracy of the whole procedure, recovery studies were carried out on argan oil samples spiked at different concentration levels from 10 to 200 µg/L. Quantitative average recovery values were obtained for all elements evaluated, demonstrating the suitability of this methodology for the determination of trace elements in argan oil samples. Aluminum, calcium, chromium, iron, potassium, lithium, magnesium, sodium, vanadium and zinc were quantitatively determined in Moroccan argan oils being found that their concentration is different of that found in other edible oils thus offering a way for authentication and for the evaluation of possible adulterations. PMID:21339122

  17. Heavy metals in aromatic spices by inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Bua, Daniel Giuseppe; Annuario, Giovanni; Albergamo, Ambrogina; Cicero, Nicola; Dugo, Giacomo

    2016-09-01

    Objective of this study was to determine the content of Cd, Hg, As and Pb in common spices traded in the Italian market, using inductively coupled plasma-mass spectrometry (ICP-MS). The results were compared with the maximum limits established by the national Legislative Decree (LD) no. 107 implementing the Council Directive 88/388/EEC and by international organisations, such as Food and Agriculture Organization (FAO) and World Health Organization (WHO). Food safety for spices was assessed considering the tolerable weekly intake (TWI) and the provisional tolerable weekly intake (PTWI), respectively, for Cd and Hg and the 95% lower confidence limit of the benchmark dose of 1% extra risk (BMDL01) for As and Pb. Investigated elements in all samples were within the maximum limits as set by the national and international normative institutions. Nevertheless, the heavy metal content of some spices exceeded the PTWI, TWI and BMDL01, which needs attention when considering consumer's health. PMID:27074712

  18. Determination of Rare Earth Elements in Thai Monazite by Inductively Coupled Plasma and Nuclear Analytical techniques

    International Nuclear Information System (INIS)

    The inductively coupled plasma atomic emission spectroscopy (ICP-AES) for the determination of individual rare-earth elements (REE) was evaluated by comparison with instrumental neutron activation analysis (INAA) and x-ray fluorescence spectrometry (XRF). The accuracy and precision of INAA and ICP-AES were evaluated by using standard reference material IGS-36, a monazite concentrate. For INAA, the results were close to the certified value while ICP-AES were in good agreement except for some low concentration rare earth. The techniques were applied for the analysis of some rare earth elements in two Thai monazite samples preparing as the in-house reference material for the Rare Earth Research and Development Center, Chemistry Division, Office of Atoms for Peace. The analytical results obtained by these techniques were in good agreement with each other

  19. Homogeneous nanocrystalline cubic silicon carbide films prepared by inductively coupled plasma chemical vapor deposition.

    Science.gov (United States)

    Cheng, Qijin; Xu, S; Long, Jidong; Huang, Shiyong; Guo, Jun

    2007-11-21

    Silicon carbide films with different carbon concentrations x(C) have been synthesized by inductively coupled plasma chemical vapor deposition from a SiH(4)/CH(4)/H(2) gas mixture at a low substrate temperature of 500 °C. The characteristics of the films were studied by x-ray photoelectron spectroscopy, x-ray diffraction, scanning electron microscopy, high-resolution transmission electron microscopy, Fourier transform infrared absorption spectroscopy, and Raman spectroscopy. Our experimental results show that, at x(C) = 49 at.%, the film is made up of homogeneous nanocrystalline cubic silicon carbide without any phase of silicon, graphite, or diamond crystallites/clusters. The average size of SiC crystallites is approximately 6 nm. At a lower value of x(C), polycrystalline silicon and amorphous silicon carbide coexist in the films. At a higher value of x(C), amorphous carbon and silicon carbide coexist in the films. PMID:21730481

  20. Al-Induced Crystallization Growth of Si Films by Inductively Coupled Plasma Chemical Vapour Deposition

    Institute of Scientific and Technical Information of China (English)

    LI Jun-Shuai; WANG Jin-Xiao; YIN Min; GAO Ping-Qi; HE De-Yan

    2006-01-01

    Polycrystalline Si (poly-Si) films are in situ grown on Al-coated glass substrates by inductively coupled plasma chemical vapour deposition at a temperature as low as 350 C. Compared to the traditional annealing crystallization of amorphous Si/Al-layer structures, no layer exchange is observed and the resultant poly-Si film is much thicker than Al layer. By analysing the depth profiles of the elemental composition, no remains of Al atoms are detected in Si layer within the limit (< 0.01 at. %) of the used evaluations. It is indicated that the poly-Si material obtained by Al-induced crystallization growth has more potential applications than that prepared by annealing the amorphous Si/Al-layer structures.

  1. Inductively Coupled Plasma: Fundamental Particle Investigations with Laser Ablation and Applications in Magnetic Sector Mass Spectrometry

    International Nuclear Information System (INIS)

    Particle size effects and elemental fractionation in laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) are investigated with nanosecond and femtosecond laser ablation, differential mobility analysis, and magnetic sector ICP-MS. Laser pulse width was found to have a significant influence on the LA particle size distribution and the elemental composition of the aerosol and thus fractionation. Emission from individual particles from solution nebulization, glass, and a pressed powder pellet are observed with high speed digital photography. The presence of intact particles in an ICP is shown to be a likely source of fractionation. A technique for the online detection of stimulated elemental release from neural tissue using magnetic sector ICP-MS is described. Detection limits of 1 (micro)g L-1 or better were found for P, Mn, Fe, Cu, and Zn in a 60 (micro)L injection in a physiological saline matrix

  2. Assessment of the analytical capabilities of inductively coupled plasma-mass spectrometry

    Science.gov (United States)

    Taylor, H.E.; Garbarino, J.R.

    1988-01-01

    A thorough assessment of the analytical capabilities of inductively coupled plasma-mass spectrometry was conducted for selected analytes of importance in water quality applications and hydrologic research. A multielement calibration curve technique was designed to produce accurate and precise results in analysis times of approximately one minute. The suite of elements included Al, As, B, Ba, Be, Cd, Co, Cr, Cu, Hg, Li, Mn, Mo, Ni, Pb, Se, Sr, V, and Zn. The effects of sample matrix composition on the accuracy of the determinations showed that matrix elements (such as Na, Ca, Mg, and K) that may be present in natural water samples at concentration levels greater than 50 mg/L resulted in as much as a 10% suppression in ion current for analyte elements. Operational detection limits are presented.

  3. Transport and trapping of dust particles in a potential well created by inductively coupled diffused plasma

    CERN Document Server

    Choudhary, Mangilal; Bandyopadhyay, P

    2016-01-01

    A versatile linear dusty (complex) plasma device is designed to study the transport and dynamical behavior of dust particles in a large volume. Diffused inductively coupled plasma is generated in the background of argon gas. A novel technique is used to introduce the dust particles in the main plasma by striking a secondary direct current (DC) glow discharge. These dust particles are found to get trapped in an electrostatic potential well which is formed due to the combination of the ambipolar electric field caused by diffusive plasma and the field produced by the charged glass wall of the vacuum chamber. According to the requirements, the volume of the dust cloud can be controlled very precisely by tuning the plasma and discharge parameters. The present device can be used to address the underlying physics behind the transport of dust particles, self excited dust acoustic waves and instabilities. The detailed design of this device, plasma production and characterization, trapping and transport of the dust par...

  4. Comparison of germanium and silicon dry etching by using inductively coupled BCl3 plasma

    International Nuclear Information System (INIS)

    We have investigated the etch rates and the angle subtended for Ge and Si as a function of the BCl3 flow rate, the inductively coupled plasma (ICP) power, and the work pressure. The Ge etch rate is always greater than the Si etch rate, and the maxima of the Ge and Si etch rates are observed to be functions of the BCl3 flow rate. The peak etch rate is at 40 sccm BCl3 flow rate. The etch rate of Ge decreases from 2370 to 1780 A/min as the BCl3 flow rate increases from 40 to 80 sccm. Also, the etch rate of Si decreases from 640 to 460 A/min as the BCl3 flow rate increases from 20 to 80 sccm. The largest Ge/Si etch rate ratio is obtained for BCl3 flow rate of 60 sccm. The etch rate of Ge decreases from 2835 to 2094 A/min as the ICP power increases from 200 to 500 W whereas the etching rate of Ge increases from 2370 to 2900 A/min as the work pressure increases from 10 to 50 mTorr. As the BCl3 flow, ICP power, and work pressure, increase the angle subtended also increases. Optical emission spectroscopy (OES) has been used to examine the gas phase species in the plasma, and emission from excited atomic B and Cl has been identified. The composition of the reaction layer on germanium due to the BCl3 plasmas has been obtained by using X-ray photoelectron spectroscopy (XPS). The reaction layer on germanium due to inductively coupled BCl3 plasma etching is found to be typically a very thin layer of the Ge-Cl and Ge-O.

  5. Ignition delay of a pulsed inductively coupled plasma (ICP) in tandem with an auxiliary ICP

    Science.gov (United States)

    Liu, Lei; Sridhar, Shyam; Donnelly, Vincent M.; Economou, Demetre J.

    2015-12-01

    Plasma ignition delays were observed in a ‘main’ inductively coupled plasma (ICP), in tandem with an ‘auxiliary’ ICP. The Faraday-shielded ICPs were separated by a grounded metal grid. Power (13.56 MHz) to the main ICP was pulsed with a frequency of 1 kHz, while the auxiliary ICP was operated in continuous wave (cw) mode. In chlorine plasmas, ignition delay was observed for duty cycles greater than 60% and, in contrast to expectation, the delay was longer with increasing duty cycle up to ~99.5%. The ignition delay could be varied by changing the auxiliary and/or main ICP power. Langmuir probe measurements provided the temporal evolution of electron temperature, and electron and positive ion densities. These measurements revealed that the plasma was ignited shortly after the decaying positive ion density (n +), in the afterglow of the main ICP, reached the density ({{n}+},\\text{aux} ) prevailing when only the auxiliary ICP was powered. At that time, production of electrons began to dominate their loss in the main ICP, due to hot electron injection from the auxiliary ICP. As a result, {{n}\\text{e}} increased from a value below {{n}\\text{e,\\text{aux}}} , improving inductive power coupling efficiency, further increasing plasma density leading to plasma ignition. Plasma ignition delay occurred when the afterglow of the pulsed plasma was not long enough for the ion density to reach {{n}+},\\text{aux} during the afterglow. Besides Cl2, plasma ignition delays were also observed in other electronegative gases (SF6, CF4/O2 and O2) but not in an electropositive gas (Ar).

  6. A “wire” signal smoothing device for laser ablation inductively coupled plasma mass spectrometry analysis

    International Nuclear Information System (INIS)

    A novel signal smoothing device for laser ablation inductively coupled plasma mass spectrometry was developed. The “wire” signal smoothing device consists of a copper cylinder filled with steel wire, with an internal volume of approx. 94 cm3. The effectiveness of the “wire” signal smoothing device was evaluated with respect to both signal stability and decay time. With the developed “wire” smoothing device, no oscillation of the signal intensity was observed, even at a repetition rate of 1 Hz. This finding indicates that this device is well suited for routine optimization of laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The signal stability was improved by a factor of 11 compared to the absence of a signal smoothing device at a repetition rate of 1 Hz. Another significant advantage of the “wire” smoothing device is that the signal decay time is similar to that without the signal smoothing device. These properties cause the “wire” smoothing device to be well suited for low repetition rate laser ablation analysis, which provides smaller elemental fractionation and better spatial resolution. The proposed “wire” signal smoothing device has been successfully used for high depth resolution zircon dating. - Highlights: ► The wire stabilizer is able to provide smooth signals at a repetition rate of 1 Hz. ► The signal decay time is similar to that in the absence of a signal stabilizer. ► The wire stabilizer has been successfully used for zircon dating.

  7. Analysis of non-equilibrium phenomena in inductively coupled plasma generators

    Science.gov (United States)

    Zhang, W.; Lani, A.; Panesi, M.

    2016-07-01

    This work addresses the modeling of non-equilibrium phenomena in inductively coupled plasma discharges. In the proposed computational model, the electromagnetic induction equation is solved together with the set of Navier-Stokes equations in order to compute the electromagnetic and flow fields, accounting for their mutual interaction. Semi-classical statistical thermodynamics is used to determine the plasma thermodynamic properties, while transport properties are obtained from kinetic principles, with the method of Chapman and Enskog. Particle ambipolar diffusive fluxes are found by solving the Stefan-Maxwell equations with a simple iterative method. Two physico-mathematical formulations are used to model the chemical reaction processes: (1) A Local Thermodynamics Equilibrium (LTE) formulation and (2) a thermo-chemical non-equilibrium (TCNEQ) formulation. In the TCNEQ model, thermal non-equilibrium between the translational energy mode of the gas and the vibrational energy mode of individual molecules is accounted for. The electronic states of the chemical species are assumed in equilibrium with the vibrational temperature, whereas the rotational energy mode is assumed to be equilibrated with translation. Three different physical models are used to account for the coupling of chemistry and energy transfer processes. Numerical simulations obtained with the LTE and TCNEQ formulations are used to characterize the extent of non-equilibrium of the flow inside the Plasmatron facility at the von Karman Institute. Each model was tested using different kinetic mechanisms to assess the sensitivity of the results to variations in the reaction parameters. A comparison of temperatures and composition profiles at the outlet of the torch demonstrates that the flow is in non-equilibrium for operating conditions characterized by pressures below 30 000 Pa, frequency 0.37 MHz, input power 80 kW, and mass flow 8 g/s.

  8. Quantitative Characterization of Gold Nanoparticles by Field-Flow Fractionation Coupled Online with Light Scattering Detection and Inductively Coupled Plasma Mass Spectrometry

    OpenAIRE

    Schmidt, Bjørn; Löschner, Katrin; Hadrup, Niels; Mortensen, Alicja; Sloth, Jens Jørgen; Bender Koch, Christian; Larsen, Erik Huusfeldt

    2011-01-01

    An analytical platform coupling asymmetric flow field-flow fractionation (AF4) with multiangle light scattering (MALS), dynamic light scattering (DLS), and inductively coupled plasma mass spectrometry (ICPMS) was established and used for separation and quantitative determination of size and mass concentration of nanoparticles (NPs) in aqueous suspension. Mixtures of three polystyrene (PS) NPs between 20 and 100 nm in diameter and mixtures of three gold (Au) NPs between 10 and 60 nm in diamete...

  9. Capacitively coupled contactless conductivity detection and sequential injection analysis in capillary electrophoresis and capillary electro-chromatography

    OpenAIRE

    Mai, Thanh Duc

    2011-01-01

    This thesis focuses on the applications of capacitively coupled contactless conductivity detection (C4D) in capillary electrophoresis (CE) hybridized with high-performance liquid chromatography (HPLC), i.e. in capillary electrochromatography and pressure-assisted capillary electrophoresis, as well as on the development and applications of an extension of CE-C4D with sequential injection analysis (SIA). At first, the in-house built C4D was used for electro-chromatographic determinations of...

  10. Supercritical Fluid Extraction Directly Coupled with Reversed Phase Liquid Chromatography for Quantitative Analysis of Analytes in Complex Matrices

    OpenAIRE

    Wang, Zhenyu

    2004-01-01

    The purpose of this research was to design a simple, novel interface for on-line coupling of Supercritical Fluid Extraction (SFE) with High Performance Reversed Phase Liquid Chromatography (HP-RPLC), and to explore its ability for quantitative analysis of analytes in different matrices. First, a simple interface was developed via a single one six-port injection valve to connect the SFE and LC systems. A water displacement method was utilized to eliminate decompressed CO2 gas in the solid phas...

  11. Identification of the Related Substances in Ampicillin Capsule by Rapid Resolution Liquid Chromatography Coupled with Electrospray Ionization Tandem Mass Spectrometry

    OpenAIRE

    Lei Zhang; Xian Long Cheng; Yang Liu; Miao Liang; Honghuan Dong; Beiran Lv; Wenning Yang; Zhiqiang Luo; Mingmin Tang

    2014-01-01

    Rapid Resolution Liquid Chromatography coupled with Electrospray Ionization Tandem Mass Spectrometry (RRLC-ESI-MSn) was used to separate and identify related substances in ampicillin capsule. The fragmentation behaviors of related substances were used to identify their chemical structures. Finally, a total of 13 related substances in ampicillin capsule were identified, including four identified components for the first time and three groups of isomers on the basis of the exact mass, fragmenta...

  12. Potential of on-line coupling of extraction and chromatography in the analysis of complex samples

    Czech Academy of Sciences Publication Activity Database

    Hyötyläinen, T.; Lüthje, K.; Rautiainen-Rämä, M.; Pól, Jaroslav; Ranta-Aho, O.; Riekkola, M. L.

    Kortrijk: I.O.P.M.S. vzw, 2004 - (Sandra, T.; Sandra, P.), J12 [International Symposium on Capillary Chromatography /27./. Riva del Garda (IT), 31.05.2004-04.06.2004] R&D Projects: GA AV ČR KJB4031405 Institutional research plan: CEZ:AV0Z4031919 Keywords : on-line - extraction * chromatography Subject RIV: CB - Analytical Chemistry, Separation

  13. [Characterization method for metallothioneins by reversed-phase liquid chromatography coupled with electrospray ionization mass spectrometry].

    Science.gov (United States)

    Huang, Zhiyong; Shen, Jincan; Zhuang, Zhixia; Wang, Xiaoru; Lee, Frank Sen-Chun

    2004-11-01

    Mammalian metallothioneins (MTs) usually have two major isoforms, MT-1 and MT-2, existing in tissues because of the genetic polymorphism. Metallothionein isoforms and sub-isoforms were characterized with a hyphenated technique of reversed-phase liquid chromatography (RPLC) coupled with electrospray ionization mass spectrometry (ESI-MS). The MT-isoform separation was carried out using a C8 narrow-bore column Vydac C8 (250 mm x 2.1 mm i.d., 5 microm, 30 nm). Buffer A was 5 mmol/L ammonium acetate in water (pH 6.0) and buffer B was 5 mmol/L ammonium acetate in methanol-water (1:1, v/v) (pH 6.0). A linear gradient elution was used by increasing buffer B from 10% to 37.5% within 40 min. The flow rate was set at 0.20 mL/min. The tentative formulas of MT isoforms and subisoforms were interpreted with the measured masses at the vicinity of apexes in total ion current chromatogram of ESI-MS and the reference data reported previously. The method was validated with the standard reference materials of MT-1 and MT-2. The results indicated that many MT species interpreted were in good agreement with the reference data reported. The MT sample from rabbit liver was measured with the established method. The results, of which the apo-MT was used by acidification of the sample for simplifying the mass spectra, showed that there were species of MT isoforms and subisoforms in rabbit livers. PMID:15807108

  14. Quantitative analysis of antibiotics in aquifer sediments by liquid chromatography coupled to high resolution mass spectrometry.

    Science.gov (United States)

    Tong, Lei; Liu, Hui; Xie, Cong; Li, Minjing

    2016-06-24

    A highly effective analytical method for multi-residue determination of antibiotics in aquifer sediments was first established in this study. Microwave-assisted solvent extraction (MASE) and solid-phase extraction were used for sample pre-concentration and purification, ultra-high performance liquid chromatography coupled to hybrid quadrupole-high resolution Orbitrap mass spectrometry (UHPLC-Q-Orbitrap) was applied for detection. For high resolution mass spectrometry (HRMS), the target compounds were tentatively identified by retention time and accurate mass which was measured with precursor ions in Target-SIM scan, and then confirmed by the monitoring of daughter ion fragments which were generated in dd-MS(2) scan. The results provided good mass accuracy with mass deviations below 2ppm (except norfloxacin with -2.3ppm) for quantitative analysis of the compounds by HRMS. Reasonable recoveries of all analytes were obtained more than 60% (except doxytetracycline) in fortification samples at concentrations higher than 10μgkg(-1). Relative standard deviations of repeatability and inter-day precision were below 21% and 11%. Limits of detection (LOD) ranged from 0.1 to 3.8μgkg(-1), whereas limits of quantification (LOQ) were established between 0.3-9.0μgkg(-1). The method was applied to analyze real aquifer sediment samples in different aquifer depth of 4.0, 7.5, 13.0 and 18.0m. Chlorotetracycline and ofloxacin were observed at relative high concentrations of 53 and 19μgkg(-1) respectively in 18.0m deepness. The exposure to low doses of these compounds in subsurface environment increases concerns on long-term ecological security of underground system. PMID:27215464

  15. Ionizing radiation effects in Acai oil analysed by gas chromatography coupled to mass spectrometry technique

    International Nuclear Information System (INIS)

    The Acai fruit is a well know Brazilian seed plant used in large scale as a source of feed stock, specially in the Brazilian North-east region. The Acai oil is use in many purposes from fuel sources to medicine. The scope of this paper is to analyzed the chemical structures modification of the acai oil after the ionizing radiation. The radiation were set in the range of 10 to 25 kGy in the extracted Acai oil. The analyses were made by gas chromatography coupled to mass spectrometry techniques. A GC/MS Shimatzu QP-5000 equipped with 30 meters DB-5 capillary column with internal diameter of 0.25 mm and 0.25 μm film thickness was used. Helium was used as carried gas and gave a column head pressure of 12 p.s.i. (1 p.s.i. = 6894.76 Pa) and an average flux of 1 ml/min. The temperature program for the GC column consisted of a 4-minutes hold at 75 deg C, a 15 deg C /min ramp to 200 deg C, 8 minutes isothermal. 20 deg C/min ramp to 250 deg C, 2 minutes isothermal. The extraction of the fatty acids was based on liquid-liquid method using chloroform as solvent. The chromatograms resulted shows the presences of the oleic acid and others fatty acids identify by the mass spectra library (NIST-92). The ionization radiation deplete the fatty acids presents in the Acai oil. Details on the chemical qualitative analytical is present as well in this work. (author)

  16. Ionizing radiation effects in Acai oil analysed by gas chromatography coupled to mass spectrometry technique

    Energy Technology Data Exchange (ETDEWEB)

    Valli, Felipe; Fernandes, Carlos Eduardo; Moura, Sergio; Machado, Ana Carolina; Furasawa, Helio Akira; Pires, Maria Aparecida Faustino; Bustillos, Oscar Vega [Instituto de Pesquisas Energeticas e Nucleares (IPEN-CNEN/SP), Sao Paulo, SP (Brazil)], E-mail: ovega@ipen.br

    2007-07-01

    The Acai fruit is a well know Brazilian seed plant used in large scale as a source of feed stock, specially in the Brazilian North-east region. The Acai oil is use in many purposes from fuel sources to medicine. The scope of this paper is to analyzed the chemical structures modification of the acai oil after the ionizing radiation. The radiation were set in the range of 10 to 25 kGy in the extracted Acai oil. The analyses were made by gas chromatography coupled to mass spectrometry techniques. A GC/MS Shimatzu QP-5000 equipped with 30 meters DB-5 capillary column with internal diameter of 0.25 mm and 0.25 {mu}m film thickness was used. Helium was used as carried gas and gave a column head pressure of 12 p.s.i. (1 p.s.i. = 6894.76 Pa) and an average flux of 1 ml/min. The temperature program for the GC column consisted of a 4-minutes hold at 75 deg C, a 15 deg C /min ramp to 200 deg C, 8 minutes isothermal. 20 deg C/min ramp to 250 deg C, 2 minutes isothermal. The extraction of the fatty acids was based on liquid-liquid method using chloroform as solvent. The chromatograms resulted shows the presences of the oleic acid and others fatty acids identify by the mass spectra library (NIST-92). The ionization radiation deplete the fatty acids presents in the Acai oil. Details on the chemical qualitative analytical is present as well in this work. (author)

  17. Sulfur analysis by inductively coupled plasma-mass spectrometry: A review

    Science.gov (United States)

    Giner Martínez-Sierra, J.; Galilea San Blas, O.; Marchante Gayón, J. M.; García Alonso, J. I.

    2015-06-01

    In recent years the number of applications of sulfur (S) analysis using inductively coupled plasma mass spectrometry (ICP-MS) as detector has increased significantly. In this article we describe in some depth the application of ICP-MS for S analysis with emphasis placed on the sulfur-specific detection by hyphenated techniques such as LC, GC, CE and LA coupled on-line to ICP-MS. The different approaches available for sulfur isotope ratio measurements by ICP-MS are also detailed. Particular attention has been paid to the quantification of peptides/proteins and the analysis of metallopeptides/metalloproteins via sulfur by LC-ICP-MS. Likewise, the speciation analysis of metal-based pharmaceuticals and metallodrugs and non-metal selective detection of pharmaceuticals via S are highlighted. Labeling procedures for metabolic applications are also included. Finally, the measurement of natural variations in S isotope composition with multicollector ICP-MS instruments is also covered in this review.

  18. Determination of trace elements in serum by dynamic reaction cell inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    D' Ilio, S. [Department of Environment and Primary Prevention, Istituto Superiore di Sanita, Viale Regina Elena 299, 00161 Rome (Italy)]. E-mail: sdilio@iss.it; Violante, N. [Department of Environment and Primary Prevention, Istituto Superiore di Sanita, Viale Regina Elena 299, 00161 Rome (Italy); Caimi, S. [Department of Environment and Primary Prevention, Istituto Superiore di Sanita, Viale Regina Elena 299, 00161 Rome (Italy); Di Gregorio, M. [Department of Environment and Primary Prevention, Istituto Superiore di Sanita, Viale Regina Elena 299, 00161 Rome (Italy); Petrucci, F. [Department of Environment and Primary Prevention, Istituto Superiore di Sanita, Viale Regina Elena 299, 00161 Rome (Italy); Senofonte, O. [Department of Environment and Primary Prevention, Istituto Superiore di Sanita, Viale Regina Elena 299, 00161 Rome (Italy)

    2006-07-28

    An inductively coupled plasma mass spectrometer (ICP-MS), equipped with a dynamic reaction cell (DRC) and coupled with a desolvating nebulizing system (Apex-ACM) to reduce the oxide formation, was used in the determination of Al, Co, Cr, Mn, Ni and Se in serum samples. The effect of the operating conditions of the DRC system was studied to get the best signal-to-background (S/B) ratio. The potentially interfering molecular ions at the masses m/z {sup 27}Al, {sup 59}Co, {sup 52}Cr, {sup 55}Mn, {sup 60}Ni and {sup 78}Se, were significantly reduced in intensity by using NH{sub 3} and H{sub 2}, as the reaction cell gases in the DRC, while a proper Dynamic Bandpass Tuning parameter q (RPq) value was optimized. The detection limits for {sup 27}Al, {sup 59}Co, {sup 52}Cr, {sup 55}Mn, {sup 60}Ni and {sup 78}Se, estimated with 3-{sigma} method, resulted to be 0.14, 0.003, 0.002, 0.01, 0.01 and 1.8 {mu}g L{sup -1}, respectively. This analytical method was developed on both a human serum certified reference material and a lyophilized animal serum produced and proposed in an intercomparison study. The results obtained for the reference samples agreed satisfactorily with the certified values. Precision (expressed as CV%) between sample replicates was better than 10% for elements determination, with the only exception of aluminium (14%)

  19. Determination of trace elements in serum by dynamic reaction cell inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    An inductively coupled plasma mass spectrometer (ICP-MS), equipped with a dynamic reaction cell (DRC) and coupled with a desolvating nebulizing system (Apex-ACM) to reduce the oxide formation, was used in the determination of Al, Co, Cr, Mn, Ni and Se in serum samples. The effect of the operating conditions of the DRC system was studied to get the best signal-to-background (S/B) ratio. The potentially interfering molecular ions at the masses m/z 27Al, 59Co, 52Cr, 55Mn, 60Ni and 78Se, were significantly reduced in intensity by using NH3 and H2, as the reaction cell gases in the DRC, while a proper Dynamic Bandpass Tuning parameter q (RPq) value was optimized. The detection limits for 27Al, 59Co, 52Cr, 55Mn, 60Ni and 78Se, estimated with 3-σ method, resulted to be 0.14, 0.003, 0.002, 0.01, 0.01 and 1.8 μg L-1, respectively. This analytical method was developed on both a human serum certified reference material and a lyophilized animal serum produced and proposed in an intercomparison study. The results obtained for the reference samples agreed satisfactorily with the certified values. Precision (expressed as CV%) between sample replicates was better than 10% for elements determination, with the only exception of aluminium (14%)

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

    International Nuclear Information System (INIS)

    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 I1 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 99Tc, 129I, 230Th, 232Th, 234U, 235U, 236U, 239Pu, 240Pu and 241Am 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

  1. Normal zone detectors for a large number of inductively coupled coils

    Energy Technology Data Exchange (ETDEWEB)

    Owen, E.W.; Shimer, D.W.

    1983-01-10

    In order to protect a set of inductively coupled superconducting magnets, it is necessary to locate and measure normal zone voltages that are small compared with the mutual and self-induced voltages. The method described in this report uses two sets of voltage measurements to locate and measure one or more normal zones in any number of coupled coils. One set of voltages is the outputs of bridges that balance out the self-induced voltages The other set of voltages can be the voltages across the coils, although alternatives are possible. The two sets of equations form a single combined set of equations. Each normal zone location or combination of normal zones has a set of these combined equations associated with it. It is demonstrated that the normal zone can be located and the correct set chosen, allowing determination of the size of the normal zone. Only a few operations take plae in a working detector: multiplication of a constant, addition, and simple decision-making. In many cases the detector for each coil, although weakly linked to the other detectors, can be considered to be independent. An example of the detector design is given for four coils with realistic parameters. The effect on accuracy of changes in the system parameters is discussed.

  2. Scandium analysis in silicon-containing minerals by inductively coupled plasma tandem mass spectrometry

    Science.gov (United States)

    Whitty-Léveillé, Laurence; Drouin, Elisabeth; Constantin, Marc; Bazin, Claude; Larivière, Dominic

    2016-04-01

    This article reports on the development of a new method for the accurate and precise determination of the amount of scandium, Sc, in silicon-containing minerals, based on the use of tandem quadrupole inductively coupled plasma mass spectrometry (ICP-MS/MS). The tandem quadrupole instrument enables new mass filtering configurations, which can reduce polyatomic interferences during the determination of Sc in mineral matrices. He and O2 were used and compared as collision and reaction gases for the removal of interferences at m/z 45 and 61. Using helium gas was ineffective to overcome all of the spectral interferences observed at m/z 45 and particularly for Si-based interferences. However, conversion of Sc+ ions into ScO+ ions (after bombardment with O2 in the octopole reaction system coupled with the use of the instrument in MS/MS mass-shift mode) provided interference-free conditions and sufficiently low limits of detection, down to 3 ng L- 1, to accurately detect Sc. The accuracy of the proposed methodology was assessed by analyzing five different reference materials (BX-N, OKA-2, NIM-L, SY-3 and GH).

  3. Investigation of large-area multicoil inductively coupled plasma sources using three-dimensional fluid model

    Science.gov (United States)

    Brcka, Jozef

    2016-07-01

    A multi inductively coupled plasma (ICP) system can be used to maintain the plasma uniformity and increase the area processed by a high-density plasma. This article presents a source in two different configurations. The distributed planar multi ICP (DM-ICP) source comprises individual ICP sources that are not overlapped and produce plasma independently. Mutual coupling of the ICPs may affect the distribution of the produced plasma. The integrated multicoil ICP (IMC-ICP) source consists of four low-inductance ICP antennas that are superimposed in an azimuthal manner. The identical geometry of the ICP coils was assumed in this work. Both configurations have highly asymmetric components. A three-dimensional (3D) plasma model of the multicoil ICP configurations with asymmetric features is used to investigate the plasma characteristics in a large chamber and the operation of the sources in inert and reactive gases. The feasibility of the computational calculation, the speed, and the computational resources of the coupled multiphysics solver are investigated in the framework of a large realistic geometry and complex reaction processes. It was determined that additional variables can be used to control large-area plasmas. Both configurations can form a plasma, that azimuthally moves in a controlled manner, the so-called “sweeping mode” (SM) or “polyphase mode” (PPM), and thus they have the potential for large-area and high-density plasma applications. The operation in the azimuthal mode has the potential to adjust the plasma distribution, the reaction chemistry, and increase or modulate the production of the radicals. The intrinsic asymmetry of the individual coils and their combined operation were investigated within a source assembly primarily in argon and CO gases. Limited investigations were also performed on operation in CH4 gas. The plasma parameters and the resulting chemistry are affected by the geometrical relation between individual antennas. The aim of

  4. Investigation on elemental and isotopic fractionation during 196 nm femtosecond laser ablation multiple collector inductively coupled plasma mass spectrometry

    OpenAIRE

    Horn, I.; Friedhelm von Blanckenburg;  

    2007-01-01

    Despite the large number of successful applications of laser ablation, elemental and isotopic fractionation coupled to inductively coupled plasma mass spectrometry (ICP-MS) remain as the main limitations for many applications of this technique in the fields of analytical chemistry and Earth Sciences. A substantial effort has been made to control such fractionations, which are well-established features of nanosecond laser ablation systems. Technological advancements made over the past decade n...

  5. Development of an axially viewed inductively coupled plasma for atomic emission spectrometry and comparison between the detection limits of lead

    International Nuclear Information System (INIS)

    An ICP(Inductively Coupled plasma) emission spectrometer was developed with an axially viewed ICP source incorporated by a 5-turned induction coil and a torch, outer quartz tube of which was 50 mm longer than that used in conventional ICP/AES(Inductively Coupled Plasma Atomic Emission Spectrometry). The optimization of the system has been performed in terms of the determination of signal-to-noise ratio and background intensity at various rf powers, sample flow rates, argon gas flow rates and cut-off gas flow rates. The spectro-analytical characteristics of the spectrum obtained between 200 and 500 nm was revealed to be similar compared with a vertically viewed ICP source. The detection limit of Pb(II) at 220.35 nm was 11 ppb which was 5 times lower than that obtained with a vertically viewed ICP source. (author)

  6. Determination of platinum surface contamination in veterinary and human oncology centres using inductively coupled plasma mass spectrometry

    NARCIS (Netherlands)

    Janssens, T.; Brouwers, E. E M; de Vos, J. P.; de Vries, N.; Schellens, J. H M; Beijnen, J. H.

    2015-01-01

    The objective of this study was to determine the surface contamination with platinum-containing antineoplastic drugs in veterinary and human oncology centres. Inductively coupled plasma mass spectrometry was used to measure platinum levels in surface samples. In veterinary and human oncology centres

  7. HIGH RESOLUTION INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY ALLOWS RAPID ASSESSMENT OF IRON ABSORPTION IN INFANTS AND CHILDREN

    Science.gov (United States)

    Stable isotope absorption studies of iron have been limited by the high cost and limited availability of isotope ratio analysis using thermal ionization MS (TIMS). The development of high-resolution double focusing inductively coupled plasma MS (ICP-MS) may permit more cost-efficient sample analysis...

  8. Sector field inductively coupled plasma mass spectrometry in the elemental and isotopic analysis of lanthanides and actinides

    International Nuclear Information System (INIS)

    Plutonium is one element which is indispensable in identifying the source and for estimating the hazardous effects of rad. The isotopic ratios of plutonium (240Pu/239Pu) and its total concentration in environmental samples were also precisely estimated by high resolution inductively coupled plasma mass spectrometry

  9. A comparison of neutron activation analysis and inductively coupled plasma mass spectrometry for trace element analysis of biological materials

    International Nuclear Information System (INIS)

    Fifty individual food types were analysed by instrumental and radiochemical neutron activation analysis as well as inductively coupled plasma mass spectrometry after testing all techniques by analysing IAEA mixed human diet, H-9. The performance of these trace element techniques and their limitations were evaluated under normal, routine, multielement surveys of a large range of solid biological materials. (author) 18 refs.; 2 tabs

  10. 40 CFR Appendix C to Part 136 - Inductively Coupled Plasma-Atomic Emission Spectrometric Method for Trace Element Analysis of...

    Science.gov (United States)

    2010-07-01

    ... absorption spectrometry, or other approved methodology. 5.2.4Wavelength scanning of analyte line region. If..., Publication No. 77-206, August 1977. 14.8“OSHA Safety and Health Standards, General Industry,” (29 CFR part... 40 Protection of Environment 22 2010-07-01 2010-07-01 false Inductively Coupled...

  11. On-line coupling of size exclusion chromatography with mixed-mode liquid chromatography for comprehensive profiling of biopharmaceutical drug product.

    Science.gov (United States)

    He, Yan; Friese, Olga V; Schlittler, Michele R; Wang, Qian; Yang, Xun; Bass, Laura A; Jones, Michael T

    2012-11-01

    A methodology based on on-line coupling of size exclusion chromatography (SEC) with mixed-mode liquid chromatography (LC) has been developed. The method allows for simultaneous measurement of a wide range of components in biopharmaceutical drug products. These components include the active pharmaceutical ingredient (protein) and various kinds of excipients such as cations, anions, nonionic hydrophobic surfactant and hydrophilic sugars. Dual short SEC columns are used to separate small molecule excipients from large protein molecules. The separated protein is quantified using a UV detector at 280 nm. The isolated excipients are switched, online, to the Trinity P1 mixed-mode column for separation, and detected by an evaporative light scattering detector (ELSD). Using a stationary phase with 1.7 μm particles in SEC allows for the use of volatile buffers for both SEC and mix-mode separation. This facilitates the detection of different excipients by ELSD and provides potential for online characterization of the protein with mass spectrometry (MS). The method has been applied to quantitate protein and excipients in different biopharmaceutical drug products including monoclonal antibodies (mAb), antibody drug conjugates (ADC) and vaccines. PMID:22999205

  12. Detection of radiation-induced hydrocarbons in irradiated fish and prawns by means of on-line coupled liquid chromatography-gas chromatography

    International Nuclear Information System (INIS)

    Radiation-induced hydrocarbons were analyzed in a fatty (halibut) and a lean fish (cod) as well as in a prawn species by on-line coupled liquid chromatography (LC) -gas chromatography (GC) combined with mass spectrometry. In irradiated halibut which is known to contain mainly saturated and monounsaturated fatty acids, all expected radiolytic alkanes, alkenes, and alkadienes could be detected. The yields of the C(n-1) and C(n-2:1) hydrocarbons were comparable to those found in irradiated lipids of terrestrial animals and plants. However, in cod and prawns which contain high levels of polyunsaturated fatty acids (PUFA), the C(n-1) hydrocarbons were found in concentrations which were up to 10 times higher whereas the C(n-2:1) products were again comparable to those of terrestrial animals and plants. The identification of radiation-induced hydrocarbons in fish lipids was achieved by transfer of the hydrocarbons from the LC column to the gas chromatographic column in fractions differing in their degree of unsaturation. For the first time, radiation-induced hydrocarbons with more than four double bonds generated from polyunsaturated fatty acids (20:4 omega 6 and 20:5 omega 3) could be identified

  13. [Rapid determination of pesticide multiresidues in vegetables and fruits by accelerated solvent extraction coupled with online gel permeation chromatography-gas chromatography-mass spectrometry].

    Science.gov (United States)

    Ouyang, Yunfu; Tang, Hongbing; Wu, Ying; Li, Guiying

    2012-07-01

    A novel method was developed for the rapid determination of 22 representative pesticide residues in vegetables and fruits based on accelerated solvent extraction (ASE) coupled with online gel permeation chromatography-gas chromatography-mass spectrometry (GPC-GC-MS). The sample was extracted by accelerated solvent extraction with dichloromethane-acetone (1:1, v/v) and purified with a carbon/NH2 column, evaporated to dryness by nitrogen, then dissolved in cyclohexane-acetone (7:3, v/v), and finally identified and quantified by GPC-GC-MS system in selected ion monitoring (SIM) mode. The results showed that the linearities of the 22 pesticides were good in their linear ranges. The limits of detection (S/N = 3) were 0.3-1.8 microg/kg. The limits of quantification (S/N = 10) ranged from 1-6 microg/kg. The recoveries for all at three spiked levels in Chinese cabbages and apples ranged from 70.5% to 107.5% with the relative standard deviations (RSDs) of 2.1%-8.7%. The proposed method is accurate, sensitive and highly efficient in the extraction, and can be used for the quick determination of the pesticide multiresidues in vegetables and fruits. PMID:23189658

  14. Headspace-solid phase microextraction coupled to gas chromatography-combustion-isotope ratio mass spectrometer and to enantioselective gas chromatography for strawberry flavoured food quality control.

    Science.gov (United States)

    Schipilliti, Luisa; Dugo, Paola; Bonaccorsi, Ivana; Mondello, Luigi

    2011-10-21

    Authenticity assessment of flavoured strawberry foods was performed using headspace-solid phase microextraction (HS-SPME) coupled to gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS). An authenticity range was achieved, investigating on the carbon isotope ratio of numerous selected aroma active volatile components (methyl butanoate, ethyl butanoate, hex-(2E)-enal, methyl hexanoate, buthyl butanoate, ethyl hexanoate, hexyl acetate, linalool, hexyl butanoate, octyl isovalerate, γ-decalactone and octyl hexanoate) of organic Italian fresh strawberries. To the author's knowledge, this is the first time that all these components were investigated simultaneously by GC-C-IRMS on the same sample. The results were compared, when applicable, with those obtained by analyzing the HS-SPME extracts of commercial flavoured food matrices. In addition, one Kenyan pineapple and one fresh Italian peach were analyzed to determine the δ(13)C(VPDB) of the volatile components common to strawberry. The δ(13)C(VPDB) values are allowed to differentiate between different biogenetic pathways (C(3) and CAM plants) and more interestingly between plants of the same CO(2) fixation group (C(3) plants). Additional analyses were performed on all the samples by means of Enantioselective Gas Chromatography (Es-GC), measuring the enantiomeric distribution of linalool and γ-decalactone. It was found that GC-C-IRMS and Es-GC measurements were in agreement to detect the presence of non-natural strawberry aromas in the food matrices studied. PMID:21872872

  15. Computational hydrodynamics and optical performance of inductively-coupled plasma adaptive lenses

    Energy Technology Data Exchange (ETDEWEB)

    Mortazavi, M.; Urzay, J., E-mail: jurzay@stanford.edu; Mani, A. [Center for Turbulence Research, Stanford University, Stanford, California 94305-3024 (United States)

    2015-06-15

    This study addresses the optical performance of a plasma adaptive lens for aero-optical applications by using both axisymmetric and three-dimensional numerical simulations. Plasma adaptive lenses are based on the effects of free electrons on the phase velocity of incident light, which, in theory, can be used as a phase-conjugation mechanism. A closed cylindrical chamber filled with Argon plasma is used as a model lens into which a beam of light is launched. The plasma is sustained by applying a radio-frequency electric current through a coil that envelops the chamber. Four different operating conditions, ranging from low to high powers and induction frequencies, are employed in the simulations. The numerical simulations reveal complex hydrodynamic phenomena related to buoyant and electromagnetic laminar transport, which generate, respectively, large recirculating cells and wall-normal compression stresses in the form of local stagnation-point flows. In the axisymmetric simulations, the plasma motion is coupled with near-wall axial striations in the electron-density field, some of which propagate in the form of low-frequency traveling disturbances adjacent to vortical quadrupoles that are reminiscent of Taylor-Görtler flow structures in centrifugally unstable flows. Although the refractive-index fields obtained from axisymmetric simulations lead to smooth beam wavefronts, they are found to be unstable to azimuthal disturbances in three of the four three-dimensional cases considered. The azimuthal striations are optically detrimental, since they produce high-order angular aberrations that account for most of the beam wavefront error. A fourth case is computed at high input power and high induction frequency, which displays the best optical properties among all the three-dimensional simulations considered. In particular, the increase in induction frequency prevents local thermalization and leads to an axisymmetric distribution of electrons even after introduction of

  16. Computational hydrodynamics and optical performance of inductively-coupled plasma adaptive lenses

    International Nuclear Information System (INIS)

    This study addresses the optical performance of a plasma adaptive lens for aero-optical applications by using both axisymmetric and three-dimensional numerical simulations. Plasma adaptive lenses are based on the effects of free electrons on the phase velocity of incident light, which, in theory, can be used as a phase-conjugation mechanism. A closed cylindrical chamber filled with Argon plasma is used as a model lens into which a beam of light is launched. The plasma is sustained by applying a radio-frequency electric current through a coil that envelops the chamber. Four different operating conditions, ranging from low to high powers and induction frequencies, are employed in the simulations. The numerical simulations reveal complex hydrodynamic phenomena related to buoyant and electromagnetic laminar transport, which generate, respectively, large recirculating cells and wall-normal compression stresses in the form of local stagnation-point flows. In the axisymmetric simulations, the plasma motion is coupled with near-wall axial striations in the electron-density field, some of which propagate in the form of low-frequency traveling disturbances adjacent to vortical quadrupoles that are reminiscent of Taylor-Görtler flow structures in centrifugally unstable flows. Although the refractive-index fields obtained from axisymmetric simulations lead to smooth beam wavefronts, they are found to be unstable to azimuthal disturbances in three of the four three-dimensional cases considered. The azimuthal striations are optically detrimental, since they produce high-order angular aberrations that account for most of the beam wavefront error. A fourth case is computed at high input power and high induction frequency, which displays the best optical properties among all the three-dimensional simulations considered. In particular, the increase in induction frequency prevents local thermalization and leads to an axisymmetric distribution of electrons even after introduction of

  17. Computational hydrodynamics and optical performance of inductively-coupled plasma adaptive lenses

    Science.gov (United States)

    Mortazavi, M.; Urzay, J.; Mani, A.

    2015-06-01

    This study addresses the optical performance of a plasma adaptive lens for aero-optical applications by using both axisymmetric and three-dimensional numerical simulations. Plasma adaptive lenses are based on the effects of free electrons on the phase velocity of incident light, which, in theory, can be used as a phase-conjugation mechanism. A closed cylindrical chamber filled with Argon plasma is used as a model lens into which a beam of light is launched. The plasma is sustained by applying a radio-frequency electric current through a coil that envelops the chamber. Four different operating conditions, ranging from low to high powers and induction frequencies, are employed in the simulations. The numerical simulations reveal complex hydrodynamic phenomena related to buoyant and electromagnetic laminar transport, which generate, respectively, large recirculating cells and wall-normal compression stresses in the form of local stagnation-point flows. In the axisymmetric simulations, the plasma motion is coupled with near-wall axial striations in the electron-density field, some of which propagate in the form of low-frequency traveling disturbances adjacent to vortical quadrupoles that are reminiscent of Taylor-Görtler flow structures in centrifugally unstable flows. Although the refractive-index fields obtained from axisymmetric simulations lead to smooth beam wavefronts, they are found to be unstable to azimuthal disturbances in three of the four three-dimensional cases considered. The azimuthal striations are optically detrimental, since they produce high-order angular aberrations that account for most of the beam wavefront error. A fourth case is computed at high input power and high induction frequency, which displays the best optical properties among all the three-dimensional simulations considered. In particular, the increase in induction frequency prevents local thermalization and leads to an axisymmetric distribution of electrons even after introduction of

  18. Relative Quantification of Sites of Peptide and Protein Modification Using Size Exclusion Chromatography Coupled with Electron Transfer Dissociation

    Science.gov (United States)

    Xie, Boer; Sharp, Joshua S.

    2016-08-01

    One difficult problem in the analysis of peptide modifications is quantifying isomeric modifications that differ by the position of the amino acid modified. HPLC separation using C18 reverse phase chromatography coupled with electron transfer dissociation (ETD) in tandem mass spectrometry has recently been shown to be able to relatively quantify how much of a given modification occurs at each amino acid position for isomeric mixtures; however, the resolution of reverse phase chromatography greatly complicates quantification of isomeric modifications by ETD because of the chromatographic separation of peptides with identical modifications at different sequence positions. Using peptide oxidation as a model system, we investigated the use of size exclusion chromatography coupled with ETD fragmentation to separate peptide sequences. This approach allows for the benefits of chromatographic separation of peptide sequences while ensuring co-elution of modification isomers for accurate relative quantification of modifications using standard data-dependent acquisitions. Using this method, the relative amount of modification at each amino acid can be accurately measured from single ETD MS/MS spectra in a standard data-dependent acquisition experiment.

  19. Relative Quantification of Sites of Peptide and Protein Modification Using Size Exclusion Chromatography Coupled with Electron Transfer Dissociation.

    Science.gov (United States)

    Xie, Boer; Sharp, Joshua S

    2016-08-01

    One difficult problem in the analysis of peptide modifications is quantifying isomeric modifications that differ by the position of the amino acid modified. HPLC separation using C18 reverse phase chromatography coupled with electron transfer dissociation (ETD) in tandem mass spectrometry has recently been shown to be able to relatively quantify how much of a given modification occurs at each amino acid position for isomeric mixtures; however, the resolution of reverse phase chromatography greatly complicates quantification of isomeric modifications by ETD because of the chromatographic separation of peptides with identical modifications at different sequence positions. Using peptide oxidation as a model system, we investigated the use of size exclusion chromatography coupled with ETD fragmentation to separate peptide sequences. This approach allows for the benefits of chromatographic separation of peptide sequences while ensuring co-elution of modification isomers for accurate relative quantification of modifications using standard data-dependent acquisitions. Using this method, the relative amount of modification at each amino acid can be accurately measured from single ETD MS/MS spectra in a standard data-dependent acquisition experiment. Graphical Abstract ᅟ. PMID:27075875

  20. Comparative analysis of steroidal saponins in four Dioscoreae herbs by high performance liquid chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Guo, Long; Zeng, Su-Ling; Zhang, Yu; Li, Ping; Liu, E-Hu

    2016-01-01

    Steroidal saponins, which exhibit multiple pharmacological effects, are the major bioactive constituents in herbal medicines from Dioscoreae species. In this study, a sensitive method based on high performance liquid chromatography-mass spectrometry (HPLC-MS) was established and validated for qualitative and quantitative analysis of steroidal saponins in four Dioscoreae herbs including Dioscoreae Nipponica Rhizome (DNR) and Dioscoreae Hypoglaucae Rhizome (DHR), Dioscoreae Spongiosae Rhizome (DSR) and Dioscoreae Rhizome (DR). A total of eleven steroidal saponins were identified by high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-QTOF/MS). Furthermore, seven major steroidal saponins was simultaneous quantified using a high performance liquid chromatography coupled with triple quadrupole mass spectrometry (HPLC-QQQ/MS). The qualitative and quantitative analysis results indicated that the chemical composition of DNR, DHR and DSR samples exhibited a high level of global similarity, while the ingredients in DR varied greatly from the other three herbs. Moreover, principal component analysis (PCA) and hierarchical clustering analysis (HCA) were performed to compare and discriminate the Dioscoreae herbs based on the quantitative data. The results demonstrated the qualitative and quantitative analysis of steroidal saponins based on HPLC-MS is a feasible method for quality control of Dioscoreae herbs. PMID:26344383

  1. Inductively coupled plasma-atomic emission spectroscopy glovebox assembly system at the West Valley Demonstration Project

    International Nuclear Information System (INIS)

    The inductively coupled plasma/atomic emission spectroscopy [ICP/AES (ICP)] system for elemental analyses in support of vitrification processing was first installed in 1986. The initial instrument was a Jobin Yvon (JY) Model JY-70 ICP that consisted of sequential and simultaneous spectrometers for analysis of nonradioactive samples as radioactive surrogates. The JY-70 ICP continued supporting nonradioactive testing during the Functional and Checkout Testing of Systems (FACTS) using the full-scale melter with ''cold'' (nonradioactive) testing campaigns. As a result, the need for another system was identified to allow for the analysis of radioactive samples. The Mass Spec (Spectrometry) Lab was established for the installation of the modified ICP system for handling radioactive samples. The conceptual setup of another ICP was predicated on the use of a hood to allow ease of accessibility of the torch, nebulizer, and spray chamber, and the minimization of air flow paths. However, reconsideration of the radioactive sample dose rate and contamination levels led to the configuration of the glovebox system with a common transfer interface box for the ICP and the inductively coupled plasma-mass spectrometer (ICP-MS) glovebox assemblies. As a result, a simultaneous Model JY-50P ICP with glovebox was installed in 1990 as a first generation ICP glovebox system. This was one of the first ICP glovebox assemblies connected with an ICP-MS glovebox system. Since the economics of processing high-level radioactive waste (HLW) required the availability of an instrument to operate 24 hours a day throughout the year without any downtime, a second generation ICP glovebox assembly was designed, manufactured, and installed in 1995 using a Model JY-46P ICP. These two ICP glovebox systems continue to support vitrification of the HLW into canisters for storage. The ICP systems have been instrumental in monitoring vitrification batch processing. To date, remote sample preparation and

  2. Dispersive liquid-liquid microextraction coupled to liquid chromatography for thiamine determination in foods.

    Science.gov (United States)

    Viñas, Pilar; López-García, Ignacio; Bravo-Bravo, María; Briceño, Marisol; Hernández-Córdoba, Manuel

    2012-05-01

    A miniaturized dispersive liquid-liquid microextraction (DLLME) procedure coupled to liquid chromatography (LC) with fluorimetric detection was evaluated for the preconcentration and determination of thiamine (vitamin B(1)). Derivatization was carried out by chemical oxidation of thiamine with 5 × 10(-5) M ferricyanide at pH 13 to form fluorescent thiochrome. For DLLME, 0.5 mL of acetonitrile (dispersing solvent) containing 90 μL of tetrachloroethane (extraction solvent) was rapidly injected into 10 mL of sample solution containing the derivatized thiochrome and 24% (w/v) sodium chloride, thereby forming a cloudy solution. Phase separation was carried out by centrifugation, and a volume of 20 μL of the sedimented phase was submitted to LC. The mobile phase was a mixture of a 90% (v/v) 10 mM KH(2)PO(4) (pH 7) solution and 10% (v/v) acetonitrile at 1 mL min(-1). An amide-based stationary phase involving a ligand with amide groups and the endcapping of trimethylsilyl was used. Specificity, linearity, precision, recovery, and sensitivity were satisfactory. Calibration graph was carried out by the standard additions method and was linear between 1 and 10 ng mL(-1). The detection limit was 0.09 ng mL(-1). The selectivity of the method was judged from the absence of interfering peaks at the thiamine elution time for blank chromatograms of unspiked samples. A relative standard deviation of 3.2% was obtained for a standard solution containing thiamine at 5 ng mL(-1). The esters thiamine monophosphate and thiamine pyrophosphate can also be determined by submitting the sample to successive acid and enzymatic treatments. The method was applied to the determination of thiamine in different foods such as beer, brewer's yeast, honey, and baby foods including infant formulas, fermented milk, cereals, and purees. For the analysis of solid samples, a previous extraction step was applied based on an acid hydrolysis with trichloroacetic acid. The reliability of the procedure was

  3. RAPID DETERMINATION OF ACTINIDES IN URINE BY INDUCTIVELY-COUPLED PLASMA MASS SPECTROMETRY AND ALPHA SPECTROMETRY: A HYBRID APPROACH

    Energy Technology Data Exchange (ETDEWEB)

    Maxwell, S.; Jones, V.

    2009-05-27

    A new rapid separation method that allows separation and preconcentration of actinides in urine samples was developed for the measurement of longer lived actinides by inductively coupled plasma mass spectrometry (ICP-MS) and short-lived actinides by alpha spectrometry; a hybrid approach. This method uses stacked extraction chromatography cartridges and vacuum box technology to facilitate rapid separations. Preconcentration, if required, is performed using a streamlined calcium phosphate precipitation. Similar technology has been applied to separate actinides prior to measurement by alpha spectrometry, but this new method has been developed with elution reagents now compatible with ICP-MS as well. Purified solutions are split between ICP-MS and alpha spectrometry so that long- and short-lived actinide isotopes can be measured successfully. The method allows for simultaneous extraction of 24 samples (including QC samples) in less than 3 h. Simultaneous sample preparation can offer significant time savings over sequential sample preparation. For example, sequential sample preparation of 24 samples taking just 15 min each requires 6 h to complete. The simplicity and speed of this new method makes it attractive for radiological emergency response. If preconcentration is applied, the method is applicable to larger sample aliquots for occupational exposures as well. The chemical recoveries are typically greater than 90%, in contrast to other reported methods using flow injection separation techniques for urine samples where plutonium yields were 70-80%. This method allows measurement of both long-lived and short-lived actinide isotopes. 239Pu, 242Pu, 237Np, 243Am, 234U, 235U and 238U were measured by ICP-MS, while 236Pu, 238Pu, 239Pu, 241Am, 243Am and 244Cm were measured by alpha spectrometry. The method can also be adapted so that the separation of uranium isotopes for assay is not required, if uranium assay by direct dilution of the urine sample is preferred instead

  4. Measurement of the isotopic abundance of boron-10 by inductively coupled plasma-quadrupole mass spectrometry

    International Nuclear Information System (INIS)

    This article describes the method for measuring the isotopic abundance of 10B in nuclear grade boron carbide using inductively coupled plasma-quadrupole mass spectrometry (ICP-QMS). The results of investigation revealed that both the integration time and the dwell time have a major influence on the reproducibility of ICP-QMS measurements. As a result of optimization of the measurement conditions, reproducibility below 0.2% relative standard deviation (RSD) (0.17% RSD maximum) was achieved. In addition, the measured value of the isotopic abundance of 10B for each sample well agreed with the values measured by the TIMS. Thus, the method described in the present investigation was very effective in the analysis of isotopic abundance of 10B in B4C or H3BO3. The results of this study suggest that ICP-QMS could be applied to the precise analysis of the isotopic abundance of 10B required in the field of nuclear applications. (author)

  5. 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.

  6. Macro-loading Effects in Inductively Coupled Plasma Etched Mercury Cadmium Telluride

    Science.gov (United States)

    Apte, Palash; Rybnicek, Kimon; Stoltz, Andrew

    2016-09-01

    This paper reports the effect of macro-loading on mercury cadmium telluride (Hg1- x Cd x Te) and Photoresist (PR) etched in an inductively coupled plasma (ICP). A significant macro-loading effect is observed, which affects the etch rates of both PR and Hg1- x Cd x Te. It is observed that the exposed silicon area has a significant effect on the PR etch rate, but not on the Hg1- x Cd x Te etch rate. It is also observed that the exposed Hg1- x Cd x Te area has a significant effect on the etch rate of the PR, but the exposed PR area does not seem to have an effect on the Hg1- x Cd x Te etch rate. Further, the exposed Hg1- x Cd x Te area is shown to affect the etch rate of the Hg1- x Cd x Te, but there does not seem to be a similar effect for the exposed PR area on the etch rate of the PR. Since the macro-loading affects the selectivity significantly, this effect can cause significant problems in the etching of deep trenches. A few techniques to reduce the effect of macro-loading on the etch rates of the PR and Hg1- x Cd x Te are listed, herein.

  7. EVALUATION OF CORROSION OF ENGINEERING CERAMICS BY ATOMIC EMISSION SPECTROMETRY IN INDUCTIVELY COUPLED PLASMA

    Directory of Open Access Journals (Sweden)

    DAGMAR GALUSKOVÁ

    2014-03-01

    Full Text Available An analytical method has been developed and verified, facilitating chemical analysis of saline aqueous solutions from corrosion tests of two types of engineering ceramics, i.e. polycrystalline alumina, and silicon nitride. The method is capable of providing complementary information related to mechanisms of corrosion and kinetics of dissolution of the two main components of the ceramics, i.e. Al in α-Al2O3, and Si in Si3N4. A radially viewed inductively coupled plasma atomic emission spectroscopy was used, and the operating conditions for the analysis were optimised. The method was validated. Internal standardisation, matrix matching, standard addition technique and direct measurement without matrix correction were applied, and the results were critically discussed. The technique of internal standard was shown to be the most sensitive. The method exhibited satisfactory precision (relative standard deviation up to 5 %, analytical recoveries from 95 to 100 %, and acceptable limits of detection based on 3σ criterion of 0.095 mg∙l-1 for Al (measured at 308.215 nm and 0.099 mg∙l-1 for Si (at 251.611 nm.

  8. Inductively coupled plasma mass spectrometer with laser ablation metal ions release detection in the human mouth

    Science.gov (United States)

    Kueerova, Hana; Dostalova, Tatjana; Prochazkova, J.

    2002-06-01

    Presence of more dental alloys in oral cavity often causes pathological symptoms. Due to various and multi-faced symptomatology, they tend to be a source of significant problems not only for the patient but also for the dentist. Metal ions released from alloys can cause subjective and objective symptoms in mouth. The aim of this study was detection of metal elements presence in saliva. There were 4 groups of examined persons: with intact teeth (15 individuals) with metallic restorations, pathological currents 5-30 (mu) A, multi-faced subjective symptomatology and uncharacteristic objective diagnosis (32 patients), with metallic restorations and no subjective symptoms (14 persons) and with metallic restorations, without pathological currents and with problems related to galvanism (13 patients). Presence of 14 metal elements was checked by inductively coupled plasma mass spectrometer with laser ablation. Nd:YAG laser detector was used. There were significant differences in content of silver, gold and mercury between persons with intact teeth and other three groups. There were no differences found between subjects with and without galvanic currents, and presence of subjective and objective symptoms.

  9. Thin film passivation of organic light emitting diodes by inductively coupled plasma chemical vapor deposition

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Han-Ki [Department of Information and Nano Materials Engineering, Kumoh National Institute of Technology (KIT), 1 Yangho-dong, Gumi, Gyeongbuk, 730-701 (Korea, Republic of)]. E-mail: hkkim@kumoh.ac.kr; Kim, Sang-Woo [Department of Information and Nano Materials Engineering, Kumoh National Institute of Technology (KIT), 1 Yangho-dong, Gumi, Gyeongbuk, 730-701 (Korea, Republic of); Kim, Do-Geun [Surface Technology Research Center, Korea Institute of Machinery and Materials, 66 Sangnam-dong, Changwon-si, Gyeongnam, 641-831 (Korea, Republic of); Kang, Jae-Wook [Organic Light Emitting Diodes (OLED) Center, Seoul National University, Silim-dong, Seoul 151-741 (Korea, Republic of); Kim, Myung Soo [Core Technology Laboratory, Samsung SDI, Co., LTD., 575 Shin-dong, Youngtong-Gu, Suwon, Gyeonggi-Do, 442-391 (Korea, Republic of); Cho, Woon Jo [Nano Device Research Center, Korea Institute of Science and Technology, 39-1, Haweolgok-Dong, Seongbuk-Gu, Seoul, 136-791 (Korea, Republic of)

    2007-04-09

    The characteristics of an SiN {sub x} passivation layer grown by a specially designed inductively coupled plasma chemical vapor deposition (ICP-CVD) system with straight antennas for the top-emitting organic light emitting diodes (TOLEDs) are investigated. Using a high-density plasma on the order of {approx} 10{sup 11} electrons/cm{sup 3} formed by nine straight antennas connected in parallel, a high-density SiN {sub x} passivation layer was deposited on a transparent Mg-Ag cathode at a substrate temperature of 40 deg. C. Even at a low substrate temperature, single SiN {sub x} passivation layer prepared by ICP-CVD showed a low water vapor transmission rate of 5 x 10{sup -2} g/m{sup 2}/day and a transparency of {approx} 85% respectively. In addition, current-voltage-luminescence results of the TOLED passivated by the SiN {sub x} layer indicated that the electrical and optical properties of the TOLED were not affected by the high-density plasma during the SiN {sub x} deposition process.

  10. Interlaboratory comparison for boron isotope ratio measurement with inductively coupled plasma-quadrupole mass spectrometer

    International Nuclear Information System (INIS)

    Boron isotope ratios were analyzed in seven domestic analytical labs for boric acid solutions with various compositions of boron isotope abundances, using an Inductively Coupled Plasma-Quadrupole Mass Spectrometer (ICP-QMS). Five sample solutions with different isotope abundances of 10B were prepared in the range of 10 to 20 % by mixing two boric acid solutions containing natural B and enriched 11B, respectively. Then, the 10B isotope abundances of each sample were certified by analyzing with thermal ionization mass spectrometry (TI-MS) according to ASTM-C791-04. Results obtained from each lab have indicated good coincidences with TI-MS results. Also, the relative standard deviations of results with ICP-QMS of seven analytical labs were 0.11 to 0.81 %. The measurement precision for ICP-QMS would be sufficient in terms of practical use, while taking into consideration a valid requirement required for verifying a depletion of the 10B isotope abundance in the PWR coolant, while this is greater than a nominal analytical error (relative value : 0.22 %) for TI-MS shown in ASTM-C791-04. (author)

  11. External control of electron energy distributions in a dual tandem inductively coupled plasma

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Lei; Sridhar, Shyam; Zhu, Weiye; Donnelly, Vincent M., E-mail: vmdonnelly@uh.edu; Economou, Demetre J., E-mail: economou@uh.edu [Plasma Processing Laboratory, Department of Chemical and Biomolecular Engineering, University of Houston, Houston, Texas 77204-4004 (United States); Logue, Michael D.; Kushner, Mark J., E-mail: mjkush@umich.edu [Department of Electrical Engineering and Computer Science, University of Michigan, Ann Arbor, Michigan 48109-2122 (United States)

    2015-08-28

    The control of electron energy probability functions (EEPFs) in low pressure partially ionized plasmas is typically accomplished through the format of the applied power. For example, through the use of pulse power, the EEPF can be modulated to produce shapes not possible under continuous wave excitation. This technique uses internal control. In this paper, we discuss a method for external control of EEPFs by transport of electrons between separately powered inductively coupled plasmas (ICPs). The reactor incorporates dual ICP sources (main and auxiliary) in a tandem geometry whose plasma volumes are separated by a grid. The auxiliary ICP is continuously powered while the main ICP is pulsed. Langmuir probe measurements of the EEPFs during the afterglow of the main ICP suggests that transport of hot electrons from the auxiliary plasma provided what is effectively an external source of energetic electrons. The tail of the EEPF and bulk electron temperature were then elevated in the afterglow of the main ICP by this external source of power. Results from a computer simulation for the evolution of the EEPFs concur with measured trends.

  12. Wireless thin film transistor based on micro magnetic induction coupling antenna.

    Science.gov (United States)

    Jun, Byoung Ok; Lee, Gwang Jun; Kang, Jong Gu; Kim, Seunguk; Choi, Ji-Woong; Cha, Seung Nam; Sohn, Jung Inn; Jang, Jae Eun

    2015-01-01

    A wireless thin film transistor (TFT) structure in which a source/drain or a gate is connected directly to a micro antenna to receive or transmit signals or power can be an important building block, acting as an electrical switch, a rectifier or an amplifier, for various electronics as well as microelectronics, since it allows simple connection with other devices, unlike conventional wire connections. An amorphous indium gallium zinc oxide (α-IGZO) TFT with magnetic antenna structure was fabricated and studied for this purpose. To enhance the induction coupling efficiency while maintaining the same small antenna size, a magnetic core structure consisting of Ni and nanowires was formed under the antenna. With the micro-antenna connected to a source/drain or a gate of the TFT, working electrical signals were well controlled. The results demonstrated the device as an alternative solution to existing wire connections which cause a number of problems in various fields such as flexible/wearable devices, body implanted devices, micro/nano robots, and sensors for the 'internet of things' (IoT). PMID:26691929

  13. Optimization of operating parameters for inductively coupled plasma mass spectrometry: A computational study

    Science.gov (United States)

    Aghaei, Maryam; Lindner, Helmut; Bogaerts, Annemie

    2012-10-01

    An inductively coupled plasma, connected to a mass spectrometer interface, is computationally investigated. The effect of pressure behind the sampler, injector gas flow rate, auxiliary gas flow rate, and applied power is studied. There seems to be an optimum range of injector gas flow rate for each setup which guaranties the presence and also a proper length of the central channel in the torch. Moreover, our modeling results show that for any specific purpose, it is possible to control that either only the central gas flow passes through the sampler orifice or that it is accompanied by the auxiliary gas flow. It was also found that depending on geometry, the variation of outgoing gas flow rate is much less than the variation of the injector gas flow rate and this causes a slightly higher pressure inside the torch. The general effect of increasing the applied power is a rise in the plasma temperature, which results in a higher ionization in the coil region. However, the negative effect is reducing the length of the cool central channel which is important to transfer the sample substances to the sampler. Using a proper applied power can enhance the efficiency of the system. Indeed, by changing the gas path lines, the power can control which flow (i.e., only from injector gas or also from the auxiliary gas) goes to the sampler orifice. Finally, as also reported from experiments in literature, the pressure behind the sampler has no dramatic effect on the plasma characteristics.

  14. Damage in etching of (Ba, Sr)TiO3 thin films using inductively coupled plasma

    International Nuclear Information System (INIS)

    High dielectric (Ba, Sr)TiO3 thin films were etched in an inductively coupled plasma as a function of the Cl2/Ar gas mixing ratio. Under Cl2 (20)/Ar (80), the maximum etch rate of the BST film was 400 Aa/min and the selectivities of BST to Pt and PR obtained were 0.4 and 0.2, respectively. Etching by-products remained on the surface of BST and resulted in varying the stochiometry. Therefore, we investigated the surface of the etched BST using x-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), and x-ray diffraction (XRD). From the results of XPS analysis, we found that metal (Ba or Sr) chloride compounds remained on the surface of the etched BST for high boiling points. The morphology of the etched surface was evaluated with AFM. The surface roughness decreased as the Cl2 increased in the Cl2/Ar plasma. From the results of XRD analysis, the crystallinity of etched BST films under Ar only and under Cl2 (20)/Ar (80) was similar to that of as-deposited BST. However, the (100) diffraction peak abruptly decreased at the Cl2 only plasma. It was assumed that metal (Ba or Sr) chloride compounds remained on the etched BST surface and changed the stoichiometry, resulting in crystallinity of the BST film during the etch process

  15. Determination of selenium in blood serum by inductively coupled plasma atomic emission spectrometry with pneumatic nebulization

    Energy Technology Data Exchange (ETDEWEB)

    Machat, Jiri; Kanicky, Viktor; Otruba, Vitezslav [Laboratory of Plasma Sources for Chemical Analysis-Laboratory of Atomic Spectrochemistry, Faculty of Science, Masaryk University Brno (Czech Republic)

    2002-02-01

    The possibility of determining selenium in blood serum using inductively coupled plasma emission spectrometry with conventional pneumatic nebulization was studied. A high-resolution spectrometer (SBW=6 pm) with laterally viewed ICP was employed. Analysis with conventional pneumatic nebulization could overcome laborious and demanding digestion, which is necessary for hydride generation. A pressure digestion with nitric acid at 160 C was sufficient to decrease the carbon content in the serum sample to 5%-10% of its original value. Spectral interference of the CN band was observed and mathematically corrected. It was found that the carbon-induced selenium line emission enhancement occurred even under ICP optimized conditions. A method of determination was developed and applied to the analysis of blood serum. True limit of detection in real samples is 0.01-0.02 mg/L and the limit of quantification (RSD 10%) is 0.03-0.07 mg/L using Se I 196.090 nm line at an integration time of 10-2 s. The method was tested by analysis of porcine blood serum and the serum reference material Seronorm MI 0181. (orig.)

  16. Synthesis of ultrafine particles and processing of nano-structured films with inductively coupled plasma

    International Nuclear Information System (INIS)

    The inductively coupled plasma (ICP) at atmospheric pressure is particularly suited for melting and evaporation of materials. The electrodeless ICP can be generated without limitation of the kind of plasma forming gases. Therefore, using an argon-oxygen gas mixture as sheath gas of the ICP nanoparticles can be processed by combustion of metal-organic liquid precursors injected in the hot plasma core. By this way, nanoparticles of alumina, titania and of a perovskite type oxide are produced. The powder particles are collected by an electrostatic filter. They are characterized by a log-normal size distribution with a median diameter of about 10 nm depending on the plasma parameters used. Interesting metastable phases and exactly doped, very pure materials can be obtained. Nanophase coatings synthesized by the ICP are made from the same precursor materials. For depositions, the plasma jet has to be supersonic. Impinging onto the substrate placed near the nozzle thin and dense coatings are obtained. The composition and the grain size of as-deposited coatings are analyzed by XRD. (author)

  17. Surface roughening of ground fused silica processed by atmospheric inductively coupled plasma

    Science.gov (United States)

    Xin, Qiang; Li, Na; Wang, Jun; Wang, Bo; Li, Guo; Ding, Fei; Jin, Huiliang

    2015-06-01

    Subsurface damage (SSD) is a defect that is inevitably induced during mechanical processes, such as grinding and polishing. This defect dramatically reduces the mechanical strength and the laser damage thresholds of optical elements. Compared with traditional mechanical machining, atmospheric pressure plasma processing (APPP) is a relatively novel technology that induces almost no SSD during the processing of silica-based optical materials. In this paper, a form of APPP, inductively coupled plasma (ICP), is used to process fused silica substrates with fluorocarbon precursor under atmospheric pressure. The surface morphology evolution of ICP-processed substrates was observed and characterized by confocal laser scanning microscope (CLSM), field emission scanning electron microscope (SEM), and atomic force microscopy (AFM). The results show that the roughness evolves with the etching depth, and the roughness evolution is a single-peaked curve. This curve results from the opening and the coalescing of surface cracks and fractures. The coalescence procedure of these microstructures was simulated with two common etched pits on a polished fused silica surface. Understanding the roughness evolution of plasma-processed surface might be helpful in optimizing the optical fabrication chain that contains APPP.

  18. Determination of copper, molybdenum and selenium in biological reference materials by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    In a contribution to the elemental characterization of 10 new reference materials, Bovine Muscle Powder (136), Corn Starch (162), Hard Red Spring Wheat Flour (165), Soft Winter Wheat Flour (166), Whole Milk Powder (183), Wheat Gluten (184), Corn Bran (186). Durum Wheat Flour (187), Whole Egg Powder (188) and Microcrystalline Cellulose (189), the total concentrations of Cu, Mo and Se were determined by the application of an analytical method based on isotope dilution inductively coupled plasma mass spectrometry. Cu and Mo contents were quantified by measurement of 65Cu/63Cu and 97Mo/100Mo isotopic ratios following spiking with 65Cu and 97Mo and digestion with nitric acid. Selenium was separated as hydrogen selenide from the matrix using sodium borohydride after spiking with 82Se and acid digestion-dry ashing and quantified by measurement of the 82Se/78Se isotopic ratio. Comparison of these results with those from a variety of other methods and assessment of the procedures using certified reference materials indicated that the determinations of Cu, Mo and Se were performed without analytical bias. (orig.)

  19. Effect of axial finiteness on electron heating in low-frequency inductively coupled plasmas

    International Nuclear Information System (INIS)

    Total power absorption inside the plasma (by taking the thermal motion of the electrons into account) has been calculated using different inductively coupled plasma models. The comparison shows that in the low-frequency region the results of the semi-infinite plasma models are different from those of the finite-length plasma models. The semi-infinite plasma models show net reduction of heating in the low-frequency region, due to thermal motion of the electrons from inside the skin region to outside the skin region. The finite-length plasma models on the other hand (due to change in the skin depth owing to the boundary condition of E=0 at z=L, and reflection of electrons from the plasma boundary) show that the decrease in heating due to the motion of the electrons from inside the skin depth to outside the skin depth is recovered by the reflection of the electrons from the plasma boundary. Hence, it is concluded that the results of the semi-infinite plasma models presented by Tyshetskiy et al. [Phys Rev. Lett. 90, 255002 (2003)] can be misleading (in the low-frequency region), since they overlooked the effect of axial finiteness of the plasma

  20. Depleted uranium analysis in blood by inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Todorov, T.I.; Xu, H.; Ejnik, J.W.; Mullick, F.G.; Squibb, K.; McDiarmid, M.A.; Centeno, J.A.

    2009-01-01

    In this study we report depleted uranium (DU) analysis in whole blood samples. Internal exposure to DU causes increased uranium levels as well as change in the uranium isotopic composition in blood specimen. For identification of DU exposure we used the 235U/238U ratio in blood samples, which ranges from 0.00725 for natural uranium to 0.002 for depleted uranium. Uranium quantification and isotopic composition analysis were performed by inductively coupled plasma mass spectrometry. For method validation we used eight spiked blood samples with known uranium concentrations and isotopic composition. The detection limit for quantification was determined to be 4 ng L-1 uranium in whole blood. The data reproduced within 1-5% RSD and an accuracy of 1-4%. In order to achieve a 235U/238U ratio range of 0.00698-0.00752% with 99.7% confidence limit a minimum whole blood uranium concentration of 60 ng L??1 was required. An additional 10 samples from a cohort of veterans exposed to DU in Gulf War I were analyzed with no knowledge of their medical history. The measured 235U/ 238U ratios in the blood samples were used to identify the presence or absence of DU exposure within this patient group. ?? 2009 The Royal Society of Chemistry.

  1. Methods for detecting and correcting inaccurate results in inductively coupled plasma-atomic emission spectrometry

    Science.gov (United States)

    Chan, George C. Y.; Hieftje, Gary M.

    2010-08-03

    A method for detecting and correcting inaccurate results in inductively coupled plasma-atomic emission spectrometry (ICP-AES). ICP-AES analysis is performed across a plurality of selected locations in the plasma on an unknown sample, collecting the light intensity at one or more selected wavelengths of one or more sought-for analytes, creating a first dataset. The first dataset is then calibrated with a calibration dataset creating a calibrated first dataset curve. If the calibrated first dataset curve has a variability along the location within the plasma for a selected wavelength, errors are present. Plasma-related errors are then corrected by diluting the unknown sample and performing the same ICP-AES analysis on the diluted unknown sample creating a calibrated second dataset curve (accounting for the dilution) for the one or more sought-for analytes. The cross-over point of the calibrated dataset curves yields the corrected value (free from plasma related errors) for each sought-for analyte.

  2. [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. PMID:26978934

  3. Heteroepitaxial growth of wafer scale highly oriented graphene using inductively coupled plasma chemical vapor deposition

    Science.gov (United States)

    Gao, Libo; Xu, Hai; Li, Linjun; Yang, Yang; Fu, Qiang; Bao, Xinhe; Loh, Kian Ping

    2016-06-01

    The chemical vapor deposition (CVD) of graphene on Cu has attracted much attention because of its industrial scalability. Herein, we report inductively coupled plasma-assisted CVD of epitaxially grown graphene on (111)-textured Cu film alloyed with a small amount of Ni, where large area high quality graphene film can be grown in less than 5 min at 800 °C, thus affording industrial scalability. The epitaxially grown graphene films on (111)-textured Cu contain grains which are predominantly aligned with the Cu lattice and about 10% of 30°-rotated grains (anti-grains). Such graphene films are exclusively monolayer and possess good electrical conductivity, high carrier mobility, and room temperature quantum Hall effect. Magnetoresistance measurements reveal that the reduction of the grain sizes from 150 nm to 50 nm produce increasing Anderson localization and the appearance of a transport gap. Owing to the presence of grain boundaries in these anti-grains, epitaxially grown graphene films possess n-type characteristics and exhibit ultra-high sensitivity to adsorbates.

  4. Inductively coupled plasma induced deep levels in epitaxial n-GaAs

    Energy Technology Data Exchange (ETDEWEB)

    Auret, F.D.; Janse van Rensburg, P.J.; Meyer, W.E.; Coelho, S.M.M. [Department of Physics, University of the Pretoria, Lynnwood Road, Pretoria 0002 (South Africa); Kolkovsky, Vl. [Technische Universitaet, Dresden, 01062 Dresden (Germany); Botha, J.R.; Nyamhere, C. [Department of Physics, Nelson Mandela Metropolitan University, PO Box 77000, Port Elizabeth 6031 (South Africa); Venter, A., E-mail: andre.venter@nmmu.ac.za [Department of Physics, Nelson Mandela Metropolitan University, PO Box 77000, Port Elizabeth 6031 (South Africa)

    2012-05-15

    The electronic properties of defects introduced by low energy inductively coupled Ar plasma etching of n-type (Si doped) GaAs were investigated by deep level transient spectroscopy (DLTS) and Laplace DLTS. Several prominent electron traps (E{sub c}-0.046 eV, E{sub c}-0.186 eV, E{sub c}-0.314 eV. E{sub c}-0.528 eV and E{sub c}-0.605 eV) were detected. The metastable defect E{sub c}-0.046 eV having a trap signature similar to E1 is observed for the first time. E{sub c}-0.314 eV and E{sub c}-0.605 eV are metastable and appear to be similar to the M3 and M4 defects present in dc H-plasma exposed GaAs.

  5. Cooperative analysis of alloying elements in zirconium alloys using inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    The Second Sub-Committee on Zircaloy Analysis, under Committee on Analytical Chemistry of Nuclear Fuels and Reactor Materials, JAERI, carried out a cooperative analysis with the nine laboratories on the determination of tin, iron, nickel and chromium in zirconium alloys to evaluate the practical applicability of inductively coupled plasma (ICP) atomic emission spectrometry. This report describes the sample decomposition procedures, determination conditions and procedures, and analytical results. The results obtained for alloying elements in samples for cooperative analysis (JAERI CRMs Z11 to Z14 and others) were compared with certified values or those obtained by X-ray fluorescence method, and were in good agreement with those values. ICP atomic emission spectrometry were shown to be an effective field method for determining alloying elements (C.V. % 2 to 7 for 0.5 to 1.90 % Sn, C.V. % 2 to 3 for 0.093 to 0.130 % Fe, C.V. % 3 to 6 for 0.095 to 0.110 % Ni and C.V. % 2 to 7 for 0.01 to 0.150 % Cr) in zirconium alloys. (author)

  6. Transport and trapping of dust particles in a potential well created by inductively coupled diffused plasmas

    Science.gov (United States)

    Choudhary, Mangilal; Mukherjee, S.; Bandyopadhyay, P.

    2016-05-01

    A versatile linear dusty (complex) plasma device is designed to study the transport and dynamical behavior of dust particles in a large volume. Diffused inductively coupled plasma is generated in the background of argon gas. A novel technique is used to introduce the dust particles in the main plasma by striking a secondary direct current glow discharge. These dust particles are found to get trapped in an electrostatic potential well, which is formed due to the combination of the ambipolar electric field caused by diffusive plasma and the field produced by the charged glass wall of the vacuum chamber. According to the requirements, the volume of the dust cloud can be controlled very precisely by tuning the plasma and discharge parameters. The present device can be used to address the underlying physics behind the transport of dust particles, self-excited dust acoustic waves, and instabilities. The detailed design of this device, plasma production and characterization, trapping and transport of the dust particle, and some of the preliminary experimental results are presented.

  7. Surface characterization of hydrophobic thin films deposited by inductively coupled and pulsed plasmas

    International Nuclear Information System (INIS)

    Different fluorocarbon thin films were deposited on Si substrates using a plasma-polymerization method. Fluorine-containing hydrophobic thin films were obtained by inductively coupled plasma (ICP) and pulsed plasma (PP) with a mixture of fluorocarbon precursors C2F6, C3F8, and c-C4F8 and the unsaturated hydrocarbons of C2H2. The influence on the fluorocarbon surfaces of the process parameters for plasma polymerization, including the gas ratio and the plasma power, were investigated under two plasma-polymerized techniques with different fluorocarbon gas precursors. The hydrophobic properties, surface morphologies, and chemical compositions were elucidated using water contact angle measurements, field emission-scanning electron microscope, x-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FT-IR), and time-of-flight secondary ion mass spectrometry (TOF-SIMS). In this study, the ICP technique provides coarser grained films and more hydrophobic surfaces as well as a higher deposition rate compared to the PP technique. XPS, FT-IR, and TOF-SIMS analyses indicated that the ICP technique produced more fluorine-related functional groups, including CF2 and CF3, on the surface. From the curve-fitted XPS results, fluorocarbon films grown under ICP technique exhibited less degree of cross-linking and higher CF2 concentrations than those grown under PP technique.

  8. Use of laser-excited atomic fluorescence spectroscopy for characterization of an argon inductively coupled plasma

    International Nuclear Information System (INIS)

    Laser-excited atomic fluorescence spectroscopy (LEAFS) is investigated and employed as a diagnostic technique for study of the argon inductively coupled plasma (ICP). Computer simulations are used to describe the behavior of nonsteady-state laser excited fluorescence (LEF) for multi-level atomic systems under conditions expected to be encountered in the ICP and an atmospheric pressure flame. These simulations are then compared to experimental data collected under similar conditions in the ICP and a flame. These studies show that LEAFS should be a useful tool for characterization of an ICP, with certain limitations. Relatively small changes in saturated LEF signals under changing quenching and mixing conditions are both predicted theoretically and observed experimentally for several atomic systems. This independence from quenching and mixing effects allows one to relate saturated LEF signals directly to relative number densities of species when spatially scanning over an inhomogeneous medium, such as an ICP discharge, where significant changes in quenching can be encountered in a single scan. SSI values are also found to be useful as indicators of relative collisional quenching rates and relative degree of LTE establishment in the ICP, as well as ease of saturation for a given transition

  9. 200-mm-diameter neutral beam source based on inductively coupled plasma etcher and silicon etching

    International Nuclear Information System (INIS)

    The authors developed a neutral beam source consisting of a 200-mm-diameter inductively coupled plasma etcher and a graphite neutralization aperture plate based on the design of a neutral beam source that Samukawa et al. [Jpn. J. Appl. Phys., Part 2 40, L779 (2001)] developed. They measured flux and energy of neutral particles, ions, and photons using a silicon wafer with a thermocouple and a Faraday cup and calculated the neutralization efficiency. An Ar neutral beam flux of more than 1 mA/cm2 in equivalent current density and a neutralization efficiency of more than 99% were obtained. The spatial uniformity of the neutral beam flux was within ±6% within a 100 mm diameter. Silicon etching using a F2-based neutral beam was done at an etch rate of about 47 nm/min, while Cl2-based neutral beam realized completely no undercut. The uniformity of etch rate was less than ±5% within the area. The etch rate increased by applying bias power to the neutralization aperture plate, which shows that accelerated neutral beam was successfully obtained. These results indicate that the neutral beam source is scalable, making it possible to obtain a large-diameter and uniform neutral beam, which is inevitable for application to mass production.

  10. The etching of silicon carbide in inductively coupled SF6/O2 plasma

    International Nuclear Information System (INIS)

    The etching mechanisms of silicon carbide in an inductively coupled plasma (ICP) reactor using a SF6/O2 gas mixture, have been investigated using optical emission spectroscopy (OES) and Langmuir probe measurements. The etching is shown to be ion induced with a high degree of anisotropy. An optimum etch rate is achieved with 20% oxygen content within the gas mixture. By studying the independent influence of the ICP power and the substrate bias voltage on the ion current density, as well as the fluorine and oxygen radical densities in the plasma, the etch mechanism is found to be dominated by the number of ions bombarding the SiC surface. The steady state sputter yield observed at P>0.7 Pa, despite the increase in F radical concentration indicates the dominant role of ion bombardment in this etch regime, while at P<0.7 Pa, the etch mechanism is limited by the number of F radicals in the plasma. The OES results have shown that the etch rate is dependent upon the concentration of reactive radicals present with the [F]/[0] ratio = 8 at the optimum. Whilst using the optimum gas composition, the parameters which dominate the physical side of the reaction, ICP power and bias voltage, produce an increase of the etch rate as the potential difference between the substrate and the plasma is increased

  11. Patterning of titanium oxide surfaces using inductively coupled plasma for gas sensing

    Energy Technology Data Exchange (ETDEWEB)

    Hotovy, I., E-mail: ivan.hotovy@stuba.sk [Institute of Electronics and Photonics, Slovak University of Technology, Ilkovicova 3, 812 19 Bratislava (Slovakia); Kostic, I. [Institute of Informatics, Slovak Academy of Sciences, Dubravska cesta 9, 845 07 Bratislava (Slovakia); Hascik, S. [Institute of Electrical Engineering, Slovak Academy of Sciences, Dubravska cesta 9, 845 07 Bratislava (Slovakia); Rehacek, V.; Predanocy, M. [Institute of Electronics and Photonics, Slovak University of Technology, Ilkovicova 3, 812 19 Bratislava (Slovakia); Bencurova, A. [Institute of Informatics, Slovak Academy of Sciences, Dubravska cesta 9, 845 07 Bratislava (Slovakia)

    2014-09-01

    Highlights: • Etching characteristics of TiO{sub 2} films using CF{sub 4} plasma in ICP system were studied. • TiO{sub 2} tips with minimal diameter of 100 nm were patterned using ICP etching. • Pyramidal TiO{sub 2} nanotips were fabricated by self-assembled AuNPs as ICP etch mask. • TiO{sub 2} tip arrays may have important application in gas microsensors. - Abstract: Titanium oxide thin films were deposited at room temperature by reactive magnetron sputtering in a mixture of oxygen and argon on oxidized silicon substrates. The optimal etching characteristics of TiO{sub 2} films by an inductively coupled plasma system were investigated. The maximum etch rate of TiO{sub 2} was 104 nm/min at fixed 200 W of ICP power and the highest investigated value of RF chuck power of 150 W. Patterning of TiO{sub 2} tip arrays by electron beam lithography and dry etching was conducted. Experimental results showed that the exposure dose optimization was a significant parameter for controlling the tip size and its shape. Pyramidal TiO{sub 2} tip arrays were successfully fabricated by dry etching in CF{sub 4}/Ar plasma through a Au nanoparticle mask. The TiO{sub 2} tip arrays can be expected to have an important application in gas microsensors.

  12. Fabrication of SiC nanopillars by inductively coupled SF6/O2 plasma etching

    International Nuclear Information System (INIS)

    In this paper, we demonstrate a top-down fabrication technique for nanometre scale silicon carbide (SiC) pillars using inductively coupled plasma etching. A set of experiments in SF6-based plasma was carried out in order to realize high aspect ratio SiC nanopillars. The etched SiC nanopillars using a small circular mask pattern (115 nm diameter) show high aspect ratio (7.4) with a height of 2.2 µm at an optimum bias voltage (300 V) and pressure (6 mTorr). Under the optimal etching conditions using a large circular mask pattern with 370 nm diameter, the obtained SiC nanopillars exhibit high anisotropy features (6.4) with a large etch depth (>7 µm). The etch characteristic of the SiC nanopillars under these conditions shows a high etch rate (550 nm min-1) and a high selectivity (over 60 for Ni). We also studied the etch profile of the SiC nanopillars and mask evolution over the etching time. As the mask pattern size shrinks in nanoscale, vertical and lateral mask erosion plays a crucial role in the etch profile of the SiC nanopillars. Long etching process makes the pillars appear with a hexagonal shape, coming from the crystallographic structure of α-SiC. It is found that the feature of pillars depends not only on the etching process parameters, but also on the crystallographic structure of the SiC phase. (paper)

  13. Optimization of inductively coupled plasma deep etching of GaN and etching damage analysis

    International Nuclear Information System (INIS)

    Inductively coupled plasma (ICP) etching of GaN with an etching depth up to 4 μm is systemically studied by varying ICP power, RF power and chamber pressure, respectively, which results in etch rates ranging from ∼370 nm/min to 900 nm/min. The surface morphology and damages of the etched surface are characterized by optical microscope, scanning electron microscope, atomic force microscopy, cathodoluminescence mapping and photoluminescence (PL) spectroscopy. Sub-micrometer-scale hexagonal pits and pillars originating from part of the structural defects within the original GaN layer are observed on the etched surface. The density of these surface features varies with etching conditions. Considerable reduction of PL band-edge emission from the etched GaN surface indicates that high-density non-radiative recombination centers are created by ICP etching. The density of these non-radiative recombination centers is found largely dependent on the degree of physical bombardments, which is a strong function of the RF power applied. Finally, a low-surface-damage etch recipe with high ICP power, low RF power, high chamber pressure is suggested.

  14. Measuring ion velocity distribution functions through high-aspect ratio holes in inductively coupled plasmas

    Science.gov (United States)

    Cunge, G.; Darnon, M.; Dubois, J.; Bezard, P.; Mourey, O.; Petit-Etienne, C.; Vallier, L.; Despiau-Pujo, E.; Sadeghi, N.

    2016-02-01

    Several issues associated with plasma etching of high aspect ratio structures originate from the ions' bombardment of the sidewalls of the feature. The off normal angle incident ions are primarily due to their temperature at the sheath edge and possibly to charging effects. We have measured the ion velocity distribution function (IVDF) at the wafer surface in an industrial inductively coupled plasma reactor by using multigrid retarding field analyzers (RFA) in front of which we place 400 μm thick capillary plates with holes of 25, 50, and 100 μm diameters. The RFA then probes IVDF at the exit of the holes with Aspect Ratios (AR) of 16, 8, and 4, respectively. The results show that the ion flux dramatically drops with the increase in AR. By comparing the measured IVDF with an analytical model, we concluded that the ion temperature is 0.27 eV in our plasma conditions. The charging effects are also observed and are shown to significantly reduce the ion energy at the bottom of the feature but only with a "minor" effect on the ion flux and the shape of the IVDF.

  15. High sensitivity ultra-broad-band absorption spectroscopy of inductively coupled chlorine plasma

    Science.gov (United States)

    Marinov, Daniil; Foucher, Mickaël; Campbell, Ewen; Brouard, Mark; Chabert, Pascal; Booth, Jean-Paul

    2016-06-01

    We propose a method to measure the densities of vibrationally excited Cl2(v) molecules in levels up to v  =  3 in pure chlorine inductively coupled plasmas (ICPs). The absorption continuum of Cl2 in the 250–450 nm spectral range is deconvoluted into the individual components originating from the different vibrational levels of the ground state, using a set of ab initio absorption cross sections. It is shown that gas heating at constant pressure is the major depletion mechanism of the Cl2 feedstock in the plasma. In these line-integrated absorption measurements, the absorption by the hot (and therefore rarefied) Cl2 gas in the reactor centre is masked by the cooler (and therefore denser) Cl2 near the walls. These radial gradients in temperature and density make it difficult to assess the degree of vibrational excitation in the centre of the reactor. The observed line-averaged vibrational distributions, when analyzed taking into account the radial temperature gradient, suggest that vibrational and translational degrees of freedom in the plasma are close to local equilibrium. This can be explained by efficient vibrational-translational (VT) relaxation between Cl2 and Cl atoms. Besides the Cl2(v) absorption band, a weak continuum absorption is observed at shorter wavelengths, and is attributed to photodetachment of Cl‑ negative ions. Thus, line-integrated densities of negative ions in chlorine plasmas can be directly measured using broad-band absorption spectroscopy.

  16. Biofuel Cell Based on Microscale Nanostructured Electrodes with Inductive Coupling to Rat Brain Neurons

    Science.gov (United States)

    Andoralov, Viktor; Falk, Magnus; Suyatin, Dmitry B.; Granmo, Marcus; Sotres, Javier; Ludwig, Roland; Popov, Vladimir O.; Schouenborg, Jens; Blum, Zoltan; Shleev, Sergey

    2013-11-01

    Miniature, self-contained biodevices powered by biofuel cells may enable a new generation of implantable, wireless, minimally invasive neural interfaces for neurophysiological in vivo studies and for clinical applications. Here we report on the fabrication of a direct electron transfer based glucose/oxygen enzymatic fuel cell (EFC) from genuinely three-dimensional (3D) nanostructured microscale gold electrodes, modified with suitable biocatalysts. We show that the process underlying the simple fabrication method of 3D nanostructured electrodes is based on an electrochemically driven transformation of physically deposited gold nanoparticles. We experimentally demonstrate that mediator-, cofactor-, and membrane-less EFCs do operate in cerebrospinal fluid and in the brain of a rat, producing amounts of electrical power sufficient to drive a self-contained biodevice, viz. 7 μW cm-2 in vitro and 2 μW cm-2 in vivo at an operating voltage of 0.4 V. Last but not least, we also demonstrate an inductive coupling between 3D nanobioelectrodes and living neurons.

  17. Low-frequency, high-density, inductively coupled plasma sources: Operation and applications

    International Nuclear Information System (INIS)

    Operation regimes, plasma parameters, and applications of the low-frequency (∼500 kHz) inductively coupled plasma (ICP) sources with a planar external coil are investigated. It is shown that highly uniform, high-density (ne∼9x1012 cm-3) plasmas can be produced in low-pressure argon discharges with moderate rf powers. The low-frequency ICP sources operate in either electrostatic (E) or electromagnetic (H) regimes in a wide pressure range without any Faraday shield or an external multipolar magnetic confinement, and exhibit high power transfer efficiency, and low circuit loss. In the H mode, the ICP features high level of uniformity over large processing areas and volumes, low electron temperatures, and plasma potentials. The low-density, highly uniform over the cross-section, plasmas with high electron temperatures and plasma and sheath potentials are characteristic to the electrostatic regime. Both operation regimes offer great potential for various plasma processing applications. As examples, the efficiency of the low-frequency ICP for steel nitriding and plasma-enhanced chemical vapor deposition of hydrogenated diamond-like carbon (DLC) films, is demonstrated. It appears possible to achieve very high nitriding rates and dramatically increase micro-hardness and wear resistance of the AISI 304 stainless steel. It is also shown that the deposition rates and mechanical properties of the DLC films can be efficiently controlled by selecting the discharge operating regime

  18. Extraction and neutralization of positive and negative ions from a pulsed electronegative inductively coupled plasma

    Science.gov (United States)

    Marinov, D.; el Otell, Z.; Bowden, M. D.; Braithwaite, N. St. J.

    2015-12-01

    Almost electron-free (ion-ion) plasmas can be transiently formed during the afterglow phase of pulsed plasmas in electronegative gases. In ion-ion plasmas, both positive and negative ions can be extracted which makes them advantageous for a number of applications. In this paper, we investigate the extraction and acceleration of positive and negative ion beams from a pulsed inductively coupled plasma in SF6. The plasma is bounded by two electrodes biased synchronously with the discharge modulation. It is shown that when a DC bias voltage is applied during the afterglow phase, positive/negative ions are accelerated in a positive/negative space charge sheath formed in front of one of the electrodes. The energy of extracted ions closely follows the amplitude of the applied bias voltage (25-150 V) and the peak beam current density reaches 2 A m-2. With a view to using the described system as a source of energetic neutral beams for low damage material processing, simultaneous extraction and surface neutralization of positive and negative ions using an extraction electrode with high aspect ratio apertures is investigated.

  19. Inductively coupled plasma mass spectrometry in the analysis of biological samples and pharmaceutical drugs

    Science.gov (United States)

    Ossipov, K.; Seregina, I. F.; Bolshov, M. A.

    2016-04-01

    Inductively coupled plasma mass spectrometry (ICP-MS) is widely used in the analysis of biological samples (whole blood, serum, blood plasma, urine, tissues, etc.) and pharmaceutical drugs. The shortcomings of this method related to spectral and non-spectral interferences are manifested in full measure in determination of the target analytes in these complex samples strongly differing in composition. The spectral interferences are caused by similarity of masses of the target component and sample matrix components. Non-spectral interferences are related to the influence of sample matrix components on the physicochemical processes taking place during formation and transportation of liquid sample aerosols into the plasma, on the value and spatial distribution of plasma temperature and on the transmission of the ion beam from the interface to mass spectrometer detector. The review is devoted to analysis of different mechanisms of appearance of non-spectral interferences and to ways for their minimization or elimination. Special attention is paid to the techniques of biological sample preparation, which largely determine the mechanisms of the influence of sample composition on the results of element determination. The ways of lowering non-spectral interferences by instrumental parameter tuning and application of internal standards are considered. The bibliography includes 189 references.

  20. Isotope ratio analysis of lead in biological materials by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Inductively coupled plasma mass spectrometry (ICP-MS) allowed 0.2-0.3% imprecision (1 sigma) in 204Pb/206Pb 207Pb/'206Pb, and 208Pb/206Pb measurements at the 20-100 ppb level, which was precise enough to detect some of the isotopic variations observed in nature. Mass discrimination could be corrected within ±0.5% of the true value by periodical analysis of standard reference material of known lead isotopic composition. As a separation method for lead in human bone, which contains enormous amounts of calcium and phosphorus, anion exchange of the Pb-Br complex was found to be effective. Lead isotope ratios in bone, measured by ICP-MS after separation, were consistent with those measured by thermal ionization mass spectrometry. Hair matrix did not have any influence on the accuracy and precision of the analysis; a digested sample could be directly analyzed and this offered rapid sample throughput. Preliminary data on lead isotope ratios in bone and hair from prehistoric and contemporary Japanese are presented. (author)