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Sample records for elemental mass spectrometry

  1. Paradigms in isotope dilution mass spectrometry for elemental speciation analysis

    International Nuclear Information System (INIS)

    Meija, Juris; Mester, Zoltan

    2008-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-01-01

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

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

    International Nuclear Information System (INIS)

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

    1978-01-01

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

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

    International Nuclear Information System (INIS)

    Moens, L.

    1997-01-01

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

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

    International Nuclear Information System (INIS)

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

    1988-01-01

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

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

    International Nuclear Information System (INIS)

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

    2011-04-01

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

  7. Mass spectrometry

    DEFF Research Database (Denmark)

    Nyvang Hartmeyer, Gitte; Jensen, Anne Kvistholm; Böcher, Sidsel

    2010-01-01

    Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) is currently being introduced for the rapid and accurate identification of bacteria. We describe 2 MALDI-TOF MS identification cases - 1 directly on spinal fluid and 1 on grown bacteria. Rapidly obtained...

  8. Uniform elemental analysis of materials by sputtering and photoionization mass spectrometry

    International Nuclear Information System (INIS)

    Chun, He; Basler, J.N.; Becker, C.H.

    1997-01-01

    Analysis of the elemental composition of surfaces commonly involves techniques in which atoms or ions are ablated from the material's surface and detected by mass spectrometry. Secondary-ion mass spectrometry is widely used for detection with high sensitivity (down to a few parts per billion) but technical problems prevent it from being truly quantitative. Some of these problems are circumvented by nonresonant laser post-ionization of sputtered atoms followed by time-of-flight mass spectrometry (surface analysis by laser ionization: SALI). But when there are large differences in ionization probabilities amongst different elements in the material, the detection sensitivity can be non-uniform and accurate quantification remains out of reach. Here we report that highly uniform, quantitative and sensitive analysis of materials can be achieved using a high-energy (5-keV) ion beam for sputtering coupled with a very-high-intensity laser to induce multiphoton ionization of the sputtered atoms. We show uniform elemental sensitivity for several samples containing elements with very different ionization potentials, suggesting that this approach can now be regarded as quantitative for essentially any material. (author)

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-01-01

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

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

    Science.gov (United States)

    Nie, Xi-Du; Fu, Liang

    2013-07-01

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

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

    Science.gov (United States)

    Yan, Xiaowen; Yang, Limin; Wang, Qiuquan

    2013-07-01

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

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

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

    International Nuclear Information System (INIS)

    Sumida, Takashi; Nakazato, Tetsuya; Tao, Hiroaki

    2003-01-01

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

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

    NARCIS (Netherlands)

    Sysoev, AA; Sysoev, AA

    2002-01-01

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

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

    International Nuclear Information System (INIS)

    Ender, R.M.

    1997-01-01

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

  17. [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.

  18. Atomic mass spectrometry

    International Nuclear Information System (INIS)

    Sanz-Medel, A.

    1997-01-01

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

  19. Mass spectrometry in clinical chemistry

    International Nuclear Information System (INIS)

    Pettersen, J.E.

    1977-01-01

    A brief description is given of the functional elements of a mass spectrometer and of some currently employed mass spectrometric techniques, such as combined gas chromatography-mass spectrometry, mass chromatography, and selected ion monitoring. Various areas of application of mass spectrometry in clinical chemistry are discussed, such as inborn errors of metabolism and other metabolic disorders, intoxications, quantitative determinations of drugs, hormones, gases, and trace elements, and the use of isotope dilution mass spectrometry as a definitive method for the establishment of true values for concentrations of various compounds in reference sera. It is concluded that mass spectrometry is of great value in clinical chemistry. (Auth.)

  20. Levels of Essential Elements in Different Medicinal Plants Determined by Using Inductively Coupled Plasma Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Eid I. Brima

    2018-01-01

    Full Text Available The objective of this study was to investigate the content of essential elements in medicinal plants in the Kingdom of Saudi Arabia (KSA. Five different medical plants (mahareeb (Cymbopogon schoenanthus, sheeh (Artemisia vulgaris, harjal (Cynanchum argel delile, nabipoot (Equisetum arvense, and cafmariam (Vitex agnus-castus were collected from Madina city in the KSA. Five elements Fe, Mn, Zn, Cu, and Se were determined by using inductively coupled plasma mass spectrometry (ICP-MS. Fe levels were the highest and Se levels were the lowest in all plants. The range levels of all elements in all plants were as follows: Fe 193.4–1757.9, Mn 23.6–143.7, Zn 15.4–32.7, Se 0.13–0.92, and Cu 11.3–21.8 µg/g. Intakes of essential elements from the medical plants in infusion were calculated: Fe 4.6–13.4, Mn 6.7–123.2, Zn 7.0–42.7, Se 0.14–1.5, and Cu 1.5–5.0 µg/dose. The calculated intakes of essential elements for all plants did not exceed the daily intake set by the World Health Organization (WHO and European Food Safety Authority (EFSA. These medicinal plants may be useful sources of essential elements, which are vital for health.

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

    Directory of Open Access Journals (Sweden)

    Emmanuelle Cordeau

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

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

    International Nuclear Information System (INIS)

    Saito, Morimasa; Sudo, Emiko

    1975-01-01

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

  3. Mass spectrometry in oceanography

    International Nuclear Information System (INIS)

    Aggarwal, Suresh K.

    2000-01-01

    Mass spectrometry plays an important role in oceanography for various applications. Different types of inorganic as well as organic mass spectrometric techniques are being exploited world-wide to understand the different aspects of marine science, for palaeogeography, palaeoclimatology and palaeoecology, for isotopic composition and concentrations of different elements as well as for speciation studies. The present paper reviews some of the applications of atomic mass spectrometric techniques in the area of oceanography

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

    Science.gov (United States)

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

    2017-08-01

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

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

    Science.gov (United States)

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

    2009-10-30

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

  6. Determination of elemental composition of metals using ambient organic mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-05-22

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

  7. Determination of elemental composition of metals using ambient organic mass spectrometry

    International Nuclear Information System (INIS)

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

    2017-01-01

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

  8. Identification of organically associated trace elements in wood and coal by inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Richaud, R; Lazaro, M J; Lachas, H; Miller, B B; Herod, A A; Dugwell, D R; Kandiyoti, R

    2000-01-01

    1-Methyl-2-pyrrolidinone (NMP) was used to extract samples of wood (forest residue) and coal; the extracts were analysed by inductively coupled plasma mass spectrometry (ICP-MS) using two different sample preparation methods, in order to identify trace elements associated with the organic part of the samples. A sample of fly ash was similarly extracted and analysed in order to assess the behaviour of the mineral matter contained within the wood and coal samples. 32% of the biomass was extracted at the higher temperature and 12% at room temperature while only 12% of the coal was extracted at the higher temperature and 3% at room temperature. Less than 2% of the ash dissolved at the higher temperature. Size exclusion chromatograms of the extracts indicated the presence of significant amounts of large molecular mass materials (>1000 mu) in the biomass and coal extracts but not in the ash extract. Trace element analyses were carried out using ICP-MS on the acid digests prepared by 'wet ashing' and microwave extraction. Sixteen elements (As, Ba, Be, Cd, Co, Cr, Cu, Ga, Mn, Mo, Ni, Pb, Sb, Se, V and Zn) were quantified, in the samples before extraction, in the extracts and in the residues. Concentrations of trace elements in the original biomass sample were lower than in the coal sample while the concentrations in the ash sample were the highest. The major trace elements in the NMP extracts were Ba, Cu, Mn and Zn from the forest residue; Ba, Cu, Mn, Pb and Zn from the coal; Cu and Zn from the ash. These elements are believed to be associated with the organic extracts from the forest residue and coal, and also from the ash. Be and Sb were not quantified in the extracts because they were present at too low concentrations; up to 40% of Mn was extracted from the biomass sample at 202 degrees C, while Se was totally extracted from the ash sample. For the forest residue, approximately 7% (at room temperature) and 45% (at 202 degrees C) of the total trace elements studied were

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

    International Nuclear Information System (INIS)

    Mohammed, A.E.W.M.

    2013-01-01

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

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

    International Nuclear Information System (INIS)

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

    1993-01-01

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

  11. Sample diagnosis using indicator elements and non-analyte signals for inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Antler, Margaret; Ying Hai; Burns, David H.; Salin, Eric D.

    2003-01-01

    A sample diagnosis procedure that uses both non-analyte and analyte signals to estimate matrix effects in inductively coupled plasma-mass spectrometry is presented. Non-analyte signals are those of background species in the plasma (e.g. N + , ArO + ), and changes in these signals can indicate changes in plasma conditions. Matrix effects of Al, Ba, Cs, K and Na on 19 non-analyte signals and 15 element signals were monitored. Multiple linear regression was used to build the prediction models, using a genetic algorithm for objective feature selection. Non-analyte elemental signals and non-analyte signals were compared for diagnosing matrix effects, and both were found to be suitable for estimating matrix effects. Individual analyte matrix effect estimation was compared with the overall matrix effect prediction, and models used to diagnose overall matrix effects were more accurate than individual analyte models. In previous work [Spectrochim. Acta Part B 57 (2002) 277], we tested models for analytical decision making. The current models were tested in the same way, and were able to successfully diagnose matrix effects with at least an 80% success rate

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

    International Nuclear Information System (INIS)

    Lee Yiling; Chang Chaochiang; Jiang Shiuhjen

    2003-01-01

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

  13. Vaporization studies on elemental tellurium and selenium by Knudsen effusion mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Viswanathan, R., E-mail: rvis1953@gmail.com; Balasubramanian, R., E-mail: rbs@igcar.gov.in; Darwin Albert Raj, D., E-mail: darwinalbertraj1953@gmail.com; Sai Baba, M., E-mail: msb@igcar.gov.in; Lakshmi Narasimhan, T.S., E-mail: tslak@igcar.gov.in

    2014-08-01

    Highlights: • A detailed KEMS study of vaporization of elemental tellurium and selenium systems. • Clusters Te{sub i}(g) (i = 2 to 7) and Se{sub i}(g) (i = 2 to 9) identified over Te(s) and Se(s). • p–T relations for Te{sub i}(g) (590 to 690 K) and Se{sub i}(g) (380 to 480 K). • Vapor phase of Te dominated by Te{sub 2}(g) (∼95%) while that of Se by Se{sub 6}(g) (∼50%) and Se{sub 5}(g) (∼25%). • Sublimation and atomization enthalpies deduced for Te{sub i}(g) and Se{sub i}(g). - Abstract: Vaporization studies on elemental tellurium and selenium were conducted by Knudsen effusion mass spectrometry in the temperature range of 590–690 K and 380–480 K, respectively. The ionic species Te{sub i}{sup +} (i = 1–7) and Se{sub i}{sup +}(g) (i = 1–9) were detected in the mass spectra over these two condensed phases. Measurement of ion intensities were performed as a function of electron impact energy and as a function of temperature (at different electron impact energies) for identifying the gaseous precursor species as well as for determining the partial pressure–temperature relations and sublimation enthalpies for these species. While the major species over elemental tellurium was confirmed to be Te{sub 2}(g) (with all other gaseous species Te{sub 3}–Te{sub 7} put together constituting less than 5%), the major species over elemental selenium was found to be Se{sub 6}(g), closely followed by Se{sub 5}(g) (with other gaseous species Se{sub 2}–Se{sub 4} and Se{sub 7}–Se{sub 9} put together also moderately constituting ∼25%). From the partial pressures, the thermodynamic data for the sublimation reactions i Te(s) = Te{sub i}(g) and i Se(s) = Se{sub i}(g) were deduced by second- and third-law methods. The atomization enthalpies of tellurium and selenium clusters were also deduced by using the recommended enthalpies of formation of monomeric species. Comparison of the findings obtained in the present study with those in previous studies revealed

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

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

    International Nuclear Information System (INIS)

    Kretschy, Daniela; Koellensperger, Gunda; Hann, Stephan

    2012-01-01

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

  16. Redox speciation of final repository relevant elements using separation methods in combination with ICP mass spectrometry

    International Nuclear Information System (INIS)

    Graser, Carl-Heinrich

    2015-01-01

    The long-term safety assessment for nuclear waste repositories requires a detailed understanding of the chemistry of actinide elements in the geosphere. The development of advanced analytical tools is required to gain detailed insights into actinide redox speciation in a given system. The mobility of radionuclides is mostly determined by the geochemical conditions which control the redox state of radionuclides. Besides the longlived radionuclides plutonium (Pu) and neptunium (Np), which are key elements in high level nuclear waste, iron (Fe) represents a main component in natural systems controlling redox related geochemical processes. Analytical techniques for determining oxidation state distribution for redox sensitive radionuclides and other metal ions often have a lack of sensitivity. The detection limits of these methods (i.e. UV/vis, TRLFS, XANES) are in general in the range of ≥ 10 -6 mol.L -1 . As a consequence ultrasensitive new analytical techniques are required. Capillary electrophoresis (CE) and ion chromatography (IC) are powerful separation methods for metal ions. In the course of this thesis different speciation method for iron, neptunium and plutonium were optimized. With the optimized setup redox speciation analysis of these elements in different samples were done. Furthermore CE hyphenated to inductively coupled plasma sector field mass spectrometry (CE - ICP - SF - MS) was used to measure the redox speciation of Pu (III, IV, V, VI), Np (IV, V, VI) and Fe (II, III) at concentrations lower than 10 -7 mol.L -1 . CE coupling and separation parameters such as sample gas pressure, make up flow rate, capillary position, auxiliary gas flow, as well as the electrolyte system were optimized to obtain the maximum sensitivity. The methodes detection limits are 10 -12 mol.L -1 for Np and Pu. The various oxidation state species of Pu and Np in different samples were separated by application of an acetate based electrolyte system. The separation of Fe (II

  17. Molecules and elements for quantitative bioanalysis: The allure of using electrospray, MALDI, and ICP mass spectrometry side-by-side.

    Science.gov (United States)

    Linscheid, Michael W

    2018-03-30

    To understand biological processes, not only reliable identification, but quantification of constituents in biological processes play a pivotal role. This is especially true for the proteome: protein quantification must follow protein identification, since sometimes minute changes in abundance tell the real tale. To obtain quantitative data, many sophisticated strategies using electrospray and MALDI mass spectrometry (MS) have been developed in recent years. All of them have advantages and limitations. Several years ago, we started to work on strategies, which are principally capable to overcome some of these limits. The fundamental idea is to use elemental signals as a measure for quantities. We began by replacing the radioactive 32 P with the "cold" natural 31 P to quantify modified nucleotides and phosphorylated peptides and proteins and later used tagging strategies for quantification of proteins more generally. To do this, we introduced Inductively Coupled Plasma Mass Spectrometry (ICP-MS) into the bioanalytical workflows, allowing not only reliable and sensitive detection but also quantification based on isotope dilution absolute measurements using poly-isotopic elements. The detection capability of ICP-MS becomes particularly attractive with heavy metals. The covalently bound proteins tags developed in our group are based on the well-known DOTA chelate complex (1,4,7,10-tetraazacyclododecane-N,N',N″,N‴-tetraacetic acid) carrying ions of lanthanoides as metal core. In this review, I will outline the development of this mutual assistance between molecular and elemental mass spectrometry and discuss the scope and limitations particularly of peptide and protein quantification. The lanthanoide tags provide low detection limits, but offer multiplexing capabilities due to the number of very similar lanthanoides and their isotopes. With isotope dilution comes previously unknown accuracy. Separation techniques such as electrophoresis and HPLC were used and just

  18. The determination of low level trace elements in coals by laser ablation-inductively coupled plasma-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Booth, C.A.; Spears, D.A.; Krause, P.; Cox, A.G. [University of Sheffield, Sheffield (United Kingdom). Dept. of Earth Sciences

    1999-11-01

    The rapid determination of elements present in low level concentrations in bituminous coals is possible using laser abalation-inductively coupled plasma-mass spectrometry (l.a.-i.c.p.-m.s.). A wide range of trace elements can routinely be determined using this technique but it is for environmentally sensitive elements, such as As, Cd, Mo, Sb, Se and Hg, that it is of most use due to the low levels of detection. Calibration of the i.c.p.-m.s. was achieved using a series of uncertified coals and the method evaluated using the South African certified coals, Sarm 18, 19 and 20. A critical evaluation of the data obtained shows that for many of the elements studied the results obtained are both accurate and precise, even at very low concentrations, with the limits of detection for all of the elements being in the {mu}g/kg (parts per billion) range. 6 refs., 3 figs., 9 tabs.

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

    Science.gov (United States)

    Kretschy, Daniela; Koellensperger, Gunda; Hann, Stephan

    2012-01-01

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

  20. Multi-elemental analysis of aqueous geochemical samples by quadrupole inductively coupled plasma-mass spectrometry (ICP-MS)

    Science.gov (United States)

    Wolf, Ruth E.; Adams, Monique

    2015-01-01

    Typically, quadrupole inductively coupled plasma-mass spectrometry (ICP-MS) is used to determine as many as 57 major, minor, and trace elements in aqueous geochemical samples, including natural surface water and groundwater, acid mine drainage water, and extracts or leachates from geological samples. The sample solution is aspirated into the inductively coupled plasma (ICP) which is an electrodeless discharge of ionized argon gas at a temperature of approximately 6,000 degrees Celsius. The elements in the sample solution are subsequently volatilized, atomized, and ionized by the ICP. The ions generated are then focused and introduced into a quadrupole mass filter which only allows one mass to reach the detector at a given moment in time. As the settings of the mass analyzer change, subsequent masses are allowed to impact the detector. Although the typical quadrupole ICP-MS system is a sequential scanning instrument (determining each mass separately), the scan speed of modern instruments is on the order of several thousand masses per second. Consequently, typical total sample analysis times of 2–3 minutes are readily achievable for up to 57 elements.

  1. Accelerator mass spectrometry of heavy elements: /sup 36/Cl to /sup 205/Pb

    Energy Technology Data Exchange (ETDEWEB)

    Henning, W

    1987-08-25

    Measurements are discussed in which the technique of accelerator mass spectrometry was applied to problems involving heavy radioisotopes. These measurements, which depend on the ion energies that can be reached with the new heavy-ion accelerator facilities, were performed at the Argonne tandem linac accelerator system (ATLAS) and at the UNILAC accelerator at GSI. The topics include a discussion of measurements of long nuclear lifetimes, of radioisotope detection of interest to solar neutrino experiments, and of a determination of the /sup 41/Ca concentration in natural samples of terrestrial origin by making use of isotopic pre-enrichment in an isotope separator. A long-known method of isobar separation, employing a gas-filled magnetic field region, has been revived for some of these measurements and its characteristics and advantages are briefly reviewed.

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  4. Glycomics using mass spectrometry

    OpenAIRE

    Wuhrer, Manfred

    2013-01-01

    Mass spectrometry plays an increasingly important role in structural glycomics. This review provides an overview on currently used mass spectrometric approaches such as the characterization of glycans, the analysis of glycopeptides obtained by proteolytic cleavage of proteins and the analysis of glycosphingolipids. The given examples are demonstrating the application of mass spectrometry to study glycosylation changes associated with congenital disorders of glycosylation, lysosomal storage di...

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

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

    International Nuclear Information System (INIS)

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

    1991-01-01

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

  7. Fourier Transform Mass Spectrometry

    Science.gov (United States)

    Scigelova, Michaela; Hornshaw, Martin; Giannakopulos, Anastassios; Makarov, Alexander

    2011-01-01

    This article provides an introduction to Fourier transform-based mass spectrometry. The key performance characteristics of Fourier transform-based mass spectrometry, mass accuracy and resolution, are presented in the view of how they impact the interpretation of measurements in proteomic applications. The theory and principles of operation of two types of mass analyzer, Fourier transform ion cyclotron resonance and Orbitrap, are described. Major benefits as well as limitations of Fourier transform-based mass spectrometry technology are discussed in the context of practical sample analysis, and illustrated with examples included as figures in this text and in the accompanying slide set. Comparisons highlighting the performance differences between the two mass analyzers are made where deemed useful in assisting the user with choosing the most appropriate technology for an application. Recent developments of these high-performing mass spectrometers are mentioned to provide a future outlook. PMID:21742802

  8. Investigating the Lymphatic System by Dual-Color Elemental Mass Spectrometry Imaging

    Directory of Open Access Journals (Sweden)

    Ann-Christin Niehoff

    2017-01-01

    Full Text Available Secondary lymphedema accompanied with strong restrictions in quality of life is still major side effects in cancer therapy. Therefore, dedicated diagnostic tools and further investigation of the lymphatic system are crucial to improve lymphedema therapy. In this pilot study, a method for quantitative analysis of the lymphatic system in a rat model by laser ablation (LA with inductively coupled plasma mass spectrometry imaging (ICP-MSI is presented. As a possible lymph marker, thulium(III(1R,4R,7R,10R-α,α′,α′′,α′′′-tetramethyl-1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetate (Tm-DOTMA is introduced and compared to the clinically used magnetic resonance imaging contrast agent gadolinium(III2,2′,2′′-(10-((2R,3S-1,3,4-trihydroxybutan-2-yl-1,4,7,10-tetraazacyclododecane-1,4,7-triyltriacetate (Gd-DO3A-butrol. Gadobutrol functioned as standard contrast media in MRI lymphangiography to detect lymphatic flow qualitatively. Thus, Tm-DOTMA was investigated as lymphatic marker to detect lymphatic flow quantitatively. Both contrast agents were successfully used to visualize the lymphatic flow in successive lymph nodes in LA-ICP-MS due to lower limits of detection compared to MRI. Furthermore, the distribution of contrast agents by multicolored imaging showed accumulation in specific areas (sectors of the lymph nodes after application of contrast agents in different areas.

  9. Mass spectrometry imaging: Towards mapping the elemental and molecular composition of the rhizosphere

    Energy Technology Data Exchange (ETDEWEB)

    Veličković, Dušan; Anderton, Christopher R.

    2017-06-01

    This short review will discuss and provide perspective into the utilization of mass spectrometry imaging (MSI) in studying the rhizosphere. It also serves to compliment the multi-omic focused review by White et al. in this journal issue, as MSI is capable of elucidating chemical distributions within samples of interest in an in situ fashions, and thus can provide spatial context to MS omics data in complementary experimental endeavors. The majority of reported MSI-based studies of plant-microbe interactions have focused on the phyllosphere and ‘associated rhizosphere’ (e.g., material that is not removed during harvesting), as sample preparation for these in situ analyses tends to be a limiting factor. These studies have provided valuable insight into the spatial arrangement of proteins, peptides, lipids, and other metabolites within these systems. We intend for this short review to be a primer about the history of MSI and its role in plant-microbe analysis. Along the way we reference many comprehensive reviews for the interested reader. Lastly, we offer a perspective on the future of MSI and its use in understanding the molecular transformations beyond what we coined as the ‘associated rhizosphere’ to the rest of rhizosphere zone and into the bulk soil.

  10. Fourier Transform Mass Spectrometry.

    Science.gov (United States)

    Gross, Michael L.; Rempel, Don L.

    1984-01-01

    Discusses the nature of Fourier transform mass spectrometry and its unique combination of high mass resolution, high upper mass limit, and multichannel advantage. Examines its operation, capabilities and limitations, applications (ion storage, ion manipulation, ion chemistry), and future applications and developments. (JN)

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

    Directory of Open Access Journals (Sweden)

    N. V. Zarubina

    2014-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2000-04-01

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

  13. Instrumentation for mass spectrometry: 1997

    Energy Technology Data Exchange (ETDEWEB)

    McLuckey, S.A.

    1997-08-01

    All mass spectrometry experiments involve the manipulation of material, an interface with the mass spectrometer, ionization, ion manipulation/analysis, detection and data collection/reduction. Each of these elements involve instrumentation. The wide range of species now amenable to mass spectrometry and the diverse areas of physical science in which it plays a role have led to a seemingly unlimited array of instrumental combinations. However, only a limited number of mass analyzers, and their combinations, dominate. The dominant analyzers include time-of-flight, Fourier transform ion cyclotron resonance, the Paul trap, the mass filter, and the sector mass spectrometer. Why there are so few (or so many, depending upon one`s point of view) can be understood upon consideration of a set of mass analyzer figures of merit. These include mass resolution, mass accuracy, mass range, dynamic range, abundance sensitivity, precision, efficiency, speed, MS{sup n} capability, compatibility with the ionizer, cost, and size. The most appropriate form of mass spectrometry is determined by the priorities of the particular measurement placed on the various mass analyzer characteristics and the relative strengths of the analyzers in meeting the requirements. Each of the analyzer types has a unique set of figures of merit that makes it optimally suited for particular applications. This paper discusses these figures of merit, provides data illustrating recent developments for each analyzer type, and gives the figures of merit of each type of analyzer as they stand in 1997. 101 refs., 24 figs.

  14. Forensic Mass Spectrometry

    Science.gov (United States)

    Hoffmann, William D.; Jackson, Glen P.

    2015-07-01

    Developments in forensic mass spectrometry tend to follow, rather than lead, the developments in other disciplines. Examples of techniques having forensic potential born independently of forensic applications include ambient ionization, imaging mass spectrometry, isotope ratio mass spectrometry, portable mass spectrometers, and hyphenated chromatography-mass spectrometry instruments, to name a few. Forensic science has the potential to benefit enormously from developments that are funded by other means, if only the infrastructure and personnel existed to adopt, validate, and implement the new technologies into casework. Perhaps one unique area in which forensic science is at the cutting edge is in the area of chemometrics and the determination of likelihood ratios for the evaluation of the weight of evidence. Such statistical techniques have been developed most extensively for ignitable-liquid residue analyses and isotope ratio analysis. This review attempts to capture the trends, motivating forces, and likely impact of developing areas of forensic mass spectrometry, with the caveat that none of this research is likely to have any real impact in the forensic community unless: (a) The instruments developed are turned into robust black boxes with red and green lights for positives and negatives, respectively, or (b) there are PhD graduates in the workforce who can help adopt these sophisticated techniques.

  15. Visualizing fossilization using laser ablation-inductively coupled plasma-mass spectrometry maps of trace elements in Late Cretaceous bones

    Science.gov (United States)

    Koenig, A.E.; Rogers, R.R.; Trueman, C.N.

    2009-01-01

    Elemental maps generated by laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) provide a previously unavailable high-resolution visualization of the complex physicochemical conditions operating within individual bones during the early stages of diagenesis and fossilization. A selection of LA-ICP-MS maps of bones collected from the Late Cretaceous of Montana (United States) and Madagascar graphically illustrate diverse paths to recrystallization, and reveal unique insights into geochemical aspects of taphonomic history. Some bones show distinct gradients in concentrations of rare earth elements and uranium, with highest concentrations at external bone margins. Others exhibit more intricate patterns of trace element uptake related to bone histology and its control on the flow paths of pore waters. Patterns of element uptake as revealed by LA-ICP-MS maps can be used to guide sampling strategies, and call into question previous studies that hinge upon localized bulk samples of fossilized bone tissue. LA-ICP-MS maps also allow for comparison of recrystallization rates among fossil bones, and afford a novel approach to identifying bones or regions of bones potentially suitable for extracting intact biogeochemical signals. ?? 2009 Geological Society of America.

  16. Elemental Composition Analysis to Investigate NOx Effects on Secondary Organic Aerosol from α-Pinene Using Ultrahigh Resolution Mass Spectrometry

    Science.gov (United States)

    Lim, H. J.; Park, J. H.; Babar, Z.

    2015-12-01

    Secondary organic aerosol (SOA) accounts for 20-70% of atmospheric fine aerosol. NOx plays crucial roles in SOA formation and consequently affects the composition and yield of SOA. SOA component speciation is incomplete due to its complex composition of polar oxygenated and multifunctional species. In this study, ultrahigh resolution mass spectrometry (UHR MS) was applied to improve the understanding of NOx effects on biogenic SOA formation by identifying the elemental composition of SOA. Additional research aim was to investigate oligomer components that are considered as a driving force for SOA formation and growth. In this study α-pinene SOA from photochemical reaction was examined. SOA formation was performed in the absence and presence of NOx at dry condition (grant funded by the Korea government (MEST) (No. 2011-01350000).

  17. Bioimaging mass spectrometry of trace elements – recent advance and applications of LA-ICP-MS: A review

    Energy Technology Data Exchange (ETDEWEB)

    Becker, J.Sabine, E-mail: s.becker@fz-juelich.de [Central Institute for Engineering, Electronics and Analytics (ZEA-3), Forschungszentrum Jülich, Jülich D-52425 (Germany); Matusch, Andreas, E-mail: a.matusch@fz-juelich.de [Institute for Neuroscience and Medicine (INM-2), Forschungszentrum Jülich, Jülich D-52425 (Germany); Wu, Bei, E-mail: b.wu@fz-juelich.de [Central Institute for Engineering, Electronics and Analytics (ZEA-3), Forschungszentrum Jülich, Jülich D-52425 (Germany)

    2014-07-04

    Highlights: • Bioimaging LA-ICP-MS is established for trace metals within biomedical specimens. • Trace metal imaging allows to study brain function and neurodegenerative diseases. • Laser microdissection ICP-MS was applied to mouse brain hippocampus and wheat root. - Abstract: Bioimaging using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) offers the capability to quantify trace elements and isotopes within tissue sections with a spatial resolution ranging about 10–100 μm. Distribution analysis adds to clarifying basic questions of biomedical research and enables bioaccumulation and bioavailability studies for ecological and toxicological risk assessment in humans, animals and plants. Major application fields of mass spectrometry imaging (MSI) and metallomics have been in brain and cancer research, animal model validation, drug development and plant science. Here we give an overview of latest achievements in methods and applications. Recent improvements in ablation systems, operation and cell design enabled progressively better spatial resolutions down to 1 μm. Meanwhile, a body of research has accumulated covering basic principles of the element architecture in animals and plants that could consistently be reproduced by several laboratories such as the distribution of Fe, Cu, Zn in rodent brain. Several studies investigated the distribution and delivery of metallo-drugs in animals. Hyper-accumulating plants and pollution indicator organisms have been the key topics in environmental science. Increasingly, larger series of samples are analyzed, may it be in the frame of comparisons between intervention and control groups, of time kinetics or of three-dimensional atlas approaches.

  18. Ambient ionization mass spectrometry

    International Nuclear Information System (INIS)

    Lebedev, A T

    2015-01-01

    Ambient ionization mass spectrometry emerged as a new scientific discipline only about ten years ago. A considerable body of information has been reported since that time. Keeping the sensitivity, performance and informativity of classical mass spectrometry methods, the new approach made it possible to eliminate laborious sample preparation procedures and triggered the development of miniaturized instruments to work directly in the field. The review concerns the theoretical foundations and design of ambient ionization methods. Their advantages and drawbacks, as well as prospects for application in chemistry, biology, medicine, environmetal analysis, etc., are discussed. The bibliography includes 194 references

  19. Quantification of elemental mapping of heterogeneous geological sample by laser ablation inductively coupled plasma mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Vaculovič, T.; Breiter, Karel; Korbelová, Zuzana; Venclová, Natalie; Tomková, Kateřina; Jonášová, Šárka; Kanický, V.

    2017-01-01

    Roč. 133, JUL 2017 (2017), s. 200-207 ISSN 0026-265X R&D Projects: GA ČR GA14-13600S Institutional support: RVO:67985831 ; RVO:67985912 Keywords : LA-ICP-MS * induced breakdown spectroscopy * atomic emission spectrometry * in-situ analysis * trace-metals Subject RIV: CB - Analytical Chemistry, Separation; AC - Archeology, Anthropology, Ethnology (ARU-G) OBOR OECD: Analytical chemistry; Archaeology (ARU-G) Impact factor: 3.034, year: 2016

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2001-01-01

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

  2. Miniaturization and Mass Spectrometry

    NARCIS (Netherlands)

    le Gac, S.; le Gac, Severine; van den Berg, Albert; van den Berg, A.; Unknown, [Unknown

    2009-01-01

    With this book we want to illustrate how two quickly growing fields of instrumentation and technology, both applied to life sciences, mass spectrometry and microfluidics (or microfabrication) naturally came to meet at the end of the last century and how this marriage impacts on several types of

  3. Analytical mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    1990-01-01

    This 43rd Annual Summer Symposium on Analytical Chemistry was held July 24--27, 1990 at Oak Ridge, TN and contained sessions on the following topics: Fundamentals of Analytical Mass Spectrometry (MS), MS in the National Laboratories, Lasers and Fourier Transform Methods, Future of MS, New Ionization and LC/MS Methods, and an extra session. (WET)

  4. Analytical mass spectrometry. Abstracts

    Energy Technology Data Exchange (ETDEWEB)

    1990-12-31

    This 43rd Annual Summer Symposium on Analytical Chemistry was held July 24--27, 1990 at Oak Ridge, TN and contained sessions on the following topics: Fundamentals of Analytical Mass Spectrometry (MS), MS in the National Laboratories, Lasers and Fourier Transform Methods, Future of MS, New Ionization and LC/MS Methods, and an extra session. (WET)

  5. Determination of refractive and volatile elements in sediment using laser ablation inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Duodu, Godfred Odame [School of Chemistry, Physics and Mechanical Engineering, Science and Engineering Faculty, Queensland University of Technology (QUT), 2 George St, 4001, QLD (Australia); Goonetilleke, Ashantha [School of Civil Engineering and Built Environment, Science and Engineering Faculty, Queensland University of Technology (QUT), 2 George St, 4001, QLD (Australia); Allen, Charlotte [Institute for Future Environments, Queensland University of Technology (QUT), 2 George St, 4001, QLD (Australia); Ayoko, Godwin A., E-mail: g.ayoko@qut.edu.au [School of Chemistry, Physics and Mechanical Engineering, Science and Engineering Faculty, Queensland University of Technology (QUT), 2 George St, 4001, QLD (Australia)

    2015-10-22

    Wet-milling protocol was employed to produce pressed powder tablets with excellent cohesion and homogeneity suitable for laser ablation (LA) analysis of volatile and refractive elements in sediment. The influence of sample preparation on analytical performance was also investigated, including sample homogeneity, accuracy and limit of detection. Milling in volatile solvent for 40 min ensured sample is well mixed and could reasonably recover both volatile (Hg) and refractive (Zr) elements. With the exception of Cr (−52%) and Nb (+26%) major, minor and trace elements in STSD-1 and MESS-3 could be analysed within ±20% of the certified values. Comparison of the method with total digestion method using HF was tested by analysing 10 different sediment samples. The laser method recovers significantly higher amounts of analytes such as Ag, Cd, Sn and Sn than the total digestion method making it a more robust method for elements across the periodic table. LA-ICP-MS also eliminates the interferences from chemical reagents as well as the health and safety risks associated with digestion processes. Therefore, it can be considered as an enhanced method for the analysis of heterogeneous matrices such as river sediments. - Highlights: • Wet milling was used to produce pressed tablet sediment for LA-ICP-MS analysis. • Milling was effective for refractive elements with narrow range of particle size. • This is the first use of LA-ICP-MS for Hg analysis in sediment samples. • Acceptable accuracy and precision were obtained for most of the elements studied. • Detection limits down to parts per trillion were observed for some elements.

  6. Determination of rare earth elements in environmental matrices by sector-field inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Riondato, J; Vanhaecke, F; Moens, L; Dams, R

    2001-07-01

    In the framework of an international certification campaign, sector-field inductively coupled plasma mass spectrometry (sector-field ICP-MS) was used for the accurate determination of the rare earth elements in five candidate reference materials: aquatic plant, calcareous soil, mussel tissue, river sediment, and tuna muscle. All samples were taken into solution by use of microwave-assisted or mixed microwave-assisted / open beaker acid digestion. Subsequently, the samples were appropriately diluted and subjected to ICP-MS analysis. Except for Sc, all the elements involved were determined at low mass resolution (R = 300). For Sc, application of a higher resolution setting (R = 3,000) was required to separate the analyte signal from those of several molecular ions which gave rise to spectral overlap at low mass resolution. Some of the heavier REE can also suffer from spectral overlap attributed to the occurrence of oxide ions (MO+) of the lighter REE and Ba. This spectral overlap could be successfully overcome by mathematical correction. Matrix effects were overcome by use of two carefully selected internal standards, such that external calibration could be used. On each occasion, a geological reference material was analyzed as a quality-control sample and the reliability of all results obtained was additionally checked by means of chondrite normalization. For tuna muscle the content of all REE was below the limit of detection. For calcareous soil and river sediment, low to sub microg g(-1) values were observed, whereas the REE content of aquatic plant and mussel tissue was considerably lower (low to sub ng g(-1)). Overall, the results obtained were in excellent agreement with the average values, calculated on the basis of all "accepted" values, obtained in different laboratories using different techniques.

  7. Determination of refractive and volatile elements in sediment using laser ablation inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Duodu, Godfred Odame; Goonetilleke, Ashantha; Allen, Charlotte; Ayoko, Godwin A

    2015-10-22

    Wet-milling protocol was employed to produce pressed powder tablets with excellent cohesion and homogeneity suitable for laser ablation (LA) analysis of volatile and refractive elements in sediment. The influence of sample preparation on analytical performance was also investigated, including sample homogeneity, accuracy and limit of detection. Milling in volatile solvent for 40 min ensured sample is well mixed and could reasonably recover both volatile (Hg) and refractive (Zr) elements. With the exception of Cr (-52%) and Nb (+26%) major, minor and trace elements in STSD-1 and MESS-3 could be analysed within ±20% of the certified values. Comparison of the method with total digestion method using HF was tested by analysing 10 different sediment samples. The laser method recovers significantly higher amounts of analytes such as Ag, Cd, Sn and Sn than the total digestion method making it a more robust method for elements across the periodic table. LA-ICP-MS also eliminates the interferences from chemical reagents as well as the health and safety risks associated with digestion processes. Therefore, it can be considered as an enhanced method for the analysis of heterogeneous matrices such as river sediments. Copyright © 2015 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    2002-01-01

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

  9. Advantages and disadvantages of application of inductively coupled plasma mass spectrometry for analysis of trace elements

    International Nuclear Information System (INIS)

    Kovacs, Bela; Borbely, Maria

    2011-01-01

    In this paper the advantages and disadvantages are detailed, moreover special interference effects of the examined elements are evaluated. The detection limits of different ICP-MS instruments are compared. As a result of our research work various solutions are proposed for multielement analysis (e.g. Se, I, Co, As, Te, Cd, Pb and Cr) of the above various samples to reach more accurate and more precise results using ICP-MS instrument

  10. Elemental fractionation in 785 nm picosecond and femtosecond laser ablation inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Shaheen, M.E., E-mail: mshaheen73@science.tanta.edu.eg [Department of Physics, Faculty of Sciences, Tanta University, Tanta (Egypt); Gagnon, J.E.; Fryer, B.J. [Great Lakes Institute for Environmental Research (GLIER), University of Windsor, Windsor, Ontario N9B 3P4 (Canada); Department of Earth and Environmental Sciences, University of Windsor, Windsor, Ontario N9B 3P4 (Canada)

    2015-05-01

    Elemental fractionation and ICP-MS signal response were investigated for two different pulse width laser beams originating from the same laser system. Femtosecond and picosecond laser beams at pulse widths of 130 fs and 110 ps, respectively, and wavelength of 785 nm were used to ablate NIST 610 synthetic glass and SRM 1107 Naval Brass B at the same spot for 800 to 1000 laser pulses at different repetition rates (5 to 50 Hz). Elemental fractionation was found to depend on repetition rate and showed a trend with femtosecond laser ablation that is opposite to that observed in picosecond laser ablation for most measured isotopes. ICP-MS signal intensity was higher in femtosecond than picosecond LA-ICP-MS in both NIST 610 and naval brass when ablation was conducted under the same fluence and repetition rate. The differences in signal intensity were partly related to differences in particle size distribution between particles generated by femtosecond and picosecond laser pulses and the consequent differences in transport and ionization efficiencies. The main reason for the higher signal intensity resulting from femtosecond laser pulses was related to the larger crater sizes compared to those created during picosecond laser ablation. Elemental ratios measured using {sup 66}Zn/{sup 63}Cu, {sup 208}Pb/{sup 238}U, {sup 232}Th/{sup 238}U, {sup 66}Zn/{sup 232}Th and {sup 66}Zn/{sup 208}Pb were found to change with the number of laser pulses with data points being more scattered in picosecond than femtosecond laser pulses. Reproducibility of replicate measurements of signal intensities, fractionation and elemental ratios was better for fs-LA-ICP-MS (RSD ~ 3 to 6%) than ps-LA-ICP-MS (RSD ~ 7 to 11%). - Highlights: • Fractionation and ICP-MS signal response were investigated for two different pulse widths using NIST 610 and Naval Brass. • Dependence of fractionation indices on repetition rate and pulse width. • Higher ablation rate was observed in picosecond compared to

  11. Elemental fractionation in 785 nm picosecond and femtosecond laser ablation inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Shaheen, M.E.; Gagnon, J.E.; Fryer, B.J.

    2015-01-01

    Elemental fractionation and ICP-MS signal response were investigated for two different pulse width laser beams originating from the same laser system. Femtosecond and picosecond laser beams at pulse widths of 130 fs and 110 ps, respectively, and wavelength of 785 nm were used to ablate NIST 610 synthetic glass and SRM 1107 Naval Brass B at the same spot for 800 to 1000 laser pulses at different repetition rates (5 to 50 Hz). Elemental fractionation was found to depend on repetition rate and showed a trend with femtosecond laser ablation that is opposite to that observed in picosecond laser ablation for most measured isotopes. ICP-MS signal intensity was higher in femtosecond than picosecond LA-ICP-MS in both NIST 610 and naval brass when ablation was conducted under the same fluence and repetition rate. The differences in signal intensity were partly related to differences in particle size distribution between particles generated by femtosecond and picosecond laser pulses and the consequent differences in transport and ionization efficiencies. The main reason for the higher signal intensity resulting from femtosecond laser pulses was related to the larger crater sizes compared to those created during picosecond laser ablation. Elemental ratios measured using 66 Zn/ 63 Cu, 208 Pb/ 238 U, 232 Th/ 238 U, 66 Zn/ 232 Th and 66 Zn/ 208 Pb were found to change with the number of laser pulses with data points being more scattered in picosecond than femtosecond laser pulses. Reproducibility of replicate measurements of signal intensities, fractionation and elemental ratios was better for fs-LA-ICP-MS (RSD ~ 3 to 6%) than ps-LA-ICP-MS (RSD ~ 7 to 11%). - Highlights: • Fractionation and ICP-MS signal response were investigated for two different pulse widths using NIST 610 and Naval Brass. • Dependence of fractionation indices on repetition rate and pulse width. • Higher ablation rate was observed in picosecond compared to femtosecond laser ablation of NIST 610 and Brass

  12. Mass spectrometry with accelerators.

    Science.gov (United States)

    Litherland, A E; Zhao, X-L; Kieser, W E

    2011-01-01

    As one in a series of articles on Canadian contributions to mass spectrometry, this review begins with an outline of the history of accelerator mass spectrometry (AMS), noting roles played by researchers at three Canadian AMS laboratories. After a description of the unique features of AMS, three examples, (14)C, (10)Be, and (129)I are given to illustrate the methods. The capabilities of mass spectrometry have been extended by the addition of atomic isobar selection, molecular isobar attenuation, further ion acceleration, followed by ion detection and ion identification at essentially zero dark current or ion flux. This has been accomplished by exploiting the techniques and accelerators of atomic and nuclear physics. In 1939, the first principles of AMS were established using a cyclotron. In 1977 the selection of isobars in the ion source was established when it was shown that the (14)N(-) ion was very unstable, or extremely difficult to create, making a tandem electrostatic accelerator highly suitable for assisting the mass spectrometric measurement of the rare long-lived radioactive isotope (14)C in the environment. This observation, together with the large attenuation of the molecular isobars (13)CH(-) and (12)CH 2(-) during tandem acceleration and the observed very low background contamination from the ion source, was found to facilitate the mass spectrometry of (14)C to at least a level of (14)C/C ~ 6 × 10(-16), the equivalent of a radiocarbon age of 60,000 years. Tandem Accelerator Mass Spectrometry, or AMS, has now made possible the accurate radiocarbon dating of milligram-sized carbon samples by ion counting as well as dating and tracing with many other long-lived radioactive isotopes such as (10)Be, (26)Al, (36)Cl, and (129)I. The difficulty of obtaining large anion currents with low electron affinities and the difficulties of isobar separation, especially for the heavier mass ions, has prompted the use of molecular anions and the search for alternative

  13. Determination of rare earth elements in seawater by inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Moeller, P.; Dulski, P.; Luck, J.

    1992-01-01

    Shortly after sampling, rare earth elements (REEs) from 11.5 l of seawater were concentrated in 35 ml solutions by ion exchange chromatography on board the German research vessel ''Sonne'' using Chelex 100 chelating resin for preconcentration. Two millilitres of a 0.2 μg g -1 Lu spike was added to the seawater samples (i) for monitoring the chemical yield which was always found to vary between 85 and 112% (mean: 100±6) and (ii) as an internal standard. Rare earth elements have been determined by ICP-MS, with REE concentrations ranging from 100 (La) to 1 (Eu) pmol kg -1 . La in blanks can be as high as 30 pmol kg -1 , but blank concentrations for other REEs range between 0.5 and 0.01 pmol kg -1 . The trend of the precision of relative response factors varies between 12% (La) and 4% (Yb). The accuracy is estimated to be about 10% with the exception of La and Ce. Methodology improvements are suggested. (author)

  14. Determination of nutrients and potentially toxic elements in Jatropha curcas seeds, oil and biodiesel using inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Maciel, P.B.; Barros de, L.L.S.; Duarte, E.C.M.; Harder, M.N.C.; Abreu, Jr.C.H.; Villanueva, F.C.A.

    2013-01-01

    Biodiesel is a renewable and biodegradable fuel that can be used in diesel engines as a replacement for fossil diesel. A suitable alternative is to produce it from Jatropha curcas, which has high quality oil concentration. Nevertheless, the presence of particular chemical elements above certain limits can affect the product quality, leading to vehicle engine problems and acting as air pollution source. The objective of this work is to develop a method for the simultaneous determination of B, Na, Mg, P, S, K, Ca, Cr, Mn, Fe, Co, Ni, Cu, Zn, Cd, Ba, and Pb in J. curcas seeds, oil and biodiesel using the inductively coupled plasma mass spectrometry (ICP-MS) technique. This material was evaluated because has been successfully employed in India for biodiesel production as well as in other places where there is an incentive to family farming, without affect the food chain. The oil was obtained from seeds via mechanical extraction and the biodiesel was achieved by oil transesterification. After optimization of the microwave digestion method for the different sample types, the samples were analyzed by ICP-MS. The certified reference material NIST SRM 1515 (apple leaves) and the recovery tests were carried out to ensure the accuracy of the proposed method, which made possible the quantification of several nutrients and potentially toxic elements in J. curcas seeds, oil and biodiesel, especially Na, K, Ca, Mg, P and S in biodiesel which are mandatory analyzed by Petroleum, Natural Gas and Biofuel National Agency (ANP). This work highlights the findings of the first study of potentially toxic and nutrient elements in the production chain steps seed-oil-biodiesel from J. curcas. (author)

  15. Hydrogen-Deuterium Exchange Mass Spectrometry Reveals Calcium Binding Properties and Allosteric Regulation of Downstream Regulatory Element Antagonist Modulator (DREAM).

    Science.gov (United States)

    Zhang, Jun; Li, Jing; Craig, Theodore A; Kumar, Rajiv; Gross, Michael L

    2017-07-18

    Downstream regulatory element antagonist modulator (DREAM) is an EF-hand Ca 2+ -binding protein that also binds to a specific DNA sequence, downstream regulatory elements (DRE), and thereby regulates transcription in a calcium-dependent fashion. DREAM binds to DRE in the absence of Ca 2+ but detaches from DRE under Ca 2+ stimulation, allowing gene expression. The Ca 2+ binding properties of DREAM and the consequences of the binding on protein structure are key to understanding the function of DREAM. Here we describe the application of hydrogen-deuterium exchange mass spectrometry (HDX-MS) and site-directed mutagenesis to investigate the Ca 2+ binding properties and the subsequent conformational changes of full-length DREAM. We demonstrate that all EF-hands undergo large conformation changes upon calcium binding even though the EF-1 hand is not capable of binding to Ca 2+ . Moreover, EF-2 is a lower-affinity site compared to EF-3 and -4 hands. Comparison of HDX profiles between wild-type DREAM and two EF-1 mutated constructs illustrates that the conformational changes in the EF-1 hand are induced by long-range structural interactions. HDX analyses also reveal a conformational change in an N-terminal leucine-charged residue-rich domain (LCD) remote from Ca 2+ -binding EF-hands. This LCD domain is responsible for the direct interaction between DREAM and cAMP response element-binding protein (CREB) and regulates the recruitment of the co-activator, CREB-binding protein. These long-range interactions strongly suggest how conformational changes transmit the Ca 2+ signal to CREB-mediated gene transcription.

  16. Laser ablation inductively coupled plasma dynamic reaction cell mass spectrometry for the multi-element analysis of polymers

    Science.gov (United States)

    Resano, M.; García-Ruiz, E.; Vanhaecke, F.

    2005-11-01

    In this work, the potential of laser ablation-inductively coupled plasma-mass spectrometry for the fast analysis of polymers has been explored. Different real-life samples (polyethylene shopping bags, an acrylonitrile butadiene styrene material and various plastic bricks) as well as several reference materials (VDA 001 to 004, Cd in polyethylene) have been selected for the study. Two polyethylene reference materials (ERM-EC 680 and 681), for which a reference or indicative value for the most relevant metals is available, have proved their suitability as standards for calibration. Special attention has been paid to the difficulties expected for the determination of Cr at the μg g - 1 level in this kind of materials, due to the interference of ArC + ions on the most abundant isotopes of Cr. The use of ammonia as a reaction gas in a dynamic reaction cell is shown to alleviate this problem, resulting in a limit of detection of 0.15 μg g - 1 for this element, while limiting only modestly the possibilities of the technique for simultaneous multi-element analysis. In this regard, As is the analyte most seriously affected by the use of ammonia, and its determination has to be carried out in vented mode, at the expense of measuring time. In all cases studied, accurate results could be obtained for elements ranging in content from the sub-μg g - 1 level to tens of thousands of μg g - 1 . However, the use of an element of known concentration as internal standard may be needed for materials with a matrix significantly different from that of the standard (polyethylene in this work). Precision ranged between 5% and 10% RSD for elements found at the 10 μg g - 1 level or higher, while this value could deteriorate to 20% for analytes found at the sub-μg g - 1 level. Overall, the technique evaluated presents many advantages for the fast and accurate multi-element analysis of these materials, avoiding laborious digestion procedures and minimizing the risk of analyte losses due

  17. Hydrogen Exchange Mass Spectrometry

    Science.gov (United States)

    Mayne, Leland

    2018-01-01

    Hydrogen exchange (HX) methods can reveal much about the structure, energetics, and dynamics of proteins. The addition of mass spectrometry (MS) to an earlier fragmentation-separation HX analysis now extends HX studies to larger proteins at high structural resolution and can provide information not available before. This chapter discusses experimental aspects of HX labeling, especially with respect to the use of MS and the analysis of MS data. PMID:26791986

  18. Stable isotope mass spectrometry in petroleum exploration

    International Nuclear Information System (INIS)

    Mathur, Manju

    1997-01-01

    The stable isotope mass spectrometry plays an important role to evaluate the stable isotopic composition of hydrocarbons. The isotopic ratios of certain elements in petroleum samples reflect certain characteristics which are useful for petroleum exploration

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

    Science.gov (United States)

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

    2012-08-01

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

  20. Elemental analysis of forensic glasses by inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Almirall, Jose R.; Duckworth, Douglas C.; Bayne, Charles K.; Morton, Sherman A.; Smith, David H.; Koons, Robert D.; Furton, Kenneth G.

    1999-02-01

    Flat glass is a common type of evidence collected from the scenes of crimes such as burglaries, vandalism, and hit-and- run accidents. The usefulness of such evidence lies in the ability to associate the glass from the scene (or a suspect) to the original source. Physical and chemical analysis of the glass can be used for discrimination between the possible sources of glass. If the sample is large enough, physical attributes such as fracture matches, density, color, and thickness can be employed for comparison between a recovered fragment(s) to the suspect source. More commonly, refractive index (RI) comparisons are employed. Due to the improved control over glass manufacturing processes, RI values often cannot differentiate glasses where approximately 6 - 9% of casework samples are not expected to be distinguished by RI alone even if they originated from different sources. Employing methods such as NAA, XRF, ICP-AES, and ICP-MS for the comparison of trace elemental compositions has been shown to be more discriminating than RI comparisons. The multielement capability and the sensitivity of ICP-AES and ICP-MS provide for excellent discrimination power. In this work, the sources of variability in ICP-MS of glass analysis are investigated to determine possible sources of variation. The sources of variation examined include errors due to sample preparation, instrument accuracy and precision, and interlaboratory reproducibility. Other sources of variation include inhomogeneity across a sheet of glass from the same source. Analysis of variance has been applied to our ICP-MS analysis of NIST standards and to the interlaboratory comparisons of float glass samples collected across a sheet in a production facility. The results of these experiments allows for a more accurate interpretation of forensic glass data and a better understanding of the discriminating power (absolute and practical) of ICP-MS.

  1. Determination of rare earth elements, thorium and uranium by inductively coupled plasma mass spectrometry and strontium isotopes by thermal ionization mass spectrometry in soil samples of Bryansk region contaminated due to Chernobyl accident

    International Nuclear Information System (INIS)

    Sahoo, S.K.; Yonehara, H.; Kurotaki, K.; Shiraishi, K.; Ramzaev, V.; Barkovski, A.

    2001-01-01

    Inductively coupled plasma mass spectrometric (ICP-MS) determination of rare earth elements (REEs), thorium and uranium in forest, pasture, field and kitchen garden soils from a Russian territory and in certified reference materials (JLK-1, JSD-2 and BCR-1) is described. In addition to concentration data, strontium isotopic composition of the soil samples were measured by thermal ionization mass spectrometry. The measurements contributed to the understanding of the background levels of these elements in an area contaminated due to Chernobyl accident. There was not a significant variation in the concentration of REEs at different depth levels in forest soil samples, however, the ratio of Th/U varied from 3.32 to 3.60. Though concentration of U and Th varied to some extent, the ratio did not show much variation. The value of 87 Sr/ 86 Sr ratio, was in the top layer soil sample relatively higher than in the lower layers. (author)

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

    International Nuclear Information System (INIS)

    Ozturk, Yildirim; Benderli, Cihan

    2010-01-01

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

  3. 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. Copyright © 2015 Elsevier GmbH. All rights reserved.

  4. Mass spectrometry of long-lived radionuclides

    International Nuclear Information System (INIS)

    Becker, Johanna Sabine.

    2003-01-01

    The capability of determining element concentrations at the trace and ultratrace level and isotope ratios is a main feature of inorganic mass spectrometry. The precise and accurate determination of isotope ratios of long-lived natural and artificial radionuclides is required, e.g. for their environmental monitoring and health control, for studying radionuclide migration, for age dating, for determining isotope ratios of radiogenic elements in the nuclear industry, for quality assurance and determination of the burn-up of fuel material in a nuclear power plant, for reprocessing plants, nuclear material accounting and radioactive waste control. Inorganic mass spectrometry, especially inductively coupled plasma mass spectrometry (ICP-MS) as the most important inorganic mass spectrometric technique today, possesses excellent sensitivity, precision and good accuracy for isotope ratio measurements and practically no restriction with respect to the ionization potential of the element investigated--therefore, thermal ionization mass spectrometry (TIMS), which has been used as the dominant analytical technique for precise isotope ratio measurements of long-lived radionuclides for many decades, is being replaced increasingly by ICP-MS. In the last few years instrumental progress in improving figures of merit for the determination of isotope ratio measurements of long-lived radionuclides in ICP-MS has been achieved by the application of a multiple ion collector device (MC-ICP-MS) and the introduction of the collision cell interface in order to dissociate disturbing argon-based molecular ions, to reduce the kinetic energy of ions and neutralize the disturbing noble gas ions (e.g. of 129 Xe + for the determination of 129 I). The review describes the state of the art and the progress of different inorganic mass spectrometric techniques such as ICP-MS, laser ablation ICP-MS vs. TIMS, glow discharge mass spectrometry, secondary ion mass spectrometry, resonance ionization mass

  5. 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)

    Popp, Maximilian; Hann, Stephan; Koellensperger, Gunda

    2010-01-01

    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.

  6. The use of inductively coupled plasma mass spectrometry (ICP-MS) for the determination of toxic and essential elements in different types of food samples

    Science.gov (United States)

    Voica, C.; Dehelean, A.; Kovacs, M. H.

    2012-02-01

    Food is the primary source of essential elements for humans and it is an important source of exposure to toxic elements. In this context, levels of essential and toxic elements must be determined routinely in consumed food products. The content of trace elements (As, Pb, Cu, Cd, Zn, Sn, Hg) in different types of food samples (e.g. rice, bread, sugar, cheese, milk, butter, wheat, coffee, chocolate, biscuits pasta, etc.) was determined, using inductively coupled plasma mass spectrometry (ICP-MS). Trace element contents in some foods were higher than maximum permissible levels of toxic metals in human food (Cd in bread, Zn in cheese, Cu in coffee, Hg in carrots and peppers).

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-04-17

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

  8. Ion detection in mass spectrometry

    International Nuclear Information System (INIS)

    Bolbach, Gerard

    2016-03-01

    This course aims at providing some elements for a better understanding of ion detectors used in mass spectrometers, of their operations, and of their limitations. A first part addresses the functions and properties of an ideal detector, how to detect ions in gas phase, and particle detectors and ion detectors used in mass spectrometry. The second part proposes an overview of currently used detectors with respect to their operation principle: detection from the ion charge (Faraday cylinder), detection by inductive effects (FTICR, Fourier Transform Ion Cyclotron Resonance), and detection by secondary electron emission. The third part discusses the specificities of secondary electron emission. The fourth one addresses operating modes and parameters related to detectors. The sixth part proposes a prospective view on future detectors by addressing the following issues: cryo-detector, inductive effect and charge detectors, ion detection and nano materials

  9. On the prospects to detect superheavy elements (SHE) in the earth's crust using the high energy synchrotron radiation and the mass spectrometry

    International Nuclear Information System (INIS)

    Schnier, C.

    2001-01-01

    There are many indications for the existence of superheavy elements (SHE) in the Earth's crust. The appropriate detection methods are X-ray fluorescence (XRF) using the high energy synchrotron radiation and the mass spectrometry. The characteristic X-rays of each element up to Z >120 (corresponding binding energy of the K-electrons E b >230 keV) can be precisely excited with synchrotron XRF. Up to now, the XRF with high energy photons has never been applied to the quest for SHE. New methods of mass spectrometry eg using resonance ionization (RIMS) are promising to detect unambiguously atomic masses about 300 in solid matrices. It is proposed to restart the quest for SHE in the nature. Finding a SHE in the Earth's crust would be very important, because of what it will tell us about the origin of the elements eg about the nucleosynthesis during a super nova explosion, the structure of the atomic nuclei and the site of SHE in the periodic table of elements. (orig.) [de

  10. Preface Miniaturization and Mass Spectrometry

    NARCIS (Netherlands)

    Unknown, [Unknown; le Gac, Severine; le Gac, S.; van den Berg, Albert; van den Berg, A.

    2009-01-01

    Miniaturization and Mass Spectrometry illustrates this trend and focuses on one particular analysis technique, mass spectrometry whose popularity has "dramatically" increased in the last two decades with the explosion of the field of biological analysis and the development of two "soft" ionization

  11. Negative chemical ionization mass spectrometry

    International Nuclear Information System (INIS)

    Smit, A.L.C.

    1979-01-01

    This thesis describes some aspects of Negative Chemical Ionization (NCI) mass spectrometry. The reasons for the growing interest in NCI are: (i) to extend the basic knowledge of negative ions and their reactions in the gas phase; (ii) to investigate whether or not this knowledge of negative ions can be used successfully to elucidate the structure of molecules by mass spectrometry. (Auth.)

  12. Laboratory of acceleration mass spectrometry

    International Nuclear Information System (INIS)

    Hybler, P.; Chrapan, J.

    2002-01-01

    In this paper authors describe the principle of the method of acceleration mass spectrometry and the construction plans of this instrument at the Faculty of ecology and environmental sciences in Banska Stiavnica. Using of this instrument for radiocarbon dating is discussed. A review of laboratories with acceleration mass spectrometry is presented

  13. Determination of the distribution of uranium and the transuranic elements in the environment by thermal ionization mass spectrometry

    International Nuclear Information System (INIS)

    Chastagner, P.

    1987-01-01

    Protection of the world population from releases of uranium, plutonium, and other transuranic materials requires, among other things, a knowledge of the sources, transport, and distribution of these elements in the environment. Both isotopic and quantitative analytical data are required in the determination of these factors. Also, the analyses must be precise and accurate enough to distinguish newly released material from older material such as the worldwide deposits from atmospheric weapons testing. For this reason, uranium, neptunium, and plutonium and other transuranic elements in the environment are routinely determined by high-sensitivity thermal ionization mass spectrometric techniques. With current instrumentation and techniques, routine isotope dilution and isotopic analyses are made with purified elemental samples as small as 2 x 10 -14 g. The detection limit for uranium and most of the transuranic isotopes is ∼ 5 x 10 18 g (∼ 13,000 atoms), which is at least an order of magnitude better than the detection limits of the radiometric counting techniques normally employed. The mass spectral sensitivities are equal for all of the isotopes of a given element but vary from element to element. Thus, each elemental sample must be highly purified. Separation techniques recover ∼ 80% of the uranium and the transuranic material from soils and other materials. Interelement separation factors > 10 5 are achieved with advanced ion exchange methods. Results of recent application of these techniques at the Savannah River Lab. and other laboratories are include

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

  15. Direct determination of trace rare earth elements in ancient porcelain samples with slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Xiang Guoqiang; Jiang Zucheng; He Man; Hu Bin

    2005-01-01

    A method for the direct determination of trace rare earth elements in ancient porcelain samples by slurry sampling fluorinating electrothermal vaporization inductively coupled plasma mass spectrometry was developed with the use of polytetrafluoroethylene as fluorinating reagent. It was found that Si, as a main matrix element in ancient porcelain sample, could be mostly removed at the ashing temperature of 1200 deg. C without considerable losses of the analytes. However, the chemical composition of ancient porcelain sample is very complicated, which makes the influences resulting from other matrix elements not be ignored. Therefore, the matrix effect of ancient porcelain sample was also investigated, and it was found that the matrix effect is obvious when the matrix concentration was larger than 0.8 g l -1 . The study results of particle size effect indicated that when the sample particle size was less than 0.057 mm, the particle size effect is negligible. Under the optimized operation conditions, the detection limits for rare earth elements by fluorinating electrothermal vaporization inductively coupled plasma mass spectrometry were 0.7 ng g -1 (Eu)-33.3 ng g -1 (Nd) with the precisions of 4.1% (Yb)-10% (La) (c = 1 μg l -1 , n = 9). The proposed method was used to directly determine the trace rare earth elements in ancient porcelain samples produced in different dynasty (Sui, Ming and Qing), and the analytical results are satisfactory

  16. Thermal ionisation mass spectrometry (TIMS): what, how and why?

    International Nuclear Information System (INIS)

    Aggarwal, S.K.

    2002-01-01

    Thermal ionisation mass spectrometry (TIMS) is one of the oldest mass spectrometric techniques, which has been used for determining the isotopic composition and concentration of different elements using isotope dilution. In spite of the introduction of many other inorganic mass spectrometric techniques like spark source mass spectrometry (SSMS), glow discharge mass spectrometry (GDMS), inductively coupled plasma-mass spectrometry (ICP-MS), secondary ion mass spectrometry (SIMS), the TIMS technique plays the role of a definitive analytical methodology and still occupies a unique position in terms of its capabilities with respect to precision and accuracy as well as sensitivity

  17. Accelerator mass spectrometry.

    Science.gov (United States)

    Hellborg, Ragnar; Skog, Göran

    2008-01-01

    In this overview the technique of accelerator mass spectrometry (AMS) and its use are described. AMS is a highly sensitive method of counting atoms. It is used to detect very low concentrations of natural isotopic abundances (typically in the range between 10(-12) and 10(-16)) of both radionuclides and stable nuclides. The main advantages of AMS compared to conventional radiometric methods are the use of smaller samples (mg and even sub-mg size) and shorter measuring times (less than 1 hr). The equipment used for AMS is almost exclusively based on the electrostatic tandem accelerator, although some of the newest systems are based on a slightly different principle. Dedicated accelerators as well as older "nuclear physics machines" can be found in the 80 or so AMS laboratories in existence today. The most widely used isotope studied with AMS is 14C. Besides radiocarbon dating this isotope is used in climate studies, biomedicine applications and many other fields. More than 100,000 14C samples are measured per year. Other isotopes studied include 10Be, 26Al, 36Cl, 41Ca, 59Ni, 129I, U, and Pu. Although these measurements are important, the number of samples of these other isotopes measured each year is estimated to be less than 10% of the number of 14C samples. Copyright 2008 Wiley Periodicals, Inc.

  18. Imaging mass spectrometry statistical analysis.

    Science.gov (United States)

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

    2012-08-30

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

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

    International Nuclear Information System (INIS)

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

    1990-01-01

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

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

    Science.gov (United States)

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

    2011-01-01

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

  1. Accelerator-based ultrasensitive mass spectrometry

    International Nuclear Information System (INIS)

    Gove, H.E.

    1985-01-01

    This chapter describes a new mass spectrometry technique involving charged particle accelerators normally used for basic research in nuclear science. Topics considered include the limitations of conventional mass spectrometry, the limitations of the direct measurement of radioactive decay, mass spectrometry using a tandem electrostatic accelerator, mass spectrometry using a cyclotron, how accelerator mass spectrometry circumvents the limitations of conventional mass spectrometry, measurements of stable isotopes, nuclear physics and astrophysics applications, modifications to existing accelerators, descriptions of dedicated systems, and future applications

  2. Ultra-sensitive quantification of lysozyme based on element chelate labeling and capillary electrophoresis–inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Yang, MingWei; Wu, WeiHua; Ruan, YaJuan; Huang, LiMei; Wu, Zujian; Cai, Yong; Fu, FengFu

    2014-01-01

    Graphical abstract: An ultra-sensitive method for the determination of lysozyme was developed based on the Gd 3+ chelate labeling and CE–ICP–MS. The proposed method has an extremely low detection limit of 3.89 attomole and has been successfully used to detect lysozyme in saliva sample, showing excellent reliability. The success of the present method provides a new possibility for biological assays and clinical diagnoses. -- Highlights: •An ultra-sensitive method for detecting lysozyme based on CE–ICP–MS was described. •The proposed method has an extremely low detection limit of 3.89 attomole. •It can be used to detect trace lysozyme in saliva sample with a satisfied recovery. •The method provides a new potential for sensitive detection of low-abundant proteins. -- Abstract: In this study, an ultra-sensitive method for the quantification of lysozyme based on the Gd 3+ diethylenetriamine-N,N,N′,N″,N″-pentaacetic acid labeling and capillary electrophoresis–inductively coupled plasma mass spectrometry (CE–ICP–MS) was described. The Gd 3+ -tagged lysozyme was effectively separated by capillary electrophoresis (CE) and sensitively determined by inductively coupled plasma mass spectrometry (ICP–MS). Based on the gadolinium-tagging and CE–ICP–MS, the lysozyme was determined within 12 min with an extremely low detection limit of 3.89 attomole (3.89 × 10 −11 mol L −1 for 100 nL of sample injection) and a RSD < 6% (n = 5). The proposed method has been successfully used to detect lysozyme in saliva samples with a recovery of 91–106%, suggesting that our method is sensitive and reliable. The success of the present method provides a new potential for the biological assays and sensitive detection of low-abundant proteins

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

    International Nuclear Information System (INIS)

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

    1979-01-01

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

  4. Guideline on Isotope Dilution Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-05-19

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

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

    Directory of Open Access Journals (Sweden)

    Nigel Cook

    2016-10-01

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

  6. The matrix effect of biological concomitant element on the signal intensity of Ge, As, and Se in inductively coupled plasma/mass spectrometry

    International Nuclear Information System (INIS)

    Park, Kyung Su; Kim, Sun Tae; Kim, Young Man; Kim, Yun Je; Lee, Won

    2002-01-01

    The non-spectroscopic interference effects that occurred in inductively coupled plasma/mass spectrometry were studied for Ge, As and Se in human urine and serum. Many biological samples contain Na, K, Cl and organic compounds, which may cause the enhancement and depression on the analyte signal. The effect of 1% concomitant elements such as N, Cl, S, P, C, Na, and K on a 100 μg/L germanium, arsenic and selenium signal has been investigated by ICP/MS. The interference effects were not in the same direction. It appeared that concomitant elements such as Cl, S and C induce an enhancement effect, whereas N and P did not show any significant effect. And, Na and K caused a depression . We have found a link between the abundance of analytes and the ionization potential of concomitant elements (eV), except carbon and nitrogen

  7. Mass Spectrometry of Halopyrazolium Salts

    DEFF Research Database (Denmark)

    Larsen, Elfinn; Egsgaard, Helge; Pande, U. C.

    1983-01-01

    Eleven halogen substituted 1-methyl-2-phenylpyrazolium bromides or chlorides were investigated by field desorption, field ionization, and electron impact mass spectrometry. Dealkylation was found to be the predominant thermal decomposition. An exchange between covalent and ionic halogen prior...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-11-15

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

  9. Cluster secondary ion mass spectrometry microscope mode mass spectrometry imaging.

    Science.gov (United States)

    Kiss, András; Smith, Donald F; Jungmann, Julia H; Heeren, Ron M A

    2013-12-30

    Microscope mode imaging for secondary ion mass spectrometry is a technique with the promise of simultaneous high spatial resolution and high-speed imaging of biomolecules from complex surfaces. Technological developments such as new position-sensitive detectors, in combination with polyatomic primary ion sources, are required to exploit the full potential of microscope mode mass spectrometry imaging, i.e. to efficiently push the limits of ultra-high spatial resolution, sample throughput and sensitivity. In this work, a C60 primary source was combined with a commercial mass microscope for microscope mode secondary ion mass spectrometry imaging. The detector setup is a pixelated detector from the Medipix/Timepix family with high-voltage post-acceleration capabilities. The system's mass spectral and imaging performance is tested with various benchmark samples and thin tissue sections. The high secondary ion yield (with respect to 'traditional' monatomic primary ion sources) of the C60 primary ion source and the increased sensitivity of the high voltage detector setup improve microscope mode secondary ion mass spectrometry imaging. The analysis time and the signal-to-noise ratio are improved compared with other microscope mode imaging systems, all at high spatial resolution. We have demonstrated the unique capabilities of a C60 ion microscope with a Timepix detector for high spatial resolution microscope mode secondary ion mass spectrometry imaging. Copyright © 2013 John Wiley & Sons, Ltd.

  10. 2D elemental mapping of sections of human kidney stones using laser ablation inductively-coupled plasma-mass spectrometry: Possibilities and limitations

    Energy Technology Data Exchange (ETDEWEB)

    Vašinová Galiová, Michaela [Department of Chemistry, Faculty of Science, Masaryk University, Kotlářská 2, 611 37 Brno (Czech Republic); Central European Institute of Technology (CEITEC), Masaryk University, Kamenice 5, 625 00 Brno (Czech Republic); Čopjaková, Renata; Škoda, Radek [Department of Geological Sciences, Faculty of Science, Masaryk University, Kotlářská 2, 611 37 Brno (Czech Republic); Štěpánková, Kateřina; Vaňková, Michaela [Department of Chemistry, Faculty of Science, Masaryk University, Kotlářská 2, 611 37 Brno (Czech Republic); Kuta, Jan [Research Centre for Toxic Compounds in the Environment (RECETOX), Masaryk University, Kamenice 126/3, 625 00 Brno (Czech Republic); Prokeš, Lubomír [Department of Chemistry, Faculty of Science, Masaryk University, Kotlářská 2, 611 37 Brno (Czech Republic); Department of Physical Electronics, Faculty of Science, Masaryk University, Kotlářská 2, 611 37 Brno (Czech Republic); Kynický, Jindřich [Department of Pedology and Geology, Faculty of Forestry and Wood Technology, Mendel University in Brno, Zemědělská 3, 613 00 Brno (Czech Republic); and others

    2014-10-01

    A 213 nm Nd:YAG-based laser ablation (LA) system coupled to quadrupole-based inductively coupled plasma-mass spectrometer and an ArF* excimer-based LA-system coupled to a double-focusing sector field inductively coupled plasma-mass spectrometer were employed to study the spatial distribution of various elements in kidney stones (uroliths). Sections of the surfaces of uroliths were ablated according to line patterns to investigate the elemental profiles for the different urolith growth zones. This exploratory study was mainly focused on the distinguishing of the main constituents of urinary calculus fragments by means of LA-ICP-mass spectrometry. Changes in the ablation rate for oxalate and phosphate phases related to matrix density and hardness are discussed. Elemental association was investigated on the basis of 2D mapping. The possibility of using NIST SRM 1486 Bone Meal as an external standard for calibration was tested. It is shown that LA-ICP-MS is helpful for determination of the mineralogical composition and size of all phases within the analyzed surface area, for tracing down elemental associations and for documenting the elemental content of urinary stones. LA-ICP-MS results (elemental contents and maps) are compared to those obtained with electron microprobe analysis and solution analysis ICP-MS. - Highlights: • Elements in phosphate and oxalate urolith phases were quantified by LA-ICP-MS. • SRM NIST 1486 Bone Meal was proved suitable for quantification in uroliths. • Different ablation rates in particular phases were included at quantification. • Oxalate and apatite phases show opposite hardness order to natural minerals. • Uroliths were classified according to elemental association to phases.

  11. Inductively coupled plasma- mass spectrometry. Chapter 13

    International Nuclear Information System (INIS)

    Mahalingam, T.R.

    1997-01-01

    Inductively Coupled Plasma - Mass Spectrometry (ICP-MS) is a new technique for elemental and isotopic analysis which is currently attracting a great deal of interest. This relatively new technique has found wide applications in different fields of research viz., nuclear, geological, biological and environmental sciences

  12. Mass spectrometry. [in organic chemistry

    Science.gov (United States)

    Burlingame, A. L.; Shackleton, C. H. L.; Howe, I.; Chizhov, O. S.

    1978-01-01

    A review of mass spectrometry in organic chemistry is given, dealing with advances in instrumentation and computer techniques, selected topics in gas-phase ion chemistry, and applications in such fields as biomedicine, natural-product studies, and environmental pollution analysis. Innovative techniques and instrumentation are discussed, along with chromatographic-mass spectrometric on-line computer techniques, mass spectral interpretation and management techniques, and such topics in gas-phase ion chemistry as electron-impact ionization and decomposition, photoionization, field ionization and desorption, high-pressure mass spectrometry, ion cyclotron resonance, and isomerization reactions of organic ions. Applications of mass spectrometry are examined with respect to bio-oligomers and their constituents, biomedically important substances, microbiology, environmental organic analysis, and organic geochemistry.

  13. Mass Spectrometry Instrumentation in Proteomics

    DEFF Research Database (Denmark)

    Sprenger, Richard Remko; Roepstorff, Peter

    2012-01-01

    Mass spectrometry has evolved into a crucial technology for the field of proteomics, enabling the comprehensive study of proteins in biological systems. Innovative developments have yielded flexible and versatile mass spectrometric tools, including quadrupole time-of-flight, linear ion trap......, Orbitrap and ion mobility instruments. Together they offer various and complementary capabilities in terms of ionization, sensitivity, speed, resolution, mass accuracy, dynamic range and methods of fragmentation. Mass spectrometers can acquire qualitative and quantitative information on a large scale...

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  15. Mass spectrometry in nuclear science and technology

    International Nuclear Information System (INIS)

    Komori, Takuji

    1985-01-01

    Mass spectrometry has been widely used and playing a very important role in the field of nuclear science and technology. A major reason for this is that not only the types of element but also its isotopes have to be identified and measured in this field. Thus, some applications of this analytical method are reviewed and discussed in this article. Its application to analytical chemistry is described in the second section following an introductory section, which includes subsections for isotropic dilution mass spectrometry, resonance ionization mass spectrometry and isotopic correlation technique. The isotopic ratio measurement for hydrogen, uranium and plutonium as well as nuclear material control and safeguards are also reviewed in this section. In the third section, mass spectrometry is discussed in relation to nuclear reactors, with subsections on natural uranium reactor and neutron flux observation. Some techniques for measuring the burnup fraction, including the heavy isotopic ratio method and fission product monitoring, are also described. In the fourth section, application of mass spectrometry to measurement of nuclear constants, such as ratio of effective cross-sectional area for 235 U, half-life and fission yield is reviewed. (Nogami, K.)

  16. Preliminary study to characterize plastic polymers using elemental analyser/isotope ratio mass spectrometry (EA/IRMS).

    Science.gov (United States)

    Berto, Daniela; Rampazzo, Federico; Gion, Claudia; Noventa, Seta; Ronchi, Francesca; Traldi, Umberto; Giorgi, Giordano; Cicero, Anna Maria; Giovanardi, Otello

    2017-06-01

    Plastic waste is a growing global environmental problem, particularly in the marine ecosystems, in consideration of its persistence. The monitoring of the plastic waste has become a global issue, as reported by several surveillance guidelines proposed by Regional Sea Conventions (OSPAR, UNEP) and appointed by the EU Marine Strategy Framework Directive. Policy responses to plastic waste vary at many levels, ranging from beach clean-up to bans on the commercialization of plastic bags and to Regional Plans for waste management and recycling. Moreover, in recent years, the production of plant-derived biodegradable plastic polymers has assumed increasing importance. This study reports the first preliminary characterization of carbon stable isotopes (δ 13 C) of different plastic polymers (petroleum- and plant-derived) in order to increase the dataset of isotopic values as a tool for further investigation in different fields of polymers research as well as in the marine environment surveillance. The δ 13 C values determined in different packaging for food uses reflect the plant origin of "BIO" materials, whereas the recycled plastic materials displayed a δ 13 C signatures between plant- and petroleum-derived polymers source. In a preliminary estimation, the different colours of plastic did not affect the variability of δ 13 C values, whereas the abiotic and biotic degradation processes that occurred in the plastic materials collected on beaches and in seawater, showed less negative δ 13 C values. A preliminary experimental field test confirmed these results. The advantages offered by isotope ratio mass spectrometry with respect to other analytical methods used to characterize the composition of plastic polymers are: high sensitivity, small amount of material required, rapidity of analysis, low cost and no limitation in black/dark samples compared with spectroscopic analysis. Copyright © 2017 Elsevier Ltd. All rights reserved.

  17. Symposium on accelerator mass spectrometry

    International Nuclear Information System (INIS)

    1981-01-01

    The area of accelerator mass spectrometry has expanded considerably over the past few years and established itself as an independent and interdisciplinary research field. Three years have passed since the first meeting was held at Rochester. A Symposium on Accelerator Mass Spectrometry was held at Argonne on May 11-13, 1981. In attendance were 96 scientists of whom 26 were from outside the United States. The present proceedings document the program and excitement of the field. Papers are arranged according to the original program. A few papers not presented at the meeting have been added to complete the information on the status of accelerator mass spectrometry. Individual papers were prepared separately for the data base

  18. Symposium on accelerator mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    None

    1981-01-01

    The area of accelerator mass spectrometry has expanded considerably over the past few years and established itself as an independent and interdisciplinary research field. Three years have passed since the first meeting was held at Rochester. A Symposium on Accelerator Mass Spectrometry was held at Argonne on May 11-13, 1981. In attendance were 96 scientists of whom 26 were from outside the United States. The present proceedings document the program and excitement of the field. Papers are arranged according to the original program. A few papers not presented at the meeting have been added to complete the information on the status of accelerator mass spectrometry. Individual papers were prepared separately for the data base.

  19. Mass spectrometry for biomarker development

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Chaochao; Liu, Tao; Baker, Erin Shammel; Rodland, Karin D.; Smith, Richard D.

    2015-06-19

    Biomarkers potentially play a crucial role in early disease diagnosis, prognosis and targeted therapy. In the past decade, mass spectrometry based proteomics has become increasingly important in biomarker development due to large advances in technology and associated methods. This chapter mainly focuses on the application of broad (e.g. shotgun) proteomics in biomarker discovery and the utility of targeted proteomics in biomarker verification and validation. A range of mass spectrometry methodologies are discussed emphasizing their efficacy in the different stages in biomarker development, with a particular emphasis on blood biomarker development.

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

  1. Method for the elucidation of the elemental composition of low molecular mass chemicals using exact masses of product ions and neutral losses: application to environmental chemicals measured by liquid chromatography with hybrid quadrupole/time-of-flight mass spectrometry.

    Science.gov (United States)

    Suzuki, Shigeru; Ishii, Tetsuko; Yasuhara, Akio; Sakai, Shinichi

    2005-01-01

    A method for elucidating the elemental compositions of low molecular weight chemicals, based primarily on mass measurements made using liquid chromatography (LC) with time-of-flight mass spectrometry (TOFMS) and quadrupole/time-of-flight mass spectrometry (LC/QTOFMS), was developed and tested for 113 chemicals of environmental interest with molecular masses up to approximately 400 Da. As the algorithm incorporating the method is not affected by differences in the instrument used, or by the ionization method and other ionization conditions, the method is useful not only for LC/TOFMS, but also for all kinds of mass spectra measured with higher accuracy and precision (uncertainties of a few mDa) employing all ionization methods and on-line separation techniques. The method involves calculating candidate compositions for intact ionized molecules (ionized forms of the sample molecule that have lost or gained no more than a proton, i.e., [M+H](+) or [M-H](-)) as well as for fragment ions and corresponding neutral losses, and eliminating those atomic compositions for the molecules that are inconsistent with the corresponding candidate compositions of fragment ions and neutral losses. Candidate compositions were calculated for the measured masses of the intact ionized molecules and of the fragment ions and corresponding neutral losses, using mass uncertainties of 2 and 5 mDa, respectively. Compositions proposed for the ionized molecule that did not correspond to the sum of the compositions of a candidate fragment ion and its corresponding neutral loss were discarded. One, 2-5, 6-10, 11-20, and >20 candidate compositions were found for 65%, 39%, 1%, 1%, and 0%, respectively, for the 124 ionized molecules formed from the 113 chemicals tested (both positive and negative ions were obtained from 11 of the chemicals). However, no candidate composition was found for 2% of the test cases (i.e., 3 chemicals), for each of which the measured mass of one of the product ions was in

  2. Membrane Assisted Simultaneous Extraction and Derivatization with Triphenylphosphine of Elemental Sulfur in Arabian Crude Samples by Gas Chromatography/Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Ibrahim Al-Zahrani

    2015-01-01

    Full Text Available Determination of trace level elemental sulfur from crude oil samples is a tedious task. Recently, several gas chromatographic methods were reported in which selective triphenylphosphine derivatization of sulfur was used to form triphenylphosphine sulfide. Direct quantitation of elemental sulfur from crude oil requires an efficient sample preparation method. This paper describes how simultaneous extraction derivatization of elemental sulfur was performed for the first time using porous hollow fiber membrane. A thick (0.25 um pore size; 1550 μm wall thickness; and 5500 μm inner diameter hollow fiber membrane filled with triphenylphosphine (dissolved N-methylpyrrolidone is used as a solvent bar. The solvent bar is tumbled freely in the crude oil sample; the elemental sulfur was extracted and derivatized. Finally, the derivatized sulfur was analyzed by gas chromatography/mass spectrometry. Various experimental conditions of solvent bar microextraction (SBME were optimized to achieve higher extraction. The linear range was established between 1 and 50 μg/mL, while a squared regression coefficient was found to be 0.9959 μg/mL. Relative standard deviation (RSD was below 10%. Relative recoveries were calculated for SBME in crude oil samples and were in the range between 98.2% and 101.2%.

  3. Determination of minor and trace elements in aromatic spices by micro-wave assisted digestion and inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Khan, Naeem; Choi, Ji Yeon; Nho, Eun Yeong; Jamila, Nargis; Habte, Girum; Hong, Joon Ho; Hwang, In Min; Kim, Kyong Su

    2014-09-01

    This study aimed at analyzing the concentrations of 23 minor and trace elements in aromatic spices by inductively coupled plasma-mass spectrometry (ICP-MS), after wet digestion by microwave system. The analytical method was validated by linearity, detection limits, precision, accuracy and recovery experiments, obtaining satisfactory values in all cases. Results indicated the presence of variable amounts of both minor and trace elements in the selected aromatic spices. Manganese was high in cinnamon (879.8 μg/g) followed by cardamom (758.1 μg/g) and clove (649.9 μg/g), strontium and zinc were high in ajwain (489.9 μg/g and 84.95 μg/g, respectively), while copper was high in mango powder (77.68 μg/g). On the whole some of the minor and essential trace elements were found to have good nutritional contribution in accordance to RDA. The levels of toxic trace elements, including As, Cd, and Pb were very low and did not found to pose any threat to consumers. Copyright © 2014 Elsevier Ltd. All rights reserved.

  4. Eleventh ISMAS workshop on mass spectrometry

    International Nuclear Information System (INIS)

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

    2004-10-01

    This volume deals with the latest developments in this field, exposing the innumerable applications of mass spectrometry. The topics covered include basic fundamentals of mass spectrometry, qualitative and quantitative aspects and data interpretation, maintenance of mass spectrometers, selection of a mass spectrometer, its applications in various branches of science as well as recent advances in mass spectrometry. Emphasis is also laid on the practical aspects of mass spectrometry. Papers relevant to INIS are indexed separately

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

    Science.gov (United States)

    Skytte, Lilian; Rasmussen, Kaare Lund

    2013-07-30

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

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

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

    International Nuclear Information System (INIS)

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

    1994-01-01

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

  8. Mass spectrometry in epigenetic research

    DEFF Research Database (Denmark)

    Beck, Hans Christian

    2010-01-01

    cancers has gained tremendous interest in recent years, and many of these inhibitors are currently undergoing clinical trials. Despite intense research, however, the exact molecular mechanisms of action of these molecules remain, to a wide extent, unclear. The recent application of mass spectrometry...

  9. Mass spectrometry of large molecules

    International Nuclear Information System (INIS)

    Facchetti, S.

    1985-01-01

    The lectures in this volume were given at a course on mass spectrometry of large molecules, organized within the framework of the Training and Education programme of the Joint Research Centre of the European Communities. Although first presented in 1983, most of the lectures have since been updated by their authors. (orig.)

  10. Mass spectrometry with particle accelerator

    International Nuclear Information System (INIS)

    Anon.

    1983-01-01

    The heavy ion accelerator use is renewing the ultrasensitive mass spectrometry in extending the detection limits. These new devices allow the measurement of rare isotope ratio, as 10 Be, 14 C, 26 Al, 36 Cl or 41 Ca, from the earth natural reservoirs [fr

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  12. Multi-element analysis of urine using dynamic reaction cell inductively coupled plasma mass spectrometry (ICP-DRC-MS — A practical application

    Directory of Open Access Journals (Sweden)

    Renata Brodzka

    2013-04-01

    Full Text Available Objectives: The method for the determination of As, Al, Cd, Ni, Pb (toxic elements and Cr, Co, Cu, Fe, Mn, Zn (essential elements in human urine by the use of Inductively Coupled Plasma Mass Spectrometry (quadrupole ICP-MS DRCe Elan, Perkin Elmer with the dynamic reaction cell (DRC was developed. Materials and Methods: The method has been applied for multi-element analysis of the urine of 16 non-exposed healthy volunteers and 27 workers employed in a copper smelter. The analysis was conducted after initial 10-fold dilution of the urine samples with 0,1% nitric acid. Rhodium was used as an internal standard. The method validation parameters such as detection limit, sensitivity, precision were described for all elements. Accuracy of the method was checked by the regular use of certified reference materials ClinCheck®-Control Urine (Recipe as well as by participation of the laboratory in the German External Quality Assessment Scheme (G-EQUAS. Results: The detection limits (DL 3s of the applied method were 0.025, 0.007, 0.002, 0.004, 0.004, 0.086, 0.037, 0.009, 0.016, 0.008, 0.064 (μg/l for Al, As, Cd, Cr, Co, Cu, Fe, Mn, Ni, Pb, Zn in urine, respectively. For each element linearity with correlation coefficient of at least 0.999 was determined. Spectral interferences from some of the ions were removed using DRC-e with addition of alternative gas: methane for cobalt, copper, cadmium, chromium, iron, manganese, nickel and rhodium, and oxygen for arsenic. Conclusions: The developed method allows to determine simultaneously eleven elements in the urine with low detection limits, high sensitivity and good accuracy. Moreover, the method is appropriate for the assessment of both environmental and occupational exposure.

  13. Improved accuracy and precision in δ15 NAIR measurements of explosives, urea, and inorganic nitrates by elemental analyzer/isotope ratio mass spectrometry using thermal decomposition.

    Science.gov (United States)

    Lott, Michael J; Howa, John D; Chesson, Lesley A; Ehleringer, James R

    2015-08-15

    Elemental analyzer systems generate N(2) and CO(2) for elemental composition and isotope ratio measurements. As quantitative conversion of nitrogen in some materials (i.e., nitrate salts and nitro-organic compounds) is difficult, this study tests a recently published method - thermal decomposition without the addition of O(2) - for the analysis of these materials. Elemental analyzer/isotope ratio mass spectrometry (EA/IRMS) was used to compare the traditional combustion method (CM) and the thermal decomposition method (TDM), where additional O(2) is eliminated from the reaction. The comparisons used organic and inorganic materials with oxidized and/or reduced nitrogen and included ureas, nitrate salts, ammonium sulfate, nitro esters, and nitramines. Previous TDM applications were limited to nitrate salts and ammonium sulfate. The measurement precision and accuracy were compared to determine the effectiveness of converting materials containing different fractions of oxidized nitrogen into N(2). The δ(13) C(VPDB) values were not meaningfully different when measured via CM or TDM, allowing for the analysis of multiple elements in one sample. For materials containing oxidized nitrogen, (15) N measurements made using thermal decomposition were more precise than those made using combustion. The precision was similar between the methods for materials containing reduced nitrogen. The %N values were closer to theoretical when measured by TDM than by CM. The δ(15) N(AIR) values of purchased nitrate salts and ureas were nearer to the known values when analyzed using thermal decomposition than using combustion. The thermal decomposition method addresses insufficient recovery of nitrogen during elemental analysis in a variety of organic and inorganic materials. Its implementation requires relatively few changes to the elemental analyzer. Using TDM, it is possible to directly calibrate certain organic materials to international nitrate isotope reference materials without off

  14. Determination of major, minor and trace elements in rock samples by laser ablation inductively coupled plasma mass spectrometry: Progress in the utilization of borate glasses as targets

    International Nuclear Information System (INIS)

    Leite, Tacito Dantas F.; Escalfoni, Rainerio; Fonseca, Teresa Cristina O. da; Miekeley, Norbert

    2011-01-01

    The present work is a continuation of a research study performed at our laboratory aiming at the multielement analysis of rock samples (basalts and shale) by inductively coupled plasma mass spectrometry in combination with laser ablation using borate glasses as analytical targets. Argon, nitrogen-argon mixtures and helium were evaluated as cell gases, the latter confirming its better performance. Different operational parameters of the laser, such as gas flow, energy, focus, scanning speed and sampling frequency were optimized. External calibration was made with standards prepared by fusion of geological reference materials (basalts 688 and BCR-2, obsidian SRM 278, and shale SGR-1) of different mass fractions in the meta-tetra borate matrix. Coefficients of determination (R 2 ) were > 0.99 for 30 elements from o total of 40 determined. Method validation was then performed using additional certified reference materials (BHVO-2, BIR-1, SCo-1) produced as borate targets in a similar way. Accuracies were better than 10% for most of the elements studied and analytical precisions, calculated from the residual standard deviations of calibration curves were, typically, between 6% and 10%. Additionally, the semiquantitative TotalQuant (registered) technique was applied, which gave, within the expected uncertainty for this calibration technique, concordant results when compared to the quantitative external calibration procedure. Both methods were then used for the analysis of marine shale samples, which are of great geological interest in petroleum prospecting.

  15. Accelerator mass spectrometry - From DNA to astrophysics

    International Nuclear Information System (INIS)

    Kutschera, W.

    2013-01-01

    A brief review of accelerator mass spectrometry (AMS) is presented. The present work touches on a few technical aspects and recent developments of AMS, and describes two specific applications of AMS, the dating of human DNA with the 14 C bomb peak and the search for superheavy elements in nature. Since two extended general reviews on technical developments in AMS [1] and applications of AMS [2] will appear in 2013, frequent reference to these reviews is made. (authors)

  16. Evaluation of pyrolysis curves for volatile elements in aqueous standards and carbon-containing matrices in electrothermal vaporization inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Silva, A.F. [Delft University of Technology, Faculty of Applied Sciences, DelftChemTech, Julianalaan 136, 2628 BL Delft (Netherlands); Universidade Federal de Santa Catarina, Departamento de Quimica, 88040-900 Florianopolis, SC (Brazil); Welz, B. [Universidade Federal de Santa Catarina, Departamento de Quimica, 88040-900 Florianopolis, SC (Brazil); Loos-Vollebregt, M.T.C. de [Delft University of Technology, Faculty of Applied Sciences, DelftChemTech, Julianalaan 136, 2628 BL Delft (Netherlands)], E-mail: m.t.c.deloos-vollebregt@tudelft.nl

    2008-07-15

    Pyrolysis curves in electrothermal atomic absorption spectrometry (ET AAS) and electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) have been compared for As, Se and Pb in lobster hepatopancreas certified reference material using Pd/Mg as the modifier. The ET AAS pyrolysis curves confirm that the analytes are not lost from the graphite furnace up to a pyrolysis temperature of 800 deg. C. Nevertheless, a downward slope of the pyrolysis curve was observed for these elements in the biological material using ETV-ICP-MS. This could be related to a gain of sensitivity at low pyrolysis temperatures due to the matrix, which can act as carrier and/or promote changes in the plasma ionization equilibrium. Experiments with the addition of ascorbic acid to the aqueous standards confirmed that the higher intensities obtained in ETV-ICP-MS are related to the presence of organic compounds in the slurry. Pyrolysis curves for As, Se and Pb in coal and coal fly ash were also investigated using the same Pd/Mg modifier. Carbon intensities were measured in all samples using different pyrolysis temperatures. It was observed that pyrolysis curves for the three analytes in all slurry samples were similar to the corresponding graphs that show the carbon intensity for the same slurries for pyrolysis temperatures from 200 deg. C up to 1000 deg. C.

  17. Mass spectrometry and tandem mass spectrometry of citrus limonoids.

    Science.gov (United States)

    Tian, Qingguo; Schwartz, Steven J

    2003-10-15

    Methods for atmospheric pressure chemical ionization tandem mass spectrometry (APCI-MS/MS) of citrus limonoid aglycones and electrospray ionization tandem mass spectrometry (ESI-MS/MS) of limonoid glucosides are reported. The fragmentation patterns of four citrus limonoid aglycones (limonin, nomilin, obacunone, and deacetylnomilin) and six limonoid glucosides, that is, limonin 17-beta-D-glucopyranoside (LG), nomilin 17-beta-D-glucopyranoside (NG), nomilinic acid 17-beta-D-glucopyranoside (NAG), deacetyl nomilinic acid 17-beta-D-glucopyranoside (DNAG), obacunone 17-beta-D-glucopyranoside (OG), and obacunoic acid 17-beta-D-glucopyranoside (OAG) were investigated using a quadruple mass spectrometer in low-energy collisionally activated dissociation (CAD). The four limonoid aglycones and four limonoid glucosides (LG, OG, NAG, and DNAG) were purified from citrus seeds; the other two limonoid glucosides (NG and OAG) were tentatively identified in the crude extract of grapefruit seeds by ESI mass spectrometry in both positive and negative ion analysis. Ammonium hydroxide or acetic acid was added to the mobile phase to facilitate ionization. During positive ion APCI analysis of limonoid aglycones, protonated molecular ion, [M + H]+, or adduct ion, [M + NH3 + H]-, was formed as base peaks when ammonium hydroxide was added to the mobile phase. Molecular anions or adduct ions with acetic acid ([M + HOAc - H] and [M + HOAc]-) or a deprotonated molecular ion were produced during negative ion APCI analysis of limonoid aglycones, depending on the mobile-phase modifier used. Positive ion ESI-MS of limonoid glucosides produced adduct ions of [M + H + NH3]+, [M + Na]+, and [M + K]+ when ammonium hydroxide was added to the mobile phase. After collisionally activated dissociation (CAD) of the limonoid aglycone molecular ions in negative ion APCI analysis, fragment ions indicated structural information of the precursor ions, showing the presence of methyl, carboxyl, and oxygenated ring

  18. Imaging Mass Spectrometry in Neuroscience

    Science.gov (United States)

    2013-01-01

    Imaging mass spectrometry is an emerging technique of great potential for investigating the chemical architecture in biological matrices. Although the potential for studying neurobiological systems is evident, the relevance of the technique for application in neuroscience is still in its infancy. In the present Review, a principal overview of the different approaches, including matrix assisted laser desorption ionization and secondary ion mass spectrometry, is provided with particular focus on their strengths and limitations for studying different neurochemical species in situ and in vitro. The potential of the various approaches is discussed based on both fundamental and biomedical neuroscience research. This Review aims to serve as a general guide to familiarize the neuroscience community and other biomedical researchers with the technique, highlighting its great potential and suitability for comprehensive and specific chemical imaging. PMID:23530951

  19. Mass Spectrometry Applications for Toxicology

    OpenAIRE

    Mbughuni, Michael M.; Jannetto, Paul J.; Langman, Loralie J.

    2016-01-01

    Toxicology is a multidisciplinary study of poisons, aimed to correlate the quantitative and qualitative relationships between poisons and their physiological and behavioural effects in living systems. Other key aspects of toxicology focus on elucidation of the mechanisms of action of poisons and development of remedies and treatment plans for associated toxic effects. In these endeavours, Mass spectrometry (MS) has become a powerful analytical technique with a wide range of application used i...

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

  1. Forensic Discrimination of Concrete Pieces by Elemental Analysis of Acid-soluble Component with Inductively Coupled Plasma-Mass Spectrometry.

    Science.gov (United States)

    Kasamatsu, Masaaki; Igawa, Takao; Suzuki, Shinichi; Suzuki, Yasuhiro

    2018-01-01

    Since fragments of concrete can be evidence of crime, a determination of whether or not they come from the same origin is required. The authors focused on nitric acid-soluble components in the fragments of concrete. As a result of qualitative analysis with ICP-MS, it was confirmed that elements such as Cu, Zn, Rb, Sr, Zr, Ba, La, Ce, Nd, and Pb were contained in the fragments. After the nitric acid-soluble components in the fragments of concrete were separated by dissolving them in nitric acid, the concentrations of these elements in the dissolved solution were quantitatively determined by ICP-MS. The concentration ratios of nine elements compared to La were used as indicators. By comparing these indicators, it was possible to discriminate between the fragments of concrete.

  2. Analysis of rare earth elements in coal fly ash using laser ablation inductively coupled plasma mass spectrometry and scanning electron microscopy

    Science.gov (United States)

    Thompson, Robert L.; Bank, Tracy; Montross, Scott; Roth, Elliot; Howard, Bret; Verba, Circe; Granite, Evan

    2018-05-01

    Reference standard NIST SRM 1633b and FA 345, a fly ash sample from an eastern U.S. coal power plant, were analyzed to determine and quantify the mineralogical association of rare earth elements (REE). These analyses were completed using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and a scanning electron microscope, equipped with an energy-dispersive X-ray spectrometer (SEM-EDS). Internal standardization was avoided by quantifying elemental concentrations by normalizing to 100% oxides. Mineral grains containing elevated REE concentrations were found in diverse chemical environments, but were most commonly found in regions where Al and Si were predominant. Dividing the spot analyses into time segments yielded plots that showed the REE content changing over time as individual mineral grains were being ablated. SEM-EDS images of FA 345 confirmed the trends that were found in the LA-ICP-MS results. Small grains of apatite, monazite, or zircon were frequently observed as free mineral grains or embedded in amorphous aluminosilicate glass and were not associated with ferrous particles. This finding is consistent with previous reports that magnetic enrichment may be an effective way of concentrating non-magnetic REE phases. Furthermore, aggressive mechanical and chemical-based separation schemes will be required to separate and recover REE from aluminosilicate glass.

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

    International Nuclear Information System (INIS)

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

    1999-01-01

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

  4. Upconversion nanoparticle as elemental tag for the determination of alpha-fetoprotein in human serum by inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Liu, Zhengru; Yang, Bin; Chen, Beibei; He, Man; Hu, Bin

    2016-12-19

    Upconversion nanoparticles (UCNPs) have received increasing attention due to their unique optical properties. Recognizing that UCNPs are lanthanide-doped nanoparticles, we incorporated UCNPs into an immunoassay with inductively coupled plasma mass spectrometry (ICP-MS) detection for the determination of specific proteins, e.g., alpha-fetoprotein (AFP). The sensitivity of the assay was enhanced because of the ICP-MS detection of UCNPs that contained large numbers of lanthanide elemental tags. Conjugates of UCNPs and antibodies were prepared and the morphology of the conjugates was characterized by transmission electron microscopy. After a sandwich immunoreaction, the AFP was determined by the ICP-MS analysis of UCNPs. Under the optimized conditions, a limit of detection (3σ) of 0.31 ng mL -1 based on 89 Y signal and 0.22 ng mL -1 based on 174 Yb signal was obtained for AFP, with a dynamic range of 0.5-35 ng mL -1 and a relative standard deviation of 4.8% (c = 5 ng mL -1 , n = 9). The developed method was applied to the determination of AFP in human serum and the recovery for the spiked sample was in the range of 98.6-123%. The proposed method is simple, rapid, selective and sensitive, and has a good tolerance for the complex biological matrix, indicating great potential for the application of UCNP in biological research as an elemental tag.

  5. Spatially and time-resolved element-specific in situ corrosion investigations with an online hyphenated microcapillary flow injection inductively coupled plasma mass spectrometry set-up

    International Nuclear Information System (INIS)

    Homazava, N.; Ulrich, A.; Kraehenbuehl, U.

    2008-01-01

    A novel technique for in situ spatial, time-resolved element-specific investigations of corrosion processes is developed. The technique is based on an online hyphenation of a specially designed microflow-capillary set-up to inductively coupled plasma mass spectrometry (ICP-MS) using flow injection sample introduction. Detailed aspects of the method development, optimization of the sample microflow introduction and flow injection characteristics for the localized corrosion analysis are described. Moreover, specific challenges of the ICP-MS analysis as applied to the analysis of corrosion sample probes, e.g. high matrix load and limited sample volume, are discussed. The efficiency of the developed technique is proved by corrosion susceptibility analysis of a commercial Al alloy. Results of the corrosion experiments of the aluminum alloy AA 6111 are presented to demonstrate the influence of various factors such as exposure time and pH value of the corrosive medium on the element-specific dissolution rates of the alloy. This novel technique provides new aspects in corrosion science and sheds new light on corrosion mechanisms

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

    Science.gov (United States)

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

    2012-10-16

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

  7. Elemental bioimaging of nanosilver-coated prostheses using X-ray fluorescence spectroscopy and laser ablation-inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Blaske, Franziska; Reifschneider, Olga; Gosheger, Georg; Wehe, Christoph A; Sperling, Michael; Karst, Uwe; Hauschild, Gregor; Höll, Steffen

    2014-01-07

    The distribution of different chemical elements from a nanosilver-coated bone implant was visualized, combining the benefits of two complementary methods for elemental bioimaging, the nondestructive micro X-ray fluorescence (μ-XRF), and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). Challenges caused by the physically inhomogeneous materials including bone and soft tissues were addressed by polymer embedding. With the use of μ-XRF, fast sample mapping was achieved obtaining titanium and vanadium signals from the metal implant as well as phosphorus and calcium signals representing hard bone tissue and sulfur distribution representing soft tissues. Only by the use of LA-ICP-MS, the required high sensitivity and low detection limits for the determination of silver were obtained. Metal distribution within the part of cancellous bone was revealed for silver as well as for the implant constituents titanium, vanadium, and aluminum. Furthermore, the detection of coinciding high local zirconium and aluminum signals at the implant surface indicates remaining blasting abrasive from preoperative surface treatment of the nanosilver-coated device.

  8. Microwave dissolution of plant tissue and the subsequent determination of trace lanthanide and actinide elements by inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Alvarado, J.S.; Neal, T.J.; Smith, L.L.; Erickson, M.D.

    1997-01-01

    Recently there has been much concern with the ability of plants to uptake heavy metals from their surroundings. With the development of instrumental techniques with low detection limits such as inductively coupled plasma-mass spectrometry (ICP-MS), attention is shifting toward achieving faster and more elegant ways of oxidizing the organic material inherent in environmental samples. Closed-vessel microwave dissolution was compared with conventional methods for the determination of concentrations of cerium, samarium, europium, terbium, uranium and thorium in a series of samples from the National Institute of Standards and Technology and from fields in Idaho. The ICP-MS technique exhibited detection limits in parts-per-trillion and linear calibration plots over three orders of magnitude for the elements under study. The results obtained by using nitric acid and hydrogen peroxide in a microwave digestion system for the analysis of reference materials showed close agreement with the accepted values. These values were compared with results obtained from dry- and wet-ashing procedures. The findings from an experiment comparing radiometric techniques for the determination of actinide elements to ICP-MS are reported

  9. Mass spectrometry. [review of techniques

    Science.gov (United States)

    Burlingame, A. L.; Kimble, B. J.; Derrick, P. J.

    1976-01-01

    Advances in mass spectrometry (MS) and its applications over the past decade are reviewed in depth, with annotated literature references. New instrumentation and techniques surveyed include: modulated-beam MS, chromatographic MS on-line computer techniques, digital computer-compatible quadrupole MS, selected ion monitoring (mass fragmentography), and computer-aided management of MS data and interpretation. Areas of application surveyed include: organic MS and electron impact MS, field ionization kinetics, appearance potentials, translational energy release, studies of metastable species, photoionization, calculations of molecular orbitals, chemical kinetics, field desorption MS, high pressure MS, ion cyclotron resonance, biochemistry, medical/clinical chemistry, pharmacology, and environmental chemistry and pollution studies.

  10. Functional genomics by mass spectrometry

    DEFF Research Database (Denmark)

    Andersen, Jens S.; Mann, M

    2000-01-01

    Systematic analysis of the function of genes can take place at the oligonucleotide or protein level. The latter has the advantage of being closest to function, since it is proteins that perform most of the reactions necessary for the cell. For most protein based ('proteomic') approaches to gene f...... numbers of intact proteins by mass spectrometry directly. Examples from this laboratory illustrate biological problem solving by modern mass spectrometric techniques. These include the analysis of the structure and function of the nucleolus and the analysis of signaling complexes....

  11. Laser sputter neutral mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    King, B V; Clarke, M; Hu, H; Betz, [Newcastle Univ., NSW (Australia). Dept. of Physics

    1994-12-31

    Laser sputter neutral mass spectrometry (LSNMS) is an emerging technique for highly sensitive surface analysis. In this technique a target is bombarded with a pulsed beam of keV ions. The sputtered particles are intercepted by a high intensity pulsed laser beam above the surface and ionised with almost 100% efficiency. The photions may then be mass analysed using a quadrupole or, more commonly, using time of flight (TOF) techniques. In this method photoions are extracted from the ionisation region, accelerated to a known energy E{sub o} and strike a channelplate detector a distance `d` away. The flight time `t` of the photoions is then related to their mass by `d` {radical}m / {radical} 2E{sub o} so measurement of `t` allows mass spectra to be obtained. It is found that LSNMS is an emerging technique of great sensitivity and flexibility, useful for both applied analysis and to investigate basic sputtering processes. 4 refs., 3 figs.

  12. Laser sputter neutral mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    King, B.V.; Clarke, M.; Hu, H.; Betz [Newcastle Univ., NSW (Australia). Dept. of Physics

    1993-12-31

    Laser sputter neutral mass spectrometry (LSNMS) is an emerging technique for highly sensitive surface analysis. In this technique a target is bombarded with a pulsed beam of keV ions. The sputtered particles are intercepted by a high intensity pulsed laser beam above the surface and ionised with almost 100% efficiency. The photions may then be mass analysed using a quadrupole or, more commonly, using time of flight (TOF) techniques. In this method photoions are extracted from the ionisation region, accelerated to a known energy E{sub o} and strike a channelplate detector a distance `d` away. The flight time `t` of the photoions is then related to their mass by `d` {radical}m / {radical} 2E{sub o} so measurement of `t` allows mass spectra to be obtained. It is found that LSNMS is an emerging technique of great sensitivity and flexibility, useful for both applied analysis and to investigate basic sputtering processes. 4 refs., 3 figs.

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

    Science.gov (United States)

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

    2017-08-29

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

  14. Ninth ISMAS workshop on mass spectrometry

    International Nuclear Information System (INIS)

    Aggarwal, S.K.

    2000-12-01

    Mass spectrometry has wide-ranging applications in such diverse areas as nuclear industry, agriculture, drugs, environment, petroleum and lentils. There is an urgent need to absorb and assimilate state-of-the-art technological developments in the field. Emerging trends in atomic mass spectrometry, advances in organic mass spectrometry, qualitative and quantitative analyses by mass spectrometry and mass spectrometry in oceanography are some of the areas that need to be expeditiously examined and are covered in this volume. Papers relevant to INIS are indexed separately

  15. Quantitative mass spectrometry: an overview

    Science.gov (United States)

    Urban, Pawel L.

    2016-10-01

    Mass spectrometry (MS) is a mainstream chemical analysis technique in the twenty-first century. It has contributed to numerous discoveries in chemistry, physics and biochemistry. Hundreds of research laboratories scattered all over the world use MS every day to investigate fundamental phenomena on the molecular level. MS is also widely used by industry-especially in drug discovery, quality control and food safety protocols. In some cases, mass spectrometers are indispensable and irreplaceable by any other metrological tools. The uniqueness of MS is due to the fact that it enables direct identification of molecules based on the mass-to-charge ratios as well as fragmentation patterns. Thus, for several decades now, MS has been used in qualitative chemical analysis. To address the pressing need for quantitative molecular measurements, a number of laboratories focused on technological and methodological improvements that could render MS a fully quantitative metrological platform. In this theme issue, the experts working for some of those laboratories share their knowledge and enthusiasm about quantitative MS. I hope this theme issue will benefit readers, and foster fundamental and applied research based on quantitative MS measurements. This article is part of the themed issue 'Quantitative mass spectrometry'.

  16. Laser ablation-inductively coupled plasma-dynamic reaction cell-mass spectrometry for the multi-element analysis of polymers

    International Nuclear Information System (INIS)

    Resano, M.; Garcia-Ruiz, E.; Vanhaecke, F.

    2005-01-01

    In this work, the potential of laser ablation-inductively coupled plasma-mass spectrometry for the fast analysis of polymers has been explored. Different real-life samples (polyethylene shopping bags, an acrylonitrile butadiene styrene material and various plastic bricks) as well as several reference materials (VDA 001 to 004, Cd in polyethylene) have been selected for the study. Two polyethylene reference materials (ERM-EC 680 and 681), for which a reference or indicative value for the most relevant metals is available, have proved their suitability as standards for calibration. Special attention has been paid to the difficulties expected for the determination of Cr at the μg g -1 level in this kind of materials, due to the interference of ArC + ions on the most abundant isotopes of Cr. The use of ammonia as a reaction gas in a dynamic reaction cell is shown to alleviate this problem, resulting in a limit of detection of 0.15 μg g -1 for this element, while limiting only modestly the possibilities of the technique for simultaneous multi-element analysis. In this regard, As is the analyte most seriously affected by the use of ammonia, and its determination has to be carried out in vented mode, at the expense of measuring time. In all cases studied, accurate results could be obtained for elements ranging in content from the sub-μg g -1 level to tens of thousands of μg g -1 . However, the use of an element of known concentration as internal standard may be needed for materials with a matrix significantly different from that of the standard (polyethylene in this work). Precision ranged between 5% and 10% RSD for elements found at the 10 μg g -1 level or higher, while this value could deteriorate to 20% for analytes found at the sub-μg g -1 level. Overall, the technique evaluated presents many advantages for the fast and accurate multi-element analysis of these materials, avoiding laborious digestion procedures and minimizing the risk of analyte losses due to the

  17. Elemental quantification of airborne particulate matter by instrumental neutron activation analysis and induced coupled plasma mass spectrometry analysis

    International Nuclear Information System (INIS)

    Hidayat, Achmad; Djojosubroto, Harjoto; Rukihati; Sutisna

    1999-01-01

    Airborne particulate were collected using Gent sampler for PM 10 and using high volume sampler for total suspended particulate (TSP). PM 10 sampling was carried out in Bandung during period of January to December 1997. Whereas TSP samples were collected at Serpong (rural area) and Jakarta (urban area) during period of May and July 1995. The concentration of the PM 10 in the air is independent to the level of the rainfall. The levels of the PM 10 and the PM 2.5 are lower than the maximum permissible levels set by the US Environmental Protection Agency in July 1997. The element detected using short lived radioactivity measurement in PM 10 and PM 2.5 were Al, Na, V, Mn, Br and Cl. Bromine concentration in both coarse and fine fractions was high, and the enrichment factor for bromine in these fraction was found between 2,000 - 10,000. The elemental concentrations of particulate matter obtained by ICP-MS was found that the Ag, Al, As, Ba, Cd, Co, Cr, Cs, Cu, Fe, In, K, Mg, Mn, Na, Ni, Pb, Rb, V and Zn in samples from Serpong area, were lower than those in samples taken from Jakarta area. The level of Pb concentrations in TSP samples from Serpong and Jakarta area were lower than Pb concentration proposed Indonesian standard of 2 μg/m 3 . The data obtained by INAA no significant different to those obtained by ICP-MS. Therefore comparative data can be obtained by these techniques. (author)

  18. Correlation of precursor and product ions in single-stage high resolution mass spectrometry. A tool for detecting diagnostic ions and improving the precursor elemental composition elucidation

    Energy Technology Data Exchange (ETDEWEB)

    Borràs, S. [Departament de Química Analítica, Universitat de Barcelona, Martí i Franquès 1-11, 08028 Barcelona (Spain); Kaufmann, A., E-mail: anton.kaufmann@klzh.ch [Official Food Control Authority, Fehrenstrasse 15, 8032 Zürich (Switzerland); Companyó, R. [Departament de Química Analítica, Universitat de Barcelona, Martí i Franquès 1-11, 08028 Barcelona (Spain)

    2013-04-15

    Highlights: ► We are describing a technique to spot ions which are derived from each other. ► Single stage high resolution data is used. ► This “in silicon” technique is compared to conventional precursor scan. ► Some applications for this technique are presented. -- Abstract: Monitoring of common diagnostic fragments is essential for recognizing molecules which are members of a particular compound class. Up to now, unit resolving tandem quadrupole mass spectrometers, operating in the precursor ion scan mode, have been typically used to perform such analysis. By means of high-resolution mass spectrometry (HRMS) a much more sensitive and selective detection can be achieved. However, using a single-stage HRMS instrument, there is no unequivocal link to the corresponding precursor ion, since such instrumentation does not permit a previous precursor selection. Thus, to address this limitation, an in silico approach to locate precursor ions, based on diagnostic fragments, was developed. Implemented as an Excel macro, the algorithm rapidly assembles and surveys exact mass data to provide a list of feasible precursor candidates according to the correlation of the chromatographic peak shape profile and other additional filtering criteria (e.g. neutral losses and isotopes). The macro was tested with two families of veterinary drugs, sulfonamides and penicillins, which are known to yield diagnostic product ions when fragmented. Data sets obtained from different food matrices (fish and liver), both at high and low concentration of the target compounds, were investigated in order to evaluate the capabilities and limitations of the reported approach. Finally, other possible applications of this technique, such as the elucidation of elemental compositions based on product ions and corresponding neutral losses, were also presented and discussed.

  19. Correlation of precursor and product ions in single-stage high resolution mass spectrometry. A tool for detecting diagnostic ions and improving the precursor elemental composition elucidation

    International Nuclear Information System (INIS)

    Borràs, S.; Kaufmann, A.; Companyó, R.

    2013-01-01

    Highlights: ► We are describing a technique to spot ions which are derived from each other. ► Single stage high resolution data is used. ► This “in silicon” technique is compared to conventional precursor scan. ► Some applications for this technique are presented. -- Abstract: Monitoring of common diagnostic fragments is essential for recognizing molecules which are members of a particular compound class. Up to now, unit resolving tandem quadrupole mass spectrometers, operating in the precursor ion scan mode, have been typically used to perform such analysis. By means of high-resolution mass spectrometry (HRMS) a much more sensitive and selective detection can be achieved. However, using a single-stage HRMS instrument, there is no unequivocal link to the corresponding precursor ion, since such instrumentation does not permit a previous precursor selection. Thus, to address this limitation, an in silico approach to locate precursor ions, based on diagnostic fragments, was developed. Implemented as an Excel macro, the algorithm rapidly assembles and surveys exact mass data to provide a list of feasible precursor candidates according to the correlation of the chromatographic peak shape profile and other additional filtering criteria (e.g. neutral losses and isotopes). The macro was tested with two families of veterinary drugs, sulfonamides and penicillins, which are known to yield diagnostic product ions when fragmented. Data sets obtained from different food matrices (fish and liver), both at high and low concentration of the target compounds, were investigated in order to evaluate the capabilities and limitations of the reported approach. Finally, other possible applications of this technique, such as the elucidation of elemental compositions based on product ions and corresponding neutral losses, were also presented and discussed

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

    International Nuclear Information System (INIS)

    Ochsenkuehn-Petropoulou, Maria; Luck, Joachim

    1991-01-01

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

  1. Principle of accelerator mass spectrometry

    International Nuclear Information System (INIS)

    Matsuzaki, Hiroyuki

    2007-01-01

    The principle of accelerator mass spectrometry (AMS) is described mainly on technical aspects: hardware construction of AMS, measurement of isotope ratio, sensitivity of measurement (measuring limit), measuring accuracy, and application of data. The content may be summarized as follows: rare isotope (often long-lived radioactive isotope) can be detected by various use of the ion energy obtained by the acceleration of ions, a measurable isotope ratio is one of rare isotope to abundant isotopes, and a measured value of isotope ratio is uncertainty to true one. Such a fact must be kept in mind on the use of AMS data to application research. (M.H.)

  2. Simultaneous mass detection for direct inlet mass spectrometry

    International Nuclear Information System (INIS)

    Gordon, R.L.

    1979-05-01

    The evolution of analytical techniques for application in trace analysis has led to interest in practical methods for real-time monitoring. Direct inlet mass spectrometry (DIMS) has been the subject of considerable activity in recent years. A DIMS instrument is described which consists of an inlet system designed to permit particles entrained in the inlet air stream to strike a hot, oxidized rhenium filament which serves as a surface ionization source. A mass analyzer and detection system then permits identification of the elemental composition of particulates which strike the filament

  3. Ultra-Sensitive Elemental Analysis Using Plasmas 4.Application of Inductively Coupled Plasma Mass Spectrometry to the Study of Environmental Radioactivity

    Science.gov (United States)

    Yoshida, Satoshi

    Applications of inductively coupled plasma mass spectrometry (ICP-MS) to the determination of long-lived radionuclides in environmental samples were summarized. In order to predict the long-term behavior of the radionuclides, related stable elements were also determined. Compared with radioactivity measurements, the ICP-MS method has advantages in terms of its simple analytical procedures, prompt measurement time, and capability of determining the isotope ratio such as240Pu/239Pu, which can not be separated by radiation. Concentration of U and Th in Japanese surface soils were determined in order to determine the background level of the natural radionuclides. The 235U/238U ratio was successfully used to detect the release of enriched U from reconversion facilities to the environment and to understand the source term. The 240Pu/239Pu ratios in environmental samples varied widely depending on the Pu sources. Applications of ICP-MS to the measurement of I and Tc isotopes were also described. The ratio between radiocesium and stable Cs is useful for judging the equilibrium of deposited radiocesium in a forest ecosystem.

  4. Microwave-assisted Extraction of Rare Earth Elements from Petroleum Refining Catalysts and Ambient Fine Aerosols Prior to Inductively Coupled Plasma - Mass Spectrometry

    Science.gov (United States)

    Mittlefehldt, David W.; Kulkarni, Pranav; Chellam, Shankar

    2006-01-01

    In the absence of a certified reference material, a robust microwave-assisted acid digestion procedure followed by inductively coupled plasma - mass spectrometry (ICP-MS) was developed to quantify rare earth elements (REEs) in fluidized-bed catalytic cracking (FCC) catalysts and atmospheric fine particulate matter (PM2.5). High temperature (200 C), high pressure (200 psig), acid digestion (HNO3, HF, and H3BO3) with 20 minute dwell time effectively solubilized REEs from six fresh catalysts, a spent catalyst, and PM2.5. This method was also employed to measure 27 non-REEs including Na, Mg, Al, Si, K, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Zr, Mo, Cd, Cs, Ba, Pb, and U. Complete extraction of several REEs (Y, La, Ce, Pr, Nd, Tb, Dy, and Er) required HF indicating that they were closely associated with the aluminosilicate structure of the zeolite FCC catalysts. Internal standardization using 115In quantitatively corrected non-spectral interferences in the catalyst digestate matrix. Inter-laboratory comparison using ICP-optical emission spectroscopy (ICP-OES) and instrumental neutron activation analysis (INAA) demonstrated the applicability of the newly developed analytical method for accurate analysis of REEs in FCC catalysts. The method developed for FCC catalysts was also successfully implemented to measure trace to ultra-trace concentrations of La, Ce, Pr, Nd, Sm, Gd, Eu, and Dy in ambient PM2.5 in an industrial area of Houston, TX.

  5. Microwave-assisted extraction of rare earth elements from petroleum refining catalysts and ambient fine aerosols prior to inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Kulkarni, Pranav; Chellam, Shankararaman; Mittlefehldt, David W.

    2007-01-01

    A robust microwave-assisted acid digestion procedure followed by inductively coupled plasma-mass spectrometry (ICP-MS) was developed to quantify rare earth elements (REEs) in fluidized-bed catalytic cracking (FCC) catalysts and atmospheric fine particulate matter (PM 2.5 ). High temperature (200 deg. C), high pressure (200 psig), acid digestion (HNO 3 , HF and H 3 BO 3 ) with 20 min dwell time effectively solubilized REEs from six fresh catalysts, a spent catalyst and PM 2.5 . This method was also employed to measure 27 non-REEs including Na, Mg, Al, Si, K, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Zr, Mo, Cd, Cs, Ba, Pb and U. Complete extraction of several REEs (Y, La, Ce, Pr, Nd, Tb, Dy and Er) required HF indicating that they were closely associated with the aluminosilicate structure of the zeolite FCC catalysts. Internal standardization using 115 In quantitatively corrected non-spectral interferences in the catalyst digestate matrix. Inter-laboratory comparison using ICP-optical emission spectroscopy (ICP-OES) and instrumental neutron activation analysis (INAA) demonstrated the applicability of the newly developed analytical method for accurate analysis of REEs in FCC catalysts. The method developed for FCC catalysts was also successfully implemented to measure trace to ultra-trace concentrations of La, Ce, Pr, Nd, Sm, Gd, Eu and Dy in ambient PM 2.5 in an industrial area of Houston, TX

  6. Simultaneous determination of platinum group elements and rhenium in rock samples using isotope dilution inductively coupled plasma mass spectrometry after cation exchange separation followed by solvent extraction

    International Nuclear Information System (INIS)

    Shinotsuka, Kazunori; Suzuki, Katsuhiko

    2007-01-01

    A simple and precise determination method for platinum group elements (PGEs) and Re in rock samples was developed using isotope dilution coupled with inductively coupled plasma mass spectrometry (ID-ICP-MS). Cation exchange separation was employed for simplicity, because it is applicable to group separation and simultaneous isotopic measurement in contrast with the widely used anion exchange separation which entails separate elution. However, its application to ID-ICP-MS has been limited due to spectral interferences from impurities retained in the PGE fraction even after ion chromatography. To overcome this limitation, solvent extraction using N-benzoyl-N-phenylhydroxylamine (BPHA) in chloroform was successfully applied for further purification. After the examination of optimum experimental parameters in cation exchange separation and solvent extraction using synthetic PGE solution, the established procedure was applied to the determination of PGEs and Re in some geochemical reference materials. The obtained results agreed well with the literature data determined using the different digestion methods (NiS fire assay and the use of a high-pressure asher) within the analytical uncertainties of each other. Significant difference in reproducibility between Ru, Ir, Pt and Os group, and Pd and Re group was observed in the results for BHVO-2 and JA-2. By considering the error factors affecting analytical reproducibility, we concluded that the difference is ascribed to the sample heterogeneity of minor minerals enriched in Ru, Ir, Pt and Os

  7. Protein Analysis by Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Cindic, M.

    2008-04-01

    Full Text Available Soft ionization techniques, electrospray (ESI and matrix-assisted laser desorption/ionization (MALDI make the analysis of biomolecules by mass spectrometry (MS possible. MS is used for determination of the molecular weight of peptides and protein, sequence analysis, characterization of protein-ligand interactions etc. The detection limit, resolution and mass accuracy depend on instrument used (Table 1. Impurities (buffers, salts, detergents can reduce the ion intensities or even totally suppress them, so a separation method (chromatography, 2D-gel electrophoresis must be used for purification of the sample.Molecular mass of intact protein can be determined by ESI or MALDI MS. Multiply charged ions are produced by ESI MS, while singly charged ions are predominant in MALDI spectra (Fig. 2.Sequence analysis of proteins by MS can be performed using peptide mass fingerprint. In this method, proteins are separated by 2-D gel electrophoresis and digested with specific protease (Table 2 or digested and then separated by two-dimensional chromatography (Fig. 1. The obtained peptide mixtures are analyzed by MS or MALDI-TOF technique. The masses determined by MS are compared with calculated masses from database entries. Different algorithms have been developed for protein identification. Example of posttranslational modifications (N- and O-glycosylation and protein sequence complex analysis after dual digestion (endoproteinase digestion followed by endoglycosidase digestion is shown in Fig. 3.It is known that detection of peptides by MS is influenced by intrinsic properties like amino acid composition, the basicity of the C-terminal amino acid, hydrophobicity, etc. Arginine-containing peptides dominate in MS spectra of tryptic digest, so the chemical derivatization of lysine terminal residue by O-methilisourea or 2-methoxy-4,5-1H-imidazole was suggested (Fig. 4.The peptide mass fingerprint method can be improved further by peptide fragmentation using tandem

  8. Exploiting dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP-MS) for sequential determination of trace elements in blood using a dilute-and-shoot procedure

    International Nuclear Information System (INIS)

    Lemos Batista, Bruno; Lisboa Rodrigues, Jairo; Andrade Nunes, Juliana; Oliveira Souza, Vanessa Cristina de; Barbosa, Fernando

    2009-01-01

    Inductively coupled plasma mass spectrometry with quadrupole (q-ICP-MS) and dynamic reaction cell (DRC-ICP-MS) were evaluated for sequential determination of As, Cd, Co, Cr, Cu, Mn, Pb, Se, Tl, V and Zn in blood. The method requires as little as 100 μL of blood. Prior to analysis, samples (100 μL) were diluted 1:50 in a solution containing 0.01% (v/v) Triton X-100 and 0.5% (v/v) nitric acid. The use of the DRC was only mandatory for Cr, Cu, V and Zn. For the other elements the equipment may be operated in a standard mode (q-ICP-MS). Ammonia was used as reaction gas. Selection of best flow rate of ammonium gas and optimization of the quadrupole dynamic band-pass tuning parameter (RPq) were carried out, using a ovine base blood for Cr and V and a synthetic matrix solution (SMS) for Zn and Cu diluted 1:50 and spiked to contain 1 μg L -1 of each element. Method detection limits (3 s) for 75 As, 114 Cd, 59 Co, 51 Cr, 63 Cu 55 Mn, 208 Pb, 82 Se, 205 Tl, 51 V, and 64 Zn were 14.0, 3.0, 11.0, 7.0, 280, 9.0, 3.0, 264, 0.7, 6.0 and 800 ng L -1 , respectively. Method validation was accomplished by the analysis of blood Reference Materials produced by the L'Institut National de Sante Publique du Quebec (Canada).

  9. Method validation for high resolution sector field inductively coupled plasma mass spectrometry determination of the emerging contaminants in the open ocean: Rare earth elements as a case study

    Science.gov (United States)

    Wysocka, Irena; Vassileva, Emilia

    2017-02-01

    Analytical procedure for the determination of fourteen rare earth elements (REEs) in the seawater samples has been developed and validated. The elements (La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) at ultra-trace level were measured by high resolution sector field inductively coupled plasma mass spectrometry (HR ICP-SFMS) after off-line analytes pre-concentration and matrix separation. The sample pre-treatment was carried out by commercially available automated system seaFAST-pico™, which is a low-pressure ion chromatography technique, based on solid phase extraction principles. Efficient elimination of seawater matrix and up to 50-fold pre-concentration of REEs enabled their accurate and precise quantification at ng L- 1 level. A validation approach in line with the requirements of ISO/IEC 17025 standard and Eurachem guidelines were followed. With this in mind, selectivity, working range, linearity, recovery (from 92% to 102%), repeatability (1%-4%), intermediate precision (2%-6%), limits of detection (0.001-0.08 ng L- 1) were systematically assessed. The total uncertainty associated to each result was estimated and the main sources of uncertainty sorted out. All major contributions to the combined uncertainty of the obtained results were identified and propagated together, following the ISO/GUM guidelines. The relative expanded uncertainty was estimated at range from 10.4% to 11.6% (k = 2). Demonstration of traceability of measurement results was also presented. Due to the low limits of detection, this method enables the determination of ultra-low levels of REEs in the open seawater as well as small variations in their concentrations. The potential of the proposed analytical procedure, based on combination of seaFAST-pico™ for sample preparation and HR ICP-SFMS, was demonstrated by direct analysis of seawater form different regions of the world.

  10. High-resolution high-sensitivity elemental imaging by secondary ion mass spectrometry: from traditional 2D and 3D imaging to correlative microscopy

    International Nuclear Information System (INIS)

    Wirtz, T; Philipp, P; Audinot, J-N; Dowsett, D; Eswara, S

    2015-01-01

    Secondary ion mass spectrometry (SIMS) constitutes an extremely sensitive technique for imaging surfaces in 2D and 3D. Apart from its excellent sensitivity and high lateral resolution (50 nm on state-of-the-art SIMS instruments), advantages of SIMS include high dynamic range and the ability to differentiate between isotopes. This paper first reviews the underlying principles of SIMS as well as the performance and applications of 2D and 3D SIMS elemental imaging. The prospects for further improving the capabilities of SIMS imaging are discussed. The lateral resolution in SIMS imaging when using the microprobe mode is limited by (i) the ion probe size, which is dependent on the brightness of the primary ion source, the quality of the optics of the primary ion column and the electric fields in the near sample region used to extract secondary ions; (ii) the sensitivity of the analysis as a reasonable secondary ion signal, which must be detected from very tiny voxel sizes and thus from a very limited number of sputtered atoms; and (iii) the physical dimensions of the collision cascade determining the origin of the sputtered ions with respect to the impact site of the incident primary ion probe. One interesting prospect is the use of SIMS-based correlative microscopy. In this approach SIMS is combined with various high-resolution microscopy techniques, so that elemental/chemical information at the highest sensitivity can be obtained with SIMS, while excellent spatial resolution is provided by overlaying the SIMS images with high-resolution images obtained by these microscopy techniques. Examples of this approach are given by presenting in situ combinations of SIMS with transmission electron microscopy (TEM), helium ion microscopy (HIM) and scanning probe microscopy (SPM). (paper)

  11. Mass Spectrometry Applications for Toxicology.

    Science.gov (United States)

    Mbughuni, Michael M; Jannetto, Paul J; Langman, Loralie J

    2016-12-01

    Toxicology is a multidisciplinary study of poisons, aimed to correlate the quantitative and qualitative relationships between poisons and their physiological and behavioural effects in living systems. Other key aspects of toxicology focus on elucidation of the mechanisms of action of poisons and development of remedies and treatment plans for associated toxic effects. In these endeavours, Mass spectrometry (MS) has become a powerful analytical technique with a wide range of application used in the Toxicological analysis of drugs, poisons, and metabolites of both. To date, MS applications have permeated all fields of toxicology which include; environmental, clinical, and forensic toxicology. While many different analytical applications are used in these fields, MS and its hyphenated applications such as; gas chromatography MS (GC-MS), liquid chromatography MS (LC-MS), inductively coupled plasma ionization MS (ICP-MS), tandem mass spectrometry (MS/MS and MS n ) have emerged as powerful tools used in toxicology laboratories. This review will focus on these hyphenated MS technologies and their applications for toxicology.

  12. Mass Spectrometry Applications for Toxicology

    Science.gov (United States)

    Mbughuni, Michael M.; Jannetto, Paul J.

    2016-01-01

    Toxicology is a multidisciplinary study of poisons, aimed to correlate the quantitative and qualitative relationships between poisons and their physiological and behavioural effects in living systems. Other key aspects of toxicology focus on elucidation of the mechanisms of action of poisons and development of remedies and treatment plans for associated toxic effects. In these endeavours, Mass spectrometry (MS) has become a powerful analytical technique with a wide range of application used in the Toxicological analysis of drugs, poisons, and metabolites of both. To date, MS applications have permeated all fields of toxicology which include; environmental, clinical, and forensic toxicology. While many different analytical applications are used in these fields, MS and its hyphenated applications such as; gas chromatography MS (GC-MS), liquid chromatography MS (LC-MS), inductively coupled plasma ionization MS (ICP-MS), tandem mass spectrometry (MS/MS and MSn) have emerged as powerful tools used in toxicology laboratories. This review will focus on these hyphenated MS technologies and their applications for toxicology. PMID:28149262

  13. Flow injection on-line dilution for multi-element determination in human urine with detection by inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald; Gammelgaard, Bente

    2001-01-01

    A simple flow injection on-line dilution procedure with detection by inductively coupled plasma mass spectrometry (ICP-MS) was developed for the determination of copper, zinc, arsenic, lead, selenium, nickel and molybdenum in human urine. Matrix effects were minimized by employing a dilution factor...

  14. Inductively coupled plasma source mass spectrometry

    International Nuclear Information System (INIS)

    Price Russ, G. III

    1993-01-01

    Inductively coupled plasma source mass spectrometry (ICP-MS) is a relatively new (5 y commercial availability) technique for simultaneously determining the concentration and isotopic composition of a large number of elements at trace levels. The principle advantages of ICP-MS are the ability to measure essentially all the metallic elements at concentrations as low as 1 part in 10 12 by weight, to analyse aqueous samples directly, to determine the isotopic composition of essentially all the metallic elements, and to analyse samples rapidly (minutes). The history of the development of ICP-MS and discussions of a variety of applications have been discussed in detail in Date and Gray (1988). Koppenaal (1988, 1990) has reviewed the ICP-MS literature. In that ICP-MS is a relatively new and still evolving technique, this chapter will discuss potential capability more than proven performance. (author). 24 refs

  15. Depth resolution of secondary ion mass spectrometry

    International Nuclear Information System (INIS)

    Pustovit, A.N.

    2004-01-01

    The effect of the solid body discreteness in the direction of the normal to the sample surface on the depth resolution of the secondary ion mass spectrometry method is analyzed. It is shown that for this case the dependence of the width at the semi-height of the delta profiles of the studied elements depth distribution on the energy and angle of incidence of the initial ions should have the form of the stepwise function. This is experimentally proved by the silicon-germanium delta-layers in the silicon samples [ru

  16. Role of Mass Spectrometry in Clinical Endocrinology.

    Science.gov (United States)

    Ketha, Siva S; Singh, Ravinder J; Ketha, Hemamalini

    2017-09-01

    The advent of mass spectrometry into the clinical laboratory has led to an improvement in clinical management of several endocrine diseases. Liquid chromatography tandem mass spectrometry found some of its first clinical applications in the diagnosis of inborn errors of metabolism, in quantitative steroid analysis, and in drug analysis laboratories. Mass spectrometry assays offer analytical sensitivity and specificity that is superior to immunoassays for many analytes. This article highlights several areas of clinical endocrinology that have witnessed the use of liquid chromatography tandem mass spectrometry to improve clinical outcomes. Copyright © 2017 Elsevier Inc. All rights reserved.

  17. Accelerator mass spectrometry in NIPNE

    International Nuclear Information System (INIS)

    Ivascu, M; Marinescu, L.; Dima, R.; Cata-Danil, D.; Petrascu, M.; Popescu, I.; Stan-Sion, C.; Radulescu, M.; Plostinaru, D.

    1997-01-01

    The Accelerator Mass Spectrometry (AMS) is today the method capable to measure the lowest concentration of a particular nuclide in sample materials. The method has applications in environmental physics, medicine, measurements of cosmic-ray or nuclear power plant produced radionuclides in the earth's atmosphere. All over the world, more than 40 charged particles and heavy ion accelerators are performing such analyses concerning the research interest of a huge number of laboratories. The Romanian Institute of Nuclear Physics and Engineering in Bucharest has initiated a construction project for the AMS facility at the FN - Van de Graaff Tandem accelerator. This program benefits of technical and financial assistance provided by IAEA in the frame of the IAEA-TC Project ROM 8014-265C. A general lay-out of the AMS project is presented. The construction work has begun and first tests of the AMS injector will take place between July - September this year. (authors)

  18. A REVIEW ON MASS SPECTROMETRY DETECTORS

    OpenAIRE

    Khatri Neetu; Gupta Ankit; Taneja Ruchi; Bilandi Ajay; Beniwal Prashant

    2012-01-01

    Mass spectrometry is an analytical technique for "weighing" molecules. Obviously, this is not done with a conventional scale or balance. Instead, mass spectrometry is based upon the principle of the motion of a charged particle that is called an ion, in an electric or magnetic field. The mass to charge ratio (m/z) of the ion affects particles motion. Since the charge of an electron is known, the mass to charge ratio (m/z) is a measurement of mass of an ion. Mass spectrometry research focuses ...

  19. Determination of rare earth elements in seawater by inductively coupled plasma mass spectrometry with off-line column preconcentration using 2,6-diacetylpyridine functionalized Amberlite XAD-4

    Energy Technology Data Exchange (ETDEWEB)

    Karadas, Cennet [Department of Chemistry, Art and Science Faculty, Balikesir University, 10100 Balikesir (Turkey); Kara, Derya, E-mail: dkara@balikesir.edu.tr [Department of Chemistry, Art and Science Faculty, Balikesir University, 10100 Balikesir (Turkey); Fisher, Andrew [School of Geography, Earth and Environmental Sciences, University of Plymouth, Drake Circus, Plymouth, Devon PL4 8AA (United Kingdom)

    2011-03-18

    An off-line column preconcentration technique using a micro-column of 2,6 diacetylpyridine functionalized Amberlite XAD-4 with inductively coupled plasma mass spectrometry (ICP-MS) as a means of detection has been developed. The aim of the method was to determine rare earth elements (REEs) (La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu) in seawater. Sample solutions (2-10 mL) were passed through the column which was then washed with ultra-pure water to remove residual matrix. The adsorbed cations on the resin were eluted by using 2 mL of 0.1 mol L{sup -1} HNO{sub 3} containing 10 ng mL{sup -1} indium as an internal standard. The eluent was analyzed for the metal concentrations using ICP-MS. Sample pH as well as the sample and eluent flow rates were optimized. The sorption capacity of resin was determined by the batch process, by equilibrating 0.05 g of the resin with solutions of 50 mL of 25 mg L{sup -1} of individual metal ions for 4 h at pH 6.0 at 26 deg. C. The sorption capacities for the resin were found to range between 47.3 {mu}mol g{sup -1} (for Lu) and 136.7 {mu}mol g{sup -1} (for Gd). Limits of detection (3{sigma}), without any preconcentration, ranged from 2 ng L{sup -1} to 10.3 ng L{sup -1} (for Tm and Lu respectively). The proposed method was applied to the determination of REEs in seawater and tap water samples.

  20. On the elemental analysis of different cigarette brands using laser induced breakdown spectroscopy and laser-ablation time of flight mass spectrometry

    Science.gov (United States)

    Ahmed, Nasar; Umar, Zeshan A.; Ahmed, Rizwan; Aslam Baig, M.

    2017-10-01

    We present qualitative and quantitative analysis of the trace elements present in different brands of tobacco available in Pakistan using laser induced breakdown spectroscopy (LIBS) and Laser ablation Time of Flight Mass Spectrometer (LA-TOFMS). The compositional analysis using the calibration free LIBS technique is based on the observed emission spectra of the laser produced plasma plume whereas the elemental composition analysis using LA-TOFMS is based on the mass spectra of the ions produced by laser ablation. The optical emission spectra of these samples contain spectral lines of calcium, magnesium, sodium, potassium, silicon, strontium, barium, lithium and aluminum with varying intensities. The corresponding mass spectra of the elements were detected in LA-TOF-MS with their composition concentration. The analysis of different brands of cigarettes demonstrates that LIBS coupled with a LA-TOF-MS is a powerful technique for the elemental analysis of the trace elements in any solid sample.

  1. Alpha spectrometry and secondary ion mass spectrometry of thorium

    International Nuclear Information System (INIS)

    Strisovska, Jana; Kuruc, Jozef; Galanda, Dusan; Matel, Lubomir; Velic, Dusan; Aranyosiova, Monika

    2009-01-01

    A sample of thorium content on steel discs was prepared by electrodeposition with a view to determining the natural thorium isotope. Thorium was determined by alpha spectrometry and by secondary ion mass spectrometry and the results of the two methods were compared

  2. NICHD Biomedical Mass Spectrometry Core Facility

    Data.gov (United States)

    Federal Laboratory Consortium — The NICHD Biomedical Mass Spectrometry Core Facility was created under the auspices of the Office of the Scientific Director to provide high-end mass-spectrometric...

  3. Atom counting with accelerator mass spectrometry

    International Nuclear Information System (INIS)

    Kutschera, Walter

    1995-01-01

    A brief review of the current status and some recent applications of accelerator mass spectrometry (AMS) are presented. Some connections to resonance ionization mass spectroscopy (RIS) as the alternate atom counting method are discussed

  4. Recent development in isotope ratio mass spectrometry

    International Nuclear Information System (INIS)

    Platzner, I.

    1992-01-01

    Within the limited of this review the following topics will be briefly discussed: a) Accuracy, precision, internal relative standard deviation (RISD) and external relative standard deviation (RESD) of isotope ratio measurements. With advanced instrumentation and use of standard reference materials, high accuracy and RESD = 0.002% (or better) may be achieved; b) The advantages of modern automatic isotope ratio mass spectrometer are briefly described. Computer controlled operation and data acquisition, and multiple ion collection are the recent important improvement; c) The isotopic fractionation during the course of isotope ratio measurement is considered as a major source of errors in thermal ionization of metallic elements. The phenomenon in strontium, neodymium, uranium, lead and calcium and methods to correct the measured data are discussed; d) Applications of isotope ratio mass spectrometry in atomic weight determinations, the isotope dilution technique, isotope geology, and isotope effects in biological systems are described together with specific applications in various research and technology area. (author)

  5. Mass spectrometry-assisted protease substrate screening

    DEFF Research Database (Denmark)

    Schlüter, Hartmut; Rykl, Jana; Thiemann, Joachim

    2007-01-01

    -phase chromatography they are analyzed by tandem mass spectrometry and the substrates identified by database searching. The proof of principle in this study is demonstrated by incubating immobilized human plasma proteins with thrombin and by identifying by tandem mass spectrometry the fibrinopeptides, released...

  6. Inorganic mass spectrometry of solid samples

    International Nuclear Information System (INIS)

    Adams, F.; Vertes, A.

    1990-01-01

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

  7. Surface analysis by imaging mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Vidová, Veronika; Volný, Michael; Lemr, Karel; Havlíček, Vladimír

    2009-01-01

    Roč. 74, 7-8 (2009), s. 1101-1116 ISSN 0010-0765 Institutional research plan: CEZ:AV0Z50200510 Keywords : secondary ion mass spectrometry * matrix assisted laser desorption ionization * mass spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 0.856, year: 2009

  8. Introduction to mass spectrometry-based proteomics

    DEFF Research Database (Denmark)

    Matthiesen, R.; Bunkenborg, J.

    2013-01-01

    Mass spectrometry has been widely applied to study biomolecules and one rapidly developing field is the global analysis of proteins, proteomics. Understanding and handling mass spectrometry data is a multifaceted task that requires many decisions to be made to get the most comprehensive informati...

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

    International Nuclear Information System (INIS)

    Ewinger, H.P.

    1993-05-01

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

  10. Zero voltage mass spectrometry probes and systems

    Science.gov (United States)

    Cooks, Robert Graham; Wleklinski, Michael Stanley; Bag, Soumabha; Li, Yafeng

    2017-10-10

    The invention generally relates to zero volt mass spectrometry probes and systems. In certain embodiments, the invention provides a system including a mass spectrometry probe including a porous material, and a mass spectrometer (bench-top or miniature mass spectrometer). The system operates without an application of voltage to the probe. In certain embodiments, the probe is oriented such that a distal end faces an inlet of the mass spectrometer. In other embodiments, the distal end of the probe is 5 mm or less from an inlet of the mass spectrometer.

  11. Mass spectrometry at the Pittsburgh conference

    International Nuclear Information System (INIS)

    Borman, S.

    1987-01-01

    Each year analytical chemists flock to the Pittsburgh Conference to learn about the latest trends in analytical instrumentation. In this Focus, a number of prominent mass spectroscopists who attended this year's meeting in Atlantic City, NJ, discuss their perceptions of current developments in the field of mass spectrometry (MS). In the June 1 issue of Analytical Chemistry, the authors coverage of the Pittsburgh Conferences continues with a follow-up article on specific developments in hyphenated mass spectrometry - primarily liquid chromatography - MS (LC/MS) and gas chromatography - infrared spectrometry MS (GC/IR/MS)

  12. Chromatography–mass spectrometry in aerospace industry

    International Nuclear Information System (INIS)

    Buryak, Alexey K; Serduk, T M

    2013-01-01

    The applications of chromatography–mass spectrometry in aerospace industry are considered. The primary attention is devoted to the development of physicochemical grounds of the use of various chromatography–mass spectrometry procedures to solve topical problems of this industry. Various methods for investigation of the composition of rocket fuels, surfaces of structural materials and environmental media affected by aerospace activities are compared. The application of chromatography–mass spectrometry for the development and evaluation of processes for decontaminations of equipment, industrial wastes and soils from rocket fuel components is substantiated. The bibliography includes 135 references.

  13. Ultra-sensitive radionuclide spectrometry. Radiometrics and mass spectrometry synergy

    International Nuclear Information System (INIS)

    Povinec, P.P.

    2005-01-01

    Recent developments in radiometrics and mass spectrometry techniques for ultra-sensitive analysis of radionuclides in the marine environment are reviewed. In the radiometrics sector the dominant development has been the utilization of large HPGe detectors in underground laboratories with anti-cosmic or anti-Compton shielding for the analysis of short and medium-lived radionuclides in the environment. In the mass spectrometry sector, applications of inductively coupled plasma mass spectrometry (ICP-MS) and accelerator mass spectrometry (AMS) for the analysis of long-lived radionuclides in the environment are the most important recent achievements. The recent developments do not only considerably decrease the detection limits for several radionuclides (up to several orders of magnitude), but they also enable to decrease sample volumes so that sampling, e.g., of the water column can be much easier and more effective. A comparison of radiometrics and mass spectrometry results for the analysis of radionuclides in the marine environment shows a reasonable agreement - within quoted uncertainties, for wide range of activities and different sample matrices analyzed. (author)

  14. Analytical evaluation of nebulizers for the introduction of acetic acid extracts aiming at the determination of trace elements by inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Gois, Jefferson S. de; Maranhao, Tatiane de A. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-970, Florianopolis, SC (Brazil); Oliveira, Fernando J.S. [Petroleo Brasileiro S.A., Gerencia de Meio Ambiente, Rio de Janeiro, RJ (Brazil); Frescura, Vera L.A.; Curtius, Adilson J. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-970, Florianopolis, SC (Brazil); Borges, Daniel L.G., E-mail: daniel.borges@ufsc.br [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-970, Florianopolis, SC (Brazil)

    2012-11-15

    Most of the official procedures aiming at classification of solid waste toxicity take into account metal solubility and bioavailability by means of extraction experiments using acetic acid solutions. Hence, the aim of this work was to investigate and optimize conditions to suppress the effect of acetic acid on the determination of trace elements using inductively coupled plasma mass spectrometry. The performance of four nebulizers (cross-flow (CFN), ultrasonic (USN), Meinhard (MN) and MicroMist (MMN)) were compared as to their efficiency in minimizing spectral and non-spectral effects on the determination of Ag, As, Ba, Cd, Cr, Hg, Pb and Se, with the ultimate goal to analyze acetic acid extracts obtained from solid waste residues. Operating conditions (desolvation temperatures for USN, RF power and nebulizer gas flow rates) were optimized individually for each nebulizer and for all analytes maintained in 0.14 mol L{sup -1} HNO{sub 3} solutions and in solutions prepared with acetic acid and acetic acid + NaOH, adjusted to pH 2.88 and 4.93, respectively. Pronounced non-spectral interferences for {sup 75}As and {sup 82}Se were observed in the presence of acetic acid for CF and MN, although to a less extent also for MMN and USN. Signal increase for blank solutions measured at m/z 208 ({sup 208}Pb) for CFN and MN, 107 ({sup 107}Ag) for USN and MN coupled to a cyclonic chamber and, m/z 82 ({sup 82}Se) for USN was observed, indicating an increased risk of spectral interference upon an increase in the concentration of acetic acid. Signal increase at specific m/z ratios, however, was not significant when the MMN was used, with the exception of m/z 52 ({sup 52}Cr) in acetic acid solutions, arising from the formation of {sup 40}Ar{sup 12}C{sup +}. This same effect was noticed for all nebulizers, although at noticeably different intensities. A signal stability study was performed, demonstrating that variations in the analytical signal were within a 20% range for all analytes

  15. Elemental analysis of coal by tandem laser induced breakdown spectroscopy and laser ablation inductively coupled plasma time of flight mass spectrometry

    International Nuclear Information System (INIS)

    Dong, Meirong; Oropeza, Dayana; Chirinos, José; González, Jhanis J.; Lu, Jidong; Mao, Xianglei; Russo, Richard E.

    2015-01-01

    The capabilities and analytical benefits of combined LIBS and LA-ICP-MS were evaluated for the analysis of coal samples. The ablation system consisted of a Nd:YAG laser operated 213 nm. A Czerny-turner spectrograph with ICCD detector and time-of-flight based mass spectrometer were utilized for LIBS and ICP-MS detection, respectively. This tandem approach allows simultaneous determination of major and minor elements (C, Si, Ca, Al, Mg), and trace elements (V, Ba, Pb, U, etc.) in the coal samples. The research focused on calibration strategies, specifically the use of univariate and multivariate data analysis on analytical performance. Partial least square regression (PLSR) was shown to minimize and compensate for matrix effects in the emission and mass spectra improving quantitative analysis by LIBS and LA-ICP-MS, respectively. The correlation between measurements from these two techniques demonstrated that mass spectral data combined with LIBS emission measurements by PLSR improved the accuracy and precision for quantitative analysis of trace elements in coal. - Highlights: • Tandem LIBS LA-ICP-MS • Simultaneous determination of major and minor elements and trace elements in the coal samples. • Extended Dynamic Range • Correlation between LIBS with LA-ICP-MS demonstrated improved the accuracy and precision for quantitative analysis of coal

  16. Elemental analysis of coal by tandem laser induced breakdown spectroscopy and laser ablation inductively coupled plasma time of flight mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Dong, Meirong [School of Electric Power, South China University of Technology, Guangzhou, Guangdong 510640 (China); Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States); Oropeza, Dayana [Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States); Chirinos, José [Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States); Escuela de Química, Facultad de Ciencias, Universidad Central de Venezuela, Caracas 1041a (Venezuela, Bolivarian Republic of); González, Jhanis J. [Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States); Lu, Jidong [School of Electric Power, South China University of Technology, Guangzhou, Guangdong 510640 (China); Mao, Xianglei [Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States); Russo, Richard E., E-mail: RERusso@lbl.gov [Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States)

    2015-07-01

    The capabilities and analytical benefits of combined LIBS and LA-ICP-MS were evaluated for the analysis of coal samples. The ablation system consisted of a Nd:YAG laser operated 213 nm. A Czerny-turner spectrograph with ICCD detector and time-of-flight based mass spectrometer were utilized for LIBS and ICP-MS detection, respectively. This tandem approach allows simultaneous determination of major and minor elements (C, Si, Ca, Al, Mg), and trace elements (V, Ba, Pb, U, etc.) in the coal samples. The research focused on calibration strategies, specifically the use of univariate and multivariate data analysis on analytical performance. Partial least square regression (PLSR) was shown to minimize and compensate for matrix effects in the emission and mass spectra improving quantitative analysis by LIBS and LA-ICP-MS, respectively. The correlation between measurements from these two techniques demonstrated that mass spectral data combined with LIBS emission measurements by PLSR improved the accuracy and precision for quantitative analysis of trace elements in coal. - Highlights: • Tandem LIBS LA-ICP-MS • Simultaneous determination of major and minor elements and trace elements in the coal samples. • Extended Dynamic Range • Correlation between LIBS with LA-ICP-MS demonstrated improved the accuracy and precision for quantitative analysis of coal.

  17. 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)

    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 -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

  18. Tandem mass spectrometry at low kinetic energy

    International Nuclear Information System (INIS)

    Cooks, R.G.; Hand, O.W.

    1987-01-01

    Recent progress in mass spectrometry, as applied to molecular analysis, is reviewed with emphasis on tandem mass spectrometry. Tandem instruments use multiple analyzers (sector magnets, quadrupole mass filters and time-of-flight devices) to select particular molecules in ionic form, react them in the gas-phase and then record the mass, momenta or kinetic energies of their products. The capabilities of tandem mass spectrometry for identification of individual molecules or particular classes of compounds in complex mixtures are illustrated. Several different types of experiments can be run using a tandem mass spectrometer; all share the feature of sifting the molecular mixture being analyzed on the basis of chemical properties expressed in terms of ionic mass, kinetic energy or charge state. Applications of mass spectrometry to biological problems often depend upon desorption methods of ionization in which samples are bombarded with particle beams. Evaporation of preformed charged species from the condensed phase into the vacuum is a particularly effective method of ionization. It is suggested that the use of accelerator mass spectrometers be extended to include problems of molecular analysis. In such experiments, low energy tandem mass spectrometry conducted in the eV or keV range of energies, would be followed by further characterization of the production ion beam using high selective MeV collision processes

  19. Methods for recalibration of mass spectrometry data

    Science.gov (United States)

    Tolmachev, Aleksey V [Richland, WA; Smith, Richard D [Richland, WA

    2009-03-03

    Disclosed are methods for recalibrating mass spectrometry data that provide improvement in both mass accuracy and precision by adjusting for experimental variance in parameters that have a substantial impact on mass measurement accuracy. Optimal coefficients are determined using correlated pairs of mass values compiled by matching sets of measured and putative mass values that minimize overall effective mass error and mass error spread. Coefficients are subsequently used to correct mass values for peaks detected in the measured dataset, providing recalibration thereof. Sub-ppm mass measurement accuracy has been demonstrated on a complex fungal proteome after recalibration, providing improved confidence for peptide identifications.

  20. Pyrolysis - gas chromatography - mass spectrometry of lignins

    Energy Technology Data Exchange (ETDEWEB)

    Martin, F; Saiz-Jimenez, C; Gonzalez-Vila, F J

    1979-01-01

    Milled wood lignins from spruce, beech and bamboo were pyrolysed. The high-boiling products of pyrolysis were studied by GLC and mass spectrometry. The forty-three products identified provide information on the structural units of lignin.

  1. Mass Spectrometry-Based Biomarker Discovery.

    Science.gov (United States)

    Zhou, Weidong; Petricoin, Emanuel F; Longo, Caterina

    2017-01-01

    The discovery of candidate biomarkers within the entire proteome is one of the most important and challenging goals in proteomic research. Mass spectrometry-based proteomics is a modern and promising technology for semiquantitative and qualitative assessment of proteins, enabling protein sequencing and identification with exquisite accuracy and sensitivity. For mass spectrometry analysis, protein extractions from tissues or body fluids and subsequent protein fractionation represent an important and unavoidable step in the workflow for biomarker discovery. Following extraction of proteins, the protein mixture must be digested, reduced, alkylated, and cleaned up prior to mass spectrometry. The aim of our chapter is to provide comprehensible and practical lab procedures for sample digestion, protein fractionation, and subsequent mass spectrometry analysis.

  2. Radiation Biomarker Research Using Mass Spectrometry

    National Research Council Canada - National Science Library

    Bach, Stephan B; Hubert, Walter

    2007-01-01

    .... This review is intended to give an overview of mass spectrometry and its application to biological systems and biomarker discovery and how that might relate to relevant radiation dosimetry studies...

  3. Mass Spectrometry Analyses of Multicellular Tumor Spheroids.

    Science.gov (United States)

    Acland, Mitchell; Mittal, Parul; Lokman, Noor A; Klingler-Hoffmann, Manuela; Oehler, Martin K; Hoffmann, Peter

    2018-05-01

    Multicellular tumor spheroids (MCTS) are a powerful biological in vitro model, which closely mimics the 3D structure of primary avascularized tumors. Mass spectrometry (MS) has established itself as a powerful analytical tool, not only to better understand and describe the complex structure of MCTS, but also to monitor their response to cancer therapeutics. The first part of this review focuses on traditional mass spectrometry approaches with an emphasis on elucidating the molecular characteristics of these structures. Then the mass spectrometry imaging (MSI) approaches used to obtain spatially defined information from MCTS is described. Finally the analysis of primary spheroids, such as those present in ovarian cancer, and the great potential that mass spectrometry analysis of these structures has for improved understanding of cancer progression and for personalized in vitro therapeutic testing is discussed. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Mass spectrometry in life science research.

    Science.gov (United States)

    Lehr, Stefan; Markgraf, Daniel

    2016-12-01

    Investigating complex signatures of biomolecules by mass spectrometry approaches has become indispensable in molecular life science research. Nowadays, various mass spectrometry-based omics technologies are available to monitor qualitative and quantitative changes within hundreds or thousands of biological active components, including proteins/peptides, lipids and metabolites. These comprehensive investigations have the potential to decipher the pathophysiology of disease development at a molecular level and to monitor the individual response of pharmacological treatment or lifestyle intervention.

  5. Determination of δ13C, δ15N, or δ34S by isotope-ratio-monitoring mass spectrometry using an elemental analyzer

    Science.gov (United States)

    Johnson, Craig A.; Stricker, Craig A.; Gulbransen, Cayce A.; Emmons, Matthew P.

    2018-02-14

    This report describes procedures used in the Geology, Geophysics, and Geochemistry Science Center of the U.S. Geological Survey in Denver, Colorado, to determine the stable-isotope ratios 13C/12C, 15N/14N, and 34S/32S in solid materials. The procedures use elemental analyzers connected directly to gas-source isotope-ratio mass spectrometers. A different elemental–analyzer–mass-spectrometer system is used for 13C/12C and 15N/14N than is used for 34S/32S to accommodate differences in reagents, catalysts, and instrument settings.

  6. Mass Spectrometry in the Home and Garden

    Science.gov (United States)

    Pulliam, Christopher J.; Bain, Ryan M.; Wiley, Joshua S.; Ouyang, Zheng; Cooks, R. Graham

    2015-02-01

    Identification of active components in a variety of chemical products used directly by consumers is described at both trace and bulk levels using mass spectrometry. The combination of external ambient ionization with a portable mass spectrometer capable of tandem mass spectrometry provides high chemical specificity and sensitivity as well as allowing on-site monitoring. These experiments were done using a custom-built portable ion trap mass spectrometer in combination with the ambient ionization methods of paper spray, leaf spray, and low temperature plasma ionization. Bactericides, garden chemicals, air fresheners, and other products were examined. Herbicide applied to suburban lawns was detected in situ on single leaves 5 d after application.

  7. Dynamic Secondary Ion Mass Spectrometry | Materials Science | NREL

    Science.gov (United States)

    Ion Mass Spectrometry (SIMS) uses a continuous, focused beam of primary ions to remove material from the surface of a sample by sputtering. The fraction of sputtered material that is ionized is extracted Identifies all elements or isotopes present in a material, from hydrogen to uranium. Different primary-ion

  8. Elucidating rhizosphere processes by mass spectrometry – A review

    Energy Technology Data Exchange (ETDEWEB)

    Rugova, Ariana [Division of Analytical Chemistry, Department of Chemistry, University of Natural Resources and Life Sciences-BOKU, Vienna (Austria); Puschenreiter, Markus [Department of Forest and Soil Sciences, Rhizosphere Ecology and Biogeochemistry Group, University of Natural Resources and Life Sciences-BOKU, Vienna (Austria); Koellensperger, Gunda [Institute of Analytical Chemistry, Faculty of Chemistry, University of Vienna, Vienna (Austria); Hann, Stephan, E-mail: stephan.hann@boku.ac.at [Division of Analytical Chemistry, Department of Chemistry, University of Natural Resources and Life Sciences-BOKU, Vienna (Austria)

    2017-03-01

    The presented review discusses state-of-the-art mass spectrometric methods, which have been developed and applied for investigation of chemical processes in the soil-root interface, the so-called rhizosphere. Rhizosphere soil's physical and chemical characteristics are to a great extent influenced by a complex mixture of compounds released from plant roots, i.e. root exudates, which have a high impact on nutrient and trace element dynamics in the soil-root interface as well as on microbial activities or soil physico-chemical characteristics. Chemical characterization as well as accurate quantification of the compounds present in the rhizosphere is a major prerequisite for a better understanding of rhizosphere processes and requires the development and application of advanced sampling procedures in combination with highly selective and sensitive analytical techniques. During the last years, targeted and non-targeted mass spectrometry-based methods have emerged and their combination with specific separation methods for various elements and compounds of a wide polarity range have been successfully applied in several studies. With this review we critically discuss the work that has been conducted within the last decade in the context of rhizosphere research and elemental or molecular mass spectrometry emphasizing different separation techniques as GC, LC and CE. Moreover, selected applications such as metal detoxification or nutrient acquisition will be discussed regarding the mass spectrometric techniques applied in studies of root exudates in plant-bacteria interactions. Additionally, a more recent isotope probing technique as novel mass spectrometry based application is highlighted. - Highlights: • State-of-the-art mass spectrometry methods developed and applied in rhizosphere research are reviewed. • Elemental and molecular mass spectrometry emphasizing different separation techniques (GC, LC or CE) are discussed. • Case studies on metal detoxification

  9. Elucidating rhizosphere processes by mass spectrometry – A review

    International Nuclear Information System (INIS)

    Rugova, Ariana; Puschenreiter, Markus; Koellensperger, Gunda; Hann, Stephan

    2017-01-01

    The presented review discusses state-of-the-art mass spectrometric methods, which have been developed and applied for investigation of chemical processes in the soil-root interface, the so-called rhizosphere. Rhizosphere soil's physical and chemical characteristics are to a great extent influenced by a complex mixture of compounds released from plant roots, i.e. root exudates, which have a high impact on nutrient and trace element dynamics in the soil-root interface as well as on microbial activities or soil physico-chemical characteristics. Chemical characterization as well as accurate quantification of the compounds present in the rhizosphere is a major prerequisite for a better understanding of rhizosphere processes and requires the development and application of advanced sampling procedures in combination with highly selective and sensitive analytical techniques. During the last years, targeted and non-targeted mass spectrometry-based methods have emerged and their combination with specific separation methods for various elements and compounds of a wide polarity range have been successfully applied in several studies. With this review we critically discuss the work that has been conducted within the last decade in the context of rhizosphere research and elemental or molecular mass spectrometry emphasizing different separation techniques as GC, LC and CE. Moreover, selected applications such as metal detoxification or nutrient acquisition will be discussed regarding the mass spectrometric techniques applied in studies of root exudates in plant-bacteria interactions. Additionally, a more recent isotope probing technique as novel mass spectrometry based application is highlighted. - Highlights: • State-of-the-art mass spectrometry methods developed and applied in rhizosphere research are reviewed. • Elemental and molecular mass spectrometry emphasizing different separation techniques (GC, LC or CE) are discussed. • Case studies on metal detoxification and

  10. Compound-specific isotope analysis of light elements using gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS) and its application to geochemistry

    International Nuclear Information System (INIS)

    Naraoka, Hiroshi; Yamada, Keita; Matsumoto, Kohei; Ishiwatari, Ryoshi

    1997-01-01

    Compound-specific isotope analysis has been developed recently using gas chromatography/combustion/mass spectrometry (GC/C/IRMS). This paper summarizes principles and progress of GC/C/IRMS, and reviews recent some important works using this new method. GC/C/IRMS is a novel tool for (1) biomarker analysis in sediments and living matter, (2) paleoenvironment analysis including reconstruction of ancient biogeochemical processes, (3) geochemical cycle study of organic compounds in a terrestrial-marine system, (4) evaluation of maturity and diagenesis of organic matter including petroleum formation, (5) ecological analysis, (6) evaluation of anthropologenic pollution in environment, (7) detection of extraterrestrial organic compounds and the formation mechanism study, (8) tracer studies in environment. (author)

  11. 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.

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  13. Optimization of on-line hydrogen stable isotope ratio measurements of halogen- and sulfur-bearing organic compounds using elemental analyzer–chromium/high-temperature conversion isotope ratio mass spectrometry (EA-Cr/HTC-IRMS)

    Science.gov (United States)

    Gehre, Matthias; Renpenning, Julian; Geilmann, Heike; Qi, Haiping; Coplen, Tyler B.; Kümmel, Steffen; Ivdra, Natalija; Brand, Willi A.; Schimmelmann, Arndt

    2017-01-01

    Rationale: Accurate hydrogen isotopic analysis of halogen- and sulfur-bearing organics has not been possible with traditional high-temperature conversion (HTC) because the formation of hydrogen-bearing reaction products other than molecular hydrogen (H2) is responsible for non-quantitative H2 yields and possible hydrogen isotopic fractionation. Our previously introduced, new chromium-based EA-Cr/HTC-IRMS (Elemental Analyzer–Chromium/High-Temperature Conversion Isotope Ratio Mass Spectrometry) technique focused primarily on nitrogen-bearing compounds. Several technical and analytical issues concerning halogen- and sulfur-bearing samples, however, remained unresolved and required further refinement of the reactor systems.

  14. Issues and opportunities in accelerator mass spectrometry for stable isotopes.

    Science.gov (United States)

    Matteson, Sam

    2008-01-01

    Accelerator mass spectrometry (AMS) has developed in the last 30 years many notable applications to the spectrometry of radioisotopes, particularly in radiocarbon dating. The instrumentation science of trace element AMS (TEAMS) that analyzes stable isotopes, also called Accelerator SIMS or MegaSIMS, while unique in many features, has also shared in many of these significant advances and has pushed TEAMS sensitivity to concentration levels surpassing many competing mass spectroscopic technologies. This review examines recent instrumentation developments, the capabilities of the new instrumentation and discernable trends for future development. Copyright 2008 Wiley Periodicals, Inc.

  15. Analysis of mass spectrometry data in proteomics

    DEFF Research Database (Denmark)

    Matthiesen, Rune; Jensen, Ole N

    2008-01-01

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

  16. Mass spectrometry: a revolution in clinical microbiology?

    Science.gov (United States)

    Lavigne, Jean-Philippe; Espinal, Paula; Dunyach-Remy, Catherine; Messad, Nourredine; Pantel, Alix; Sotto, Albert

    2013-02-01

    Recently, different bacteriological laboratory interventions that decrease reporting time have been developed. These promising new broad-based techniques have merit, based on their ability to identify rapidly many bacteria, organisms difficult to grow or newly emerging strains, as well as their capacity to track disease transmission. The benefit of rapid reporting of identification and/or resistance of bacteria can greatly impact patient outcomes, with an improvement in the use of antibiotics, in the reduction of the emergence of multidrug resistant bacteria and in mortality rates. Different techniques revolve around mass spectrometry (MS) technology: matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS), PCR combined with electrospray ionization-mass spectrometry (PCR/ESIMS), iPLEX MassArray system and other new evolutions combining different techniques. This report emphasizes the (r)evolution of these technologies in clinical microbiology.

  17. A new HF-resistant tandem spray chamber for improved determination of trace elements and Pb isotopes using inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Krachler, Michael; Rausch, Nicole; Feuerbacher, Helmut; Klemens, Patrick

    2005-01-01

    The use of a new HF-resistant tandem spray chamber arrangement consisting of a cyclonic spray chamber and a Scott-type spray chamber made from PFA and PEEK provides a straightforward approach for improving the performance of inductively coupled-mass spectrometry (ICP-MS). The characteristics of the tandem spray chamber were critically evaluated against a PEEK cyclonic and a PFA Scott-type spray chamber, respectively. Sensitivity across the entire mass range was increased by about three times compared to the conventional setup utilizing only one spray chamber. Precision of the results, especially at low signal intensities, improved by 160% and 31% compared to the cyclonic and Scott-type spray chamber, respectively. Using the tandem spray chamber, the oxide formation rate was lowered by about 50%. Signals as low as 30 counts could be determined under routine measurement conditions with a RSD of 2.4% thus allowing to precisely quantify small concentration differences at the ng l -1 concentration level. The excellent precision (0.02-0.07%) of 206 Pb / 207 Pb and 206 Pb / 208 Pb ratios determined in pore water samples was rather limited by the instrumental capabilities of the single collector ICP-MS instrument than by the performance of the tandem spray chamber

  18. Trace elements in free-range hen eggs in the Campania region (Italy) analyzed by inductively coupled plasma mass spectrometry (ICP-MS).

    Science.gov (United States)

    Esposito, Mauro; Cavallo, Stefania; Chiaravalle, Eugenio; Miedico, Oto; Pellicanò, Roberta; Rosato, Guido; Sarnelli, Paolo; Baldi, Loredana

    2016-06-01

    Eggs from hens raised on rural or domestic farms are a good indicator of environmental contamination, as the hens are in close contact with the ground and the air and can therefore accumulate heavy metals and other toxic contaminants from the environment as well as from the diet. In this paper, we report the results of the determination of 19 trace elements (As, Be, Cd, Co, Cr, Cu, Hg, Mo, Mn, Ni, Pb, Sb, Se, Sn, Sr, Tl, U, V, Zn) in 39 hen egg samples collected from domestic poultry farms in the territory dubbed the "Land of fires" in the Campania region (Italy). This area is characterized by environmental problems caused by the illegal dumping of industrial or domestic waste in fields or by roadsides. In some cases, these wastes have been burned, thereby spreading persistent contaminants into the atmosphere. The content of trace elements in whole egg samples was determined by mass spectrometer after a microwave-assisted digestion procedure. Because European legislation does not indicate maximum values of these elements in this foodstuff, the results were compared with the content of trace elements reported in literature for eggs, in particular home-produced eggs, in various countries. In some cases (Cd, Cu, Ni, Mn), the content determined in this study was in line with those reported elsewhere, in other cases (Pb, Cr), lower values were found.

  19. [Imaging Mass Spectrometry in Histopathologic Analysis].

    Science.gov (United States)

    Yamazaki, Fumiyoshi; Seto, Mitsutoshi

    2015-04-01

    Matrix-assisted laser desorption/ionization (MALDI)-imaging mass spectrometry (IMS) enables visualization of the distribution of a range of biomolecules by integrating biochemical information from mass spectrometry with positional information from microscopy. IMS identifies a target molecule. In addition, IMS enables global analysis of biomolecules containing unknown molecules by detecting the ratio of the molecular weight to electric charge without any target, which makes it possible to identify novel molecules. IMS generates data on the distribution of lipids and small molecules in tissues, which is difficult to visualize with either conventional counter-staining or immunohistochemistry. In this review, we firstly introduce the principle of imaging mass spectrometry and recent advances in the sample preparation method. Secondly, we present findings regarding biological samples, especially pathological ones. Finally, we discuss the limitations and problems of the IMS technique and clinical application, such as in drug development.

  20. Sequencing Cyclic Peptides by Multistage Mass Spectrometry

    Science.gov (United States)

    Mohimani, Hosein; Yang, Yu-Liang; Liu, Wei-Ting; Hsieh, Pei-Wen; Dorrestein, Pieter C.; Pevzner, Pavel A.

    2012-01-01

    Some of the most effective antibiotics (e.g., Vancomycin and Daptomycin) are cyclic peptides produced by non-ribosomal biosynthetic pathways. While hundreds of biomedically important cyclic peptides have been sequenced, the computational techniques for sequencing cyclic peptides are still in their infancy. Previous methods for sequencing peptide antibiotics and other cyclic peptides are based on Nuclear Magnetic Resonance spectroscopy, and require large amount (miligrams) of purified materials that, for most compounds, are not possible to obtain. Recently, development of mass spectrometry based methods has provided some hope for accurate sequencing of cyclic peptides using picograms of materials. In this paper we develop a method for sequencing of cyclic peptides by multistage mass spectrometry, and show its advantages over single stage mass spectrometry. The method is tested on known and new cyclic peptides from Bacillus brevis, Dianthus superbus and Streptomyces griseus, as well as a new family of cyclic peptides produced by marine bacteria. PMID:21751357

  1. Parsimonious Charge Deconvolution for Native Mass Spectrometry

    Science.gov (United States)

    2018-01-01

    Charge deconvolution infers the mass from mass over charge (m/z) measurements in electrospray ionization mass spectra. When applied over a wide input m/z or broad target mass range, charge-deconvolution algorithms can produce artifacts, such as false masses at one-half or one-third of the correct mass. Indeed, a maximum entropy term in the objective function of MaxEnt, the most commonly used charge deconvolution algorithm, favors a deconvolved spectrum with many peaks over one with fewer peaks. Here we describe a new “parsimonious” charge deconvolution algorithm that produces fewer artifacts. The algorithm is especially well-suited to high-resolution native mass spectrometry of intact glycoproteins and protein complexes. Deconvolution of native mass spectra poses special challenges due to salt and small molecule adducts, multimers, wide mass ranges, and fewer and lower charge states. We demonstrate the performance of the new deconvolution algorithm on a range of samples. On the heavily glycosylated plasma properdin glycoprotein, the new algorithm could deconvolve monomer and dimer simultaneously and, when focused on the m/z range of the monomer, gave accurate and interpretable masses for glycoforms that had previously been analyzed manually using m/z peaks rather than deconvolved masses. On therapeutic antibodies, the new algorithm facilitated the analysis of extensions, truncations, and Fab glycosylation. The algorithm facilitates the use of native mass spectrometry for the qualitative and quantitative analysis of protein and protein assemblies. PMID:29376659

  2. Fourier transform ion cyclotron resonance mass spectrometry

    Science.gov (United States)

    Marshall, Alan G.

    1998-06-01

    As for Fourier transform infrared (FT-IR) interferometry and nuclear magnetic resonance (NMR) spectroscopy, the introduction of pulsed Fourier transform techniques revolutionized ion cyclotron resonance mass spectrometry: increased speed (factor of 10,000), increased sensitivity (factor of 100), increased mass resolution (factor of 10,000-an improvement not shared by the introduction of FT techniques to IR or NMR spectroscopy), increased mass range (factor of 500), and automated operation. FT-ICR mass spectrometry is the most versatile technique for unscrambling and quantifying ion-molecule reaction kinetics and equilibria in the absence of solvent (i.e., the gas phase). In addition, FT-ICR MS has the following analytically important features: speed (~1 second per spectrum); ultrahigh mass resolution and ultrahigh mass accuracy for analysis of mixtures and polymers; attomole sensitivity; MSn with one spectrometer, including two-dimensional FT/FT-ICR/MS; positive and/or negative ions; multiple ion sources (especially MALDI and electrospray); biomolecular molecular weight and sequencing; LC/MS; and single-molecule detection up to 108 Dalton. Here, some basic features and recent developments of FT-ICR mass spectrometry are reviewed, with applications ranging from crude oil to molecular biology.

  3. A history of mass spectrometry in Australia

    Energy Technology Data Exchange (ETDEWEB)

    Downard, K.M.; de Laeter, J.R. [University of Sydney, Sydney, NSW (Australia)

    2005-09-01

    An interest in mass spectrometry in Australia can be traced back to the 1920s with an early correspondence with Francis Aston who first visited these shores a decade earlier. The region has a rich tradition in both the development of the field and its application, from early measurements of ionization and appearance potentials by Jim Morrison at the Council for Scientific and Industrial Research (CSIR) around 1950 to the design and construction of instrumentation including the first use of a triple quadrupole mass spectrometer for tandem mass spectrometry, the first suite of programs to simulate ion optics (SIMION), the development of early TOF/TOF instruments and orthogonal acceleration and the local design and construction of several generations of a sensitive high-resolution ion microprobe (SHRIMP) instrument. Mass spectrometry has been exploited in the study and characterization of the constituents of this nation's unique flora and fauna from Australian apples, honey, tea plant and eucalyptus oil, snake, spider, fish and frog venoms, coal, oil, sediments and shale, environmental studies of groundwater to geochronological dating of limestone and granite, other terrestrial and meteoritic rocks and coral from the Great Barrier Reef. This article traces the history of mass spectrometry in its many guises and applications in the island continent of Australia. It focuses on contributions of scientists who played a major role in the early establishment of mass spectrometry in Australia. In general, those who are presently active in the field, and whose histories are incomplete, have been mentioned at best only briefly despite their important contributions to the field.

  4. Laser-induced mass spectrometry

    International Nuclear Information System (INIS)

    Polanyi, J.C.

    1981-01-01

    This invention provides a method for the spectroscopic analysis of gas. The gas molecules are internally excited by irradiation with laser light having a wavelength which is absorbed by the sample. The gas is then ionized and passed through a mass spectrometer and the amount of the ionized species in the irradiated and ionized sample is compared with that in a similar ionized but not irradiated sample

  5. Phylogenetic Analysis Using Protein Mass Spectrometry.

    Science.gov (United States)

    Ma, Shiyong; Downard, Kevin M; Wong, Jason W H

    2017-01-01

    Through advances in molecular biology, comparative analysis of DNA sequences is currently the cornerstone in the study of molecular evolution and phylogenetics. Nevertheless, protein mass spectrometry offers some unique opportunities to enable phylogenetic analyses in organisms where DNA may be difficult or costly to obtain. To date, the methods of phylogenetic analysis using protein mass spectrometry can be classified into three categories: (1) de novo protein sequencing followed by classical phylogenetic reconstruction, (2) direct phylogenetic reconstruction using proteolytic peptide mass maps, and (3) mapping of mass spectral data onto classical phylogenetic trees. In this chapter, we provide a brief description of the three methods and the protocol for each method along with relevant tools and algorithms.

  6. Inorganic trace analysis by laser ionization mass spectrometry

    International Nuclear Information System (INIS)

    Becker, S.; Dietze, H.J.

    1991-01-01

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

  7. Laser ionization mass spectrometry in inorganic trace analysis

    International Nuclear Information System (INIS)

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

    1992-01-01

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

  8. Determination of trace elements in biological samples treated with formic acid by inductively coupled plasma mass spectrometry using a microconcentric nebulizer

    International Nuclear Information System (INIS)

    Tormen, Luciano; Gil, Raul A.; Frescura, Vera L.A.; Dante Martinez, Luis; Curtius, Adilson J.

    2010-01-01

    A simple and fast method for the determination of As, Ba, Cd, Co, Cu, Fe, Ga, Mn, Mo, Ni, Pb, Rb, Se, Sr, Tl, U, V and Zn in biological samples by inductively coupled plasma mass spectrometry (ICP-MS), after sample solubilization with formic acid and introduction by a microconcentric nebulizer, is proposed. The sample is mixed with formic acid, kept at 90 o C for one hour and then diluted with nitric acid aqueous solution to a 50% v/v formic acid and 1% v/v nitric acid final concentrations. The final sample solution flow rate for introduction into the plasma was 30 μL min -1 . The optimized and adopted nebulizer gas flow rate was 0.7 L min -1 and RF power was 800 W. These conditions are very different than those normally used when a conventional nebulizer is employed. Rodhium was used as internal standard. External calibration against aqueous standard solutions, without formic acid, could be used for quantification, except for As, Se and Zn. However, external calibration with 50% formic acid allows the determination of all analytes with high accuracy and it is recommended. The detection limits were between 0.0005 (Tl) and 0.22 mg kg -1 (Fe) and the precision expressed by the relative standard deviations (RSD) were between 0.2% (Sr) and 3.5% (Ga). Accuracy was validated by the analysis of four certified reference biological materials of animal tissues, comparing the results by linear regressions and by the t-test at a 95% confidence level. The recommended procedure avoids plasma instability and carbon deposit on the cones.

  9. Identification of bacteria using mass spectrometry techniques

    Czech Academy of Sciences Publication Activity Database

    Krásný, Lukáš; Hynek, R.; Hochel, I.

    2013-01-01

    Roč. 353, NOV 2013 (2013), s. 67-79 ISSN 1387-3806 R&D Projects: GA ČR GAP503/10/0664 Institutional support: RVO:61388971 Keywords : Mass spectrometry * Bacteria * Identification Subject RIV: EE - Microbiology, Virology Impact factor: 2.227, year: 2013

  10. Four decades of joy in mass spectrometry

    NARCIS (Netherlands)

    Nibbering, N.M.M.

    2006-01-01

    Tremendous developments in mass spectrometry have taken place in the last 40 years. This holds for both the science and the instrumental revolutions in this field. In chemistry the research was heavily focused on organic molecules that upon electron ionization fragmented via complex mechanistic

  11. Characterization of synthetic peptides by mass spectrometry

    DEFF Research Database (Denmark)

    Prabhala, Bala Krishna; Mirza, Osman Asghar; Højrup, Peter

    2015-01-01

    Mass spectrometry (MS) is well suited for analysis of the identity and purity of synthetic peptides. The sequence of a synthetic peptide is most often known, so the analysis is mainly used to confirm the identity and purity of the peptide. Here, simple procedures are described for MALDI......-TOF-MS and LC-MS of synthetic peptides....

  12. Nanostructure-initiator mass spectrometry biometrics

    Science.gov (United States)

    Leclerc, Marion; Bowen, Benjamin; Northen, Trent

    2015-09-08

    Several embodiments described herein are drawn to methods of identifying an analyte on a subject's skin, methods of generating a fingerprint, methods of determining a physiological change in a subject, methods of diagnosing health status of a subject, and assay systems for detecting an analyte and generating a fingerprint, by nanostructure-initiator mass spectrometry (NIMS).

  13. Characterization of microbial siderophores by mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Pluháček, Tomáš; Lemr, Karel; Ghosh, D.; Milde, D.; Novák, Jiří; Havlíček, Vladimír

    2016-01-01

    Roč. 35, č. 1 (2016), s. 35-47 ISSN 0277-7037 R&D Projects: GA MŠk(CZ) LD13038; GA ČR(CZ) GAP206/12/1150; GA MŠk(CZ) LO1509 Institutional support: RVO:61388971 Keywords : iron * siderophores * mass spectrometry Subject RIV: CE - Biochemistry Impact factor: 9.373, year: 2016

  14. Polymer and Additive Mass Spectrometry Literature Review

    Energy Technology Data Exchange (ETDEWEB)

    Shear, Trevor Allan [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-06-06

    The use of mass spectrometry in fields related to polymers has increased significantly over the past three decades and will be explored in this literature review. The importance of this technique is highlighted when exploring how polymers degrade, verifying purchased materials, and as internal requirements change. The primary focus will be on four ionization techniques and the triple quadrupole and quadrupole / time-of-flight mass spectrometers. The advantages and limitations of each will also be explored.

  15. Radiocarbon accelerator mass spectrometry: background and contamination

    International Nuclear Information System (INIS)

    Beukens, R.P.

    1993-01-01

    Since the advent of radiocarbon accelerator mass spectrometry (AMS) many studies have been conducted to understand the background from mass spectrometric processes and the origins of contamination associated with the ion source and sample preparation. By studying the individual contributions a better understanding of these processes has been obtained and it has been demonstrated that it is possible to date samples reliably up to 60 000 BP. (orig.)

  16. Optimization Of A Mass Spectrometry Process

    International Nuclear Information System (INIS)

    Lopes, Jose; Alegria, F. Correa; Redondo, Luis; Barradas, N. P.; Alves, E.; Rocha, Jorge

    2011-01-01

    In this paper we present and discuss a system developed in order to optimize the mass spectrometry process of an ion implanter. The system uses a PC to control and display the mass spectrum. The operator interacts with the I/O board, that interfaces with the computer and the ion implanter by a LabVIEW code. Experimental results are shown and the capabilities of the system are discussed.

  17. Elemental ratios for characterization of quantum-dots populations in complex mixtures by asymmetrical flow field-flow fractionation on-line coupled to fluorescence and inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Menendez-Miranda, Mario; Fernandez-Arguelles, Maria T.; Costa-Fernandez, Jose M.; Encinar, Jorge Ruiz; Sanz-Medel, Alfredo

    2014-01-01

    Highlights: • The hyphenated system allows unequivocal identification of nanoparticle populations. • AF4 separation permitted detection of unexpected nanosized species in a sample. • ICP-QQQ provides elemental ratios with adequate accuracy in every nanoparticle. • Purity and chemical composition of different quantum dot samples were assessed. - Abstract: Separation and identification of nanoparticles of different composition, with similar particle diameter, coexisting in heterogeneous suspensions of polymer-coated CdSe/ZnS quantum dots (QDs) have been thoroughly assessed by asymmetric flow field-flow fractionation (AF4) coupled on-line to fluorescence and inductively coupled plasma mass spectrometry (ICPMS) detectors. Chemical characterization of any previously on-line separated nanosized species was achieved by the measurement of the elemental molar ratios of every element involved in the synthesis of the QDs, using inorganic standards and external calibration by flow injection analysis (FIA). Such elemental molar ratios, strongly limited so far to pure single nanoparticles suspensions, have been achieved with adequate accuracy by coupling for the first time an ICP-QQQ instrument to an AF4 system. This hyphenation turned out to be instrumental to assess the chemical composition of the different populations of nanoparticles coexisting in the relatively complex mixtures, due to its capabilities to detect the hardly detectable elements involved in the synthesis. Interestingly such information, complementary to that obtained by fluorescence, was very valuable to detect and identify unexpected nanosized species, present at significant level, produced during QDs synthesis and hardly detectable by standard approaches

  18. Cytosolic distributions of highly toxic metals Cd and Tl and several essential elements in the liver of brown trout (Salmo trutta L.) analyzed by size exclusion chromatography and inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Dragun, Zrinka; Krasnići, Nesrete; Kolar, Nicol; Filipović Marijić, Vlatka; Ivanković, Dušica; Erk, Marijana

    2018-05-15

    Cytosolic distributions of nonessential metals Cd and Tl and seven essential elements among compounds of different molecular masses were studied in the liver of brown trout (Salmo trutta) from the karstic Krka River in Croatia. Analyses were done by size exclusion high performance liquid chromatography and high resolution inductively coupled plasma mass spectrometry. Common feature of Cd and Tl, as highly toxic elements, was their distribution within only two narrow peaks. The increase of cytosolic Cd concentrations was reflected in marked increase of Cd elution within low molecular mass peak (maximum at ∼15 kDa), presumably containing metallothioneins (MTs), which indicated successful Cd detoxification in brown trout liver under studied exposure conditions. Contrary, the increase of cytosolic Tl concentrations was reflected in marked increase of Tl elution within high molecular mass peak (maximum at 140 kDa), which probably indicated incomplete Tl detoxification. Common feature of the majority of studied essential elements was their distribution within more peaks, often broad and not well resolved, which is consistent with their numerous physiological functions. Among observed associations of essential metals/nonmetal to proteins, the following could be singled out: Cu and Zn association to MTs, Fe association to storage protein ferritin, and Se association to compounds of very low molecular masses (<5 kDa). The obtained results present the first step towards identification of metal-binding compounds in hepatic cytosol of brown trout, and thus a significant contribution to better understanding of metal fate in the liver of that important bioindicator species. Copyright © 2018 Elsevier Ltd. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2002-09-01

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

  20. Accelerator mass spectrometry: state of the art

    Energy Technology Data Exchange (ETDEWEB)

    Tuniz, C. [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia)

    1996-12-31

    Accelerator Mass Spectrometry (AMS) is the analytical technique of choice for the detection of long-lived radionuclides which cannot be practically analysed with decay counting or conventional mass spectrometry. The main use of AMS has been in the analysis of radiocarbon and other cosmogenic radionuclides for archaeological, geological and environmental applications. In addition, AMS has been recently applied in biomedicine to study exposure of human tissues to chemicals and biomolecules at attomole levels. There is also a world-wide effort to analyse rare nuclides of heavier masses, such as long-lived actinides, with important applications in safeguards and nuclear waste disposal. The use of AMS is limited by the expensive accelerator technology required and there are several attempts to develop smaller and cheaper AMS spectrometers. 5 refs.

  1. Accelerator mass spectrometry: state of the art

    Energy Technology Data Exchange (ETDEWEB)

    Tuniz, C [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia)

    1997-12-31

    Accelerator Mass Spectrometry (AMS) is the analytical technique of choice for the detection of long-lived radionuclides which cannot be practically analysed with decay counting or conventional mass spectrometry. The main use of AMS has been in the analysis of radiocarbon and other cosmogenic radionuclides for archaeological, geological and environmental applications. In addition, AMS has been recently applied in biomedicine to study exposure of human tissues to chemicals and biomolecules at attomole levels. There is also a world-wide effort to analyse rare nuclides of heavier masses, such as long-lived actinides, with important applications in safeguards and nuclear waste disposal. The use of AMS is limited by the expensive accelerator technology required and there are several attempts to develop smaller and cheaper AMS spectrometers. 5 refs.

  2. Space Applications of Mass Spectrometry. Chapter 31

    Science.gov (United States)

    Hoffman, John H.; Griffin, Timothy P.; Limero, Thomas; Arkin, C. Richard

    2010-01-01

    Mass spectrometers have been involved in essentially all aspects of space exploration. This chapter outlines some of these many uses. Mass spectrometers have not only helped to expand our knowledge and understanding of the world and solar system around us, they have helped to put man safely in space and expand our frontier. Mass spectrometry continues to prove to be a very reliable, robust, and flexible analytical instrument, ensuring that its use will continue to help aid our investigation of the universe and this small planet that we call home.

  3. High-accuracy mass spectrometry for fundamental studies.

    Science.gov (United States)

    Kluge, H-Jürgen

    2010-01-01

    Mass spectrometry for fundamental studies in metrology and atomic, nuclear and particle physics requires extreme sensitivity and efficiency as well as ultimate resolving power and accuracy. An overview will be given on the global status of high-accuracy mass spectrometry for fundamental physics and metrology. Three quite different examples of modern mass spectrometric experiments in physics are presented: (i) the retardation spectrometer KATRIN at the Forschungszentrum Karlsruhe, employing electrostatic filtering in combination with magnetic-adiabatic collimation-the biggest mass spectrometer for determining the smallest mass, i.e. the mass of the electron anti-neutrino, (ii) the Experimental Cooler-Storage Ring at GSI-a mass spectrometer of medium size, relative to other accelerators, for determining medium-heavy masses and (iii) the Penning trap facility, SHIPTRAP, at GSI-the smallest mass spectrometer for determining the heaviest masses, those of super-heavy elements. Finally, a short view into the future will address the GSI project HITRAP at GSI for fundamental studies with highly-charged ions.

  4. Elemental ratios for characterization of quantum-dots populations in complex mixtures by asymmetrical flow field-flow fractionation on-line coupled to fluorescence and inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Menendez-Miranda, Mario; Fernandez-Arguelles, Maria T; Costa-Fernandez, Jose M; Encinar, Jorge Ruiz; Sanz-Medel, Alfredo

    2014-08-11

    Separation and identification of nanoparticles of different composition, with similar particle diameter, coexisting in heterogeneous suspensions of polymer-coated CdSe/ZnS quantum dots (QDs) have been thoroughly assessed by asymmetric flow field-flow fractionation (AF4) coupled on-line to fluorescence and inductively coupled plasma mass spectrometry (ICPMS) detectors. Chemical characterization of any previously on-line separated nanosized species was achieved by the measurement of the elemental molar ratios of every element involved in the synthesis of the QDs, using inorganic standards and external calibration by flow injection analysis (FIA). Such elemental molar ratios, strongly limited so far to pure single nanoparticles suspensions, have been achieved with adequate accuracy by coupling for the first time an ICP-QQQ instrument to an AF4 system. This hyphenation turned out to be instrumental to assess the chemical composition of the different populations of nanoparticles coexisting in the relatively complex mixtures, due to its capabilities to detect the hardly detectable elements involved in the synthesis. Interestingly such information, complementary to that obtained by fluorescence, was very valuable to detect and identify unexpected nanosized species, present at significant level, produced during QDs synthesis and hardly detectable by standard approaches. Copyright © 2014. Published by Elsevier B.V.

  5. High-throughput simultaneous determination of plasma water deuterium and 18-oxygen enrichment using a high-temperature conversion elemental analyzer with isotope ratio mass spectrometry.

    Science.gov (United States)

    Richelle, M; Darimont, C; Piguet-Welsch, C; Fay, L B

    2004-01-01

    This paper presents a high-throughput method for the simultaneous determination of deuterium and oxygen-18 (18O) enrichment of water samples isolated from blood. This analytical method enables rapid and simple determination of these enrichments of microgram quantities of water. Water is converted into hydrogen and carbon monoxide gases by the use of a high-temperature conversion elemental analyzer (TC-EA), that are then transferred on-line into the isotope ratio mass spectrometer. Accuracy determined with the standard light Antartic precipitation (SLAP) and Greenland ice sheet precipitation (GISP) is reliable for deuterium and 18O enrichments. The range of linearity is from 0 up to 0.09 atom percent excess (APE, i.e. -78 up to 5725 delta per mil (dpm)) for deuterium enrichment and from 0 up to 0.17 APE (-11 up to 890 dpm) for 18O enrichment. Memory effects do exist but can be avoided by analyzing the biological samples in quintuplet. This method allows the determination of 1440 samples per week, i.e. 288 biological samples per week. Copyright 2004 John Wiley & Sons, Ltd.

  6. Alpha spectrometry and the secondary ion mass spectrometry of thorium

    International Nuclear Information System (INIS)

    Strisovska, J.; Kuruc, J.; Galanda, D.; Matel, L.; Aranyosiova, M.; Velic, D.

    2009-01-01

    The main objective of this master thesis was preparation of samples with thorium content on the steel discs by electrodeposition for determination of natural thorium isotope by alpha spectrometry and the secondary ion mass spectrometry and finding out their possible linear correlation between these methods. The samples with electrolytically excluded isotope of 232 Th were prepared by electrodeposition from solution Th(NO 3 ) 4 ·12 H2 O on steel discs in electrodeposition cell with use of solutions Na 2 SO 4 , NaHSO 4 , KOH and (NH 4 ) 2 (C 2 O 4 ) by electric current 0.75 A. Discs were measured by alpha spectrometer. Activity was calculated from the registered impulses for 232 Th and surface's weight. After alpha spectrometry measurements discs were analyzed by TOF-SIMS IV which is installed in the International Laser Centre in Bratislava. Intensities of isotope of 232 Th and ions of ThO + , ThOH + , ThO 2 H + , Th 2 O 4 H + , ThO 2 - , ThO 3 H - , ThH 3 O 3 - and ThN 2 O 5 H - were identified. The linear correlation is between surface's weights of Th and intensities of ions of Th + from SIMS, however the correlation coefficient has relatively low value. We found out with SIMS method that oxidized and hydride forms of thorium are significantly represented in samples with electroplated thorium. (authors)

  7. Mass Spectrometry Imaging under Ambient Conditions

    Science.gov (United States)

    Wu, Chunping; Dill, Allison L.; Eberlin, Livia S.; Cooks, R. Graham; Ifa, Demian R.

    2012-01-01

    Mass spectrometry imaging (MSI) has emerged as an important tool in the last decade and it is beginning to show potential to provide new information in many fields owing to its unique ability to acquire molecularly specific images and to provide multiplexed information, without the need for labeling or staining. In MSI, the chemical identity of molecules present on a surface is investigated as a function of spatial distribution. In addition to now standard methods involving MSI in vacuum, recently developed ambient ionization techniques allow MSI to be performed under atmospheric pressure on untreated samples outside the mass spectrometer. Here we review recent developments and applications of MSI emphasizing the ambient ionization techniques of desorption electrospray ionization (DESI), laser ablation electrospray ionization (LAESI), probe electrospray ionization (PESI), desorption atmospheric pressure photoionization (DAPPI), femtosecond laser desorption ionization (fs-LDI), laser electrospray mass spectrometry (LEMS), infrared laser ablation metastable-induced chemical ionization (IR-LAMICI), liquid microjunction surface sampling probe mass spectrometry (LMJ-SSP MS), nanospray desorption electrospray ionization (nano-DESI), and plasma sources such as the low temperature plasma (LTP) probe and laser ablation coupled to flowing atmospheric-pressure afterglow (LA-FAPA). Included are discussions of some of the features of ambient MSI including the ability to implement chemical reactions with the goal of providing high abundance ions characteristic of specific compounds of interest and the use of tandem mass spectrometry to either map the distribution of targeted molecules with high specificity or to provide additional MS information in the structural identification of compounds. We also describe the role of bioinformatics in acquiring and interpreting the chemical and spatial information obtained through MSI, especially in biological applications for tissue

  8. Mass spectrometry applied to high temperature chemistry, (2)

    International Nuclear Information System (INIS)

    Asano, Mitsuru; Kato, Eiichi; Sata, Toshiyuki.

    1980-01-01

    The application of mass spectrometry to high temperature chemistry is reviewed. As a blanket material for fusion reactors, the behavior of lithium has been investigated by using mass analysers. The enthalpies of the chemical reactions of metallic lithium were obtained. The enthalpies of isomolecular exchange reactions and the derived atomization energies of LiD, Li 2 D and Li 2 D 2 were also obtained by mass spectrometry. The thermomechanical character of lithium oxide was studied. The vaporization behaviors of LiCrO 2 and Li 5 FeO 4 were studied with a quadrupole mass analyser. The vaporization of cobalt from nickel alloy was studied. The evaporated ions were analysed with a mass analyser. The measurement of the vaporized molecules of metals and fused silicate was made by mass spectrometry. The activities of Fe-V system were determined by measuring the ion current ratio. The activities of Fe-V-Cr system were also obtained. The vapor pressure of phosphor from Fe-P alloys can be measured. The activity coefficients and interaction parameters for the dilute solutions of elements, such as Mn, Al, Cu, Cr, Co, Ni, Si, Ti, V, B, Zr, Mo, C, S, and P, dissolved in liquid iron are shown in a table. The activities of NaCl-KCl system were derived by measuring the ion current ratio and by monomer-dimer method. (Kato, T.)

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

    Science.gov (United States)

    2016-12-01

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

  10. Boundaries of mass resolution in native mass spectrometry

    NARCIS (Netherlands)

    Lössl, Philip|info:eu-repo/dai/nl/371559693; Snijder, Joost|info:eu-repo/dai/nl/338018328; Heck, Albert J R|info:eu-repo/dai/nl/105189332

    Over the last two decades, native mass spectrometry (MS) has emerged as a valuable tool to study intact proteins and noncovalent protein complexes. Studied experimental systems range from small-molecule (drug)-protein interactions, to nanomachineries such as the proteasome and ribosome, to even

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

    Science.gov (United States)

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

    2015-07-01

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

  12. Burnup determination of mass spectrometry for nuclear fuels

    International Nuclear Information System (INIS)

    Zhang Chunhua.

    1987-01-01

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

  13. [Sample preparation and bioanalysis in mass spectrometry].

    Science.gov (United States)

    Bourgogne, Emmanuel; Wagner, Michel

    2015-01-01

    The quantitative analysis of compounds of clinical interest of low molecular weight (sample preparation. Sample preparation is a crucial part of chemical/biological analysis and in a sense is considered the bottleneck of the whole analytical process. The main objectives of sample preparation are the removal of potential interferences, analyte preconcentration, and converting (if needed) the analyte into a more suitable form for detection or separation. Without chromatographic separation, endogenous compounds, co-eluted products may affect a quantitative method in mass spectrometry performance. This work focuses on three distinct parts. First, quantitative bioanalysis will be defined, different matrices and sample preparation techniques currently used in bioanalysis by mass spectrometry of/for small molecules of clinical interest in biological fluids. In a second step the goals of sample preparation will be described. Finally, in a third step, sample preparation strategies will be made either directly ("dilute and shoot") or after precipitation.

  14. Monolithic multinozzle emitters for nanoelectrospray mass spectrometry

    Science.gov (United States)

    Wang, Daojing [Daly City, CA; Yang, Peidong [Kensington, CA; Kim, Woong [Seoul, KR; Fan, Rong [Pasadena, CA

    2011-09-20

    Novel and significantly simplified procedures for fabrication of fully integrated nanoelectrospray emitters have been described. For nanofabricated monolithic multinozzle emitters (NM.sup.2 emitters), a bottom up approach using silicon nanowires on a silicon sliver is used. For microfabricated monolithic multinozzle emitters (M.sup.3 emitters), a top down approach using MEMS techniques on silicon wafers is used. The emitters have performance comparable to that of commercially-available silica capillary emitters for nanoelectrospray mass spectrometry.

  15. A mass spectrometry proteomics data management platform.

    Science.gov (United States)

    Sharma, Vagisha; Eng, Jimmy K; Maccoss, Michael J; Riffle, Michael

    2012-09-01

    Mass spectrometry-based proteomics is increasingly being used in biomedical research. These experiments typically generate a large volume of highly complex data, and the volume and complexity are only increasing with time. There exist many software pipelines for analyzing these data (each typically with its own file formats), and as technology improves, these file formats change and new formats are developed. Files produced from these myriad software programs may accumulate on hard disks or tape drives over time, with older files being rendered progressively more obsolete and unusable with each successive technical advancement and data format change. Although initiatives exist to standardize the file formats used in proteomics, they do not address the core failings of a file-based data management system: (1) files are typically poorly annotated experimentally, (2) files are "organically" distributed across laboratory file systems in an ad hoc manner, (3) files formats become obsolete, and (4) searching the data and comparing and contrasting results across separate experiments is very inefficient (if possible at all). Here we present a relational database architecture and accompanying web application dubbed Mass Spectrometry Data Platform that is designed to address the failings of the file-based mass spectrometry data management approach. The database is designed such that the output of disparate software pipelines may be imported into a core set of unified tables, with these core tables being extended to support data generated by specific pipelines. Because the data are unified, they may be queried, viewed, and compared across multiple experiments using a common web interface. Mass Spectrometry Data Platform is open source and freely available at http://code.google.com/p/msdapl/.

  16. High-sensitivity mass spectrometry with a tandem accelerator

    International Nuclear Information System (INIS)

    Henning, W.

    1984-01-01

    The characteristic features of accelerator mass spectrometry are discussed. A short overview is given of the current status of mass spectrometry with high-energy (MeV/nucleon) heavy-ion accelerators. Emphasis is placed on studies with tandem accelerators and on future mass spectrometry of heavier isotopes with the new generation of higher-voltage tandems

  17. Multielement ultratrace analysis in tungsten using secondary ion mass spectrometry

    International Nuclear Information System (INIS)

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

    1987-01-01

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

  18. Analysis of biogenic carbonates by inductively coupled plasma-mass spectrometry (ICP-MS). Flow injection on-line solid-phase preconcentration for trace element determination in fish otoliths.

    Science.gov (United States)

    Arslan, Z; Paulson, A J

    2002-04-01

    The aragonite deposits within the ear bones (otoliths) of teleost fish retain a chemical signal reflecting the life history of fish (similar to rings of trees) and the nature of fish habitats. Otoliths dissolved in acid solutions contain high concentrations of calcium and a variety of proteins. Elimination of matrix salts and organic interferences during preconcentration is essential for accurate determination of trace elements in otolith solutions by inductively coupled plasma-quadrupole mass spectrometry. An iminodiacetate-based chelating resin (Toyopearl AF-Chelate 650 M) has been used for on-line preconcentration and matrix separation for the determination of 31 transition and rare elements. Successful preconcentration of the elements was achieved at pH 5 by on-line buffering, except Mn which required pH 8.8. Sample solutions were loaded on to the column for 1 min at 3.2 mL min(-1), and then eluted directly into the mass spectrometer with 4% v/v nitric acid. This procedure enabled up to 25-fold preconcentration with successful removal of the calcium matrix. The effect of heat-assisted oxidation with concentrated nitric acid was investigated to eliminate the organic matrix. It was found that heating to dryness after dissolution and further mineralization with the acid significantly improved the retention of the transition elements. The method was validated by analysis of a certified reference material produced from saggittal otoliths of emperor snapper ( Lutjanus sebae), and then applied to the determination of trace metal concentrations in juvenile bluefin tuna ( Thunnus thynnus) from the Western Pacific Ocean.

  19. Mass spectrometry by means of tandem accelerators

    International Nuclear Information System (INIS)

    Tuniz, C.

    1985-01-01

    Mass spectrometry based on an accelerator allows to measure rare cosmogenic isotopes found in natural samples with isotopic abundances up to 10E-15. The XTU Tandem of Legnaro National Laboratories can measure mean heavy isotopes (36Cl, 41Ca, 129I) in applications interesting cosmochronology and Medicine. The TTT-3 Tandem of the Naples University has been modified in view of precision studies of C14 in Archeology, Paleantology and Geology. In this paper a review is made of principles and methodologies and of some applicationy in the framework of the National Program for mass spectrametry research with the aid of accelerators

  20. 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

    Science.gov (United States)

    Pedreira, W. R.; Sarkis, J. E. S.; da Silva Queiroz, C. A.; Rodrigues, C.; Tomiyoshi, I. A.; Abrão, A.

    2003-02-01

    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.

  1. 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)

    Pedreira, W.R.; Sarkis, J.E.S.; Silva Queiroz, C.A. da; Rodrigues, C.; Tomiyoshi, I.A.; Abrao, A.

    2003-01-01

    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

  2. Measurement of elemental speciation by liquid chromatography -- inductively coupled plasma mass spectrometry (LC-ICP-MS) with the direct injection nebulizer (DIN)

    Energy Technology Data Exchange (ETDEWEB)

    Shum, Sam [Iowa State Univ., Ames, IA (United States)

    1993-05-01

    This thesis is divided into 4 parts: elemental speciation, speciation of mercury and lead compounds by microbore column LC-ICP-MS with direct injection nebulization, spatially resolved measurements of size and velocity distributions of aerosol droplets from a direct injection nebulizer, and elemental speciation by anion exchange and size exclusion chromatography with detection by ICP-MS with direct injection nebulization.

  3. Elucidating rhizosphere processes by mass spectrometry - A review.

    Science.gov (United States)

    Rugova, Ariana; Puschenreiter, Markus; Koellensperger, Gunda; Hann, Stephan

    2017-03-01

    The presented review discusses state-of-the-art mass spectrometric methods, which have been developed and applied for investigation of chemical processes in the soil-root interface, the so-called rhizosphere. Rhizosphere soil's physical and chemical characteristics are to a great extent influenced by a complex mixture of compounds released from plant roots, i.e. root exudates, which have a high impact on nutrient and trace element dynamics in the soil-root interface as well as on microbial activities or soil physico-chemical characteristics. Chemical characterization as well as accurate quantification of the compounds present in the rhizosphere is a major prerequisite for a better understanding of rhizosphere processes and requires the development and application of advanced sampling procedures in combination with highly selective and sensitive analytical techniques. During the last years, targeted and non-targeted mass spectrometry-based methods have emerged and their combination with specific separation methods for various elements and compounds of a wide polarity range have been successfully applied in several studies. With this review we critically discuss the work that has been conducted within the last decade in the context of rhizosphere research and elemental or molecular mass spectrometry emphasizing different separation techniques as GC, LC and CE. Moreover, selected applications such as metal detoxification or nutrient acquisition will be discussed regarding the mass spectrometric techniques applied in studies of root exudates in plant-bacteria interactions. Additionally, a more recent isotope probing technique as novel mass spectrometry based application is highlighted. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Multielement determination of trace elements in seawater by inductively coupled plasma mass spectrometry after tandem preconcentration with cooperation of chelating resin adsorption and lanthanum coprecipitation

    International Nuclear Information System (INIS)

    Yabutani, Tomoki; Chiba, Koichi; Haraguchi, Hiroki

    2001-01-01

    A tandem preconcentration method, in which chelating resin adsorption and La coprecipitation were cooperatively employed for preconcentration, was developed as a pretreatment method for simultaneous multielement determination of trace elements in seawater by ICP-MS. First, the seawater sample (250 ml) was treated with a chelating resin for preconcentration of trace elements, and then trace elements with good recoveries were determined by ICP-MS. Trace elements with the chemical properties of oxoanion- and hydride-formation, which were poorly recovered in the chelating resin preconcentration, were further subjected to preconcentration by La coprecipitation. As a result, more than 30 elements could be determined in the concentration range from 9.6 μg L -1 for Mo to 0.00018 μg L -1 for Tm, when the present tandem method was applied to the analysis of open seawater standard reference material (NASS-4). Furthermore, the analytical results for open seawater reference materials were compared with those for coastal seawater reference material as well as for coastal seawater collected in the Ise Bay. It was found that the multielement data for trace elements in these seawater samples clearly showed different elemental distributions, reflecting the different marine environments. (author)

  5. Development of analytical methods for the determination of trace elements in sediment with Neutron ActivAtion method (NAA) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

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

    2005-01-01

    The analytical methods for the determination of major elements (Al, Ca, K, Fe, Mg) in sediment have been investigated with ICP-MS. The analytical results of major elements with Cool ICP-MS were much better than those with normal ICP-MS. The analytical results were compared with those of NAA. NAA were a little superior to ICP-MS for the determination of major elements in sediment, and NAA is a non-destructive analytical method. The analytical methods for the determination of minor elements (Cr, Ce, U, Co, Pb, As, Se) in sediment have been also studied with ICP-MS. The analytical results by standard calibration with ICP-MS were not accurate due to matrix interferences. Thus, internal standard method was applied, then the analytical results for minor element with ICP-MS were greatly improved. The analytical results obtained by ICP-MS were compared with those obtained by NAA. It showed that the two analytical methods have great capabilities for the determination of minor elements in sediments

  6. Mass spectrometry imaging: Towards a lipid microscope?

    Science.gov (United States)

    Touboul, David; Brunelle, Alain; Laprévote, Olivier

    2011-01-01

    Biological imaging techniques are the most efficient way to locally measure the variation of different parameters on tissue sections. These analyses are gaining increasing interest since 20 years and allow observing extremely complex biological phenomena at lower and lower time and resolution scale. Nevertheless, most of them only target very few compounds of interest, which are chosen a priori, due to their low resolution power and sensitivity. New chemical imaging technique has to be introduced in order to overcome these limitations, leading to more informative and sensitive analyses for biologists and physicians. Two major mass spectrometry methods can be efficiently used to generate the distribution of biological compounds over a tissue section. Matrix-Assisted Laser Desorption/Ionisation-Mass Spectrometry (MALDI-MS) needs the co-crystallization of the sample with a matrix before to be irradiated by a laser, whereas the analyte is directly desorbed by a primary ion bombardment for Secondary Ion Mass Spectrometry (SIMS) experiments. In both cases, energy used for desorption/ionization is locally deposited -some tens of microns for the laser and some hundreds of nanometers for the ion beam- meaning that small areas over the surface sample can be separately analyzed. Step by step analysis allows spectrum acquisitions over the tissue sections and the data are treated by modern informatics software in order to create ion density maps, i.e., the intensity plot of one specific ion versus the (x,y) position. Main advantages of SIMS and MALDI compared to other chemical imaging techniques lie in the simultaneous acquisition of a large number of biological compounds in mixture with an excellent sensitivity obtained by Time-of-Flight (ToF) mass analyzer. Moreover, data treatment is done a posteriori, due to the fact that no compound is selectively marked, and let us access to the localization of different lipid classes in only one complete acquisition. Copyright © 2010

  7. Hydrogen/deuterium exchange in mass spectrometry.

    Science.gov (United States)

    Kostyukevich, Yury; Acter, Thamina; Zherebker, Alexander; Ahmed, Arif; Kim, Sunghwan; Nikolaev, Eugene

    2018-03-30

    The isotopic exchange approach is in use since the first observation of such reactions in 1933 by Lewis. This approach allows the investigation of the pathways of chemical and biochemical reactions, determination of structure, composition, and conformation of molecules. Mass spectrometry has now become one of the most important analytical tools for the monitoring of the isotopic exchange reactions. Investigation of conformational dynamics of proteins, quantitative measurements, obtaining chemical, and structural information about individual compounds of the complex natural mixtures are mainly based on the use of isotope exchange in combination with high resolution mass spectrometry. The most important reaction is the Hydrogen/Deuterium exchange, which is mainly performed in the solution. Recently we have developed the approach allowing performing of the Hydrogen/Deuterium reaction on-line directly in the ionization source under atmospheric pressure. Such approach simplifies the sample preparation and can accelerate the exchange reaction so that certain hydrogens that are considered as non-labile will also participate in the exchange. The use of in-ionization source H/D exchange in modern mass spectrometry for structural elucidation of molecules serves as the basic theme in this review. We will focus on the mechanisms of the isotopic exchange reactions and on the application of in-ESI, in-APCI, and in-APPI source Hydrogen/Deuterium exchange for the investigation of petroleum, natural organic matter, oligosaccharides, and proteins including protein-protein complexes. The simple scenario for adaptation of H/D exchange reactions into mass spectrometric method is also highlighted along with a couple of examples collected from previous studies. © 2018 Wiley Periodicals, Inc.

  8. Computational mass spectrometry for small molecules

    Science.gov (United States)

    2013-01-01

    The identification of small molecules from mass spectrometry (MS) data remains a major challenge in the interpretation of MS data. This review covers the computational aspects of identifying small molecules, from the identification of a compound searching a reference spectral library, to the structural elucidation of unknowns. In detail, we describe the basic principles and pitfalls of searching mass spectral reference libraries. Determining the molecular formula of the compound can serve as a basis for subsequent structural elucidation; consequently, we cover different methods for molecular formula identification, focussing on isotope pattern analysis. We then discuss automated methods to deal with mass spectra of compounds that are not present in spectral libraries, and provide an insight into de novo analysis of fragmentation spectra using fragmentation trees. In addition, this review shortly covers the reconstruction of metabolic networks using MS data. Finally, we list available software for different steps of the analysis pipeline. PMID:23453222

  9. Bk and Cf chromatographic separation and 249Bk/248Cm and 249Cf/248Cm elemental ratios determination by inductively coupled plasma quadrupole mass spectrometry

    International Nuclear Information System (INIS)

    Gourgiotis, A.; Isnard, H.; Nonell, A.; Aubert, M.; Stadelmann, G.; Dupont, E.; AlMahamid, I.; Tiang, G.; Rao, L.; Lukens, W.; Cassette, P.; Panebianco, S.; Letourneau, A.; Chartier, F.

    2013-01-01

    The French Atomic Energy Commission has carried out several experiments for the study of minor-actinide transmutation processes in high intensity thermal neutron flux. In this context a Cm sample enriched in 248 Cm (97%) was irradiated in a thermal neutron flux at the High Flux Reactor (HFR) of the Laue-Langevin Institute (ILL). The precise and accurate determination of Cf isotope ratios and of 249 Bk/ 248 Cm and 249 Cf/ 248 Cm elemental ratios in the 248 Cm irradiated sample is crucial for the calculation of actinide neutron capture cross-sections.This work describes an analytical procedure for the separation and the isotope ratio measurement of Bk and Cf in the irradiated sample.The Bk and Cf separation is based on a lanthanides separation protocol previously developed by the laboratory. Well-defined retention times for Bk and Cf were obtained by coupling the Ionic Chromatography (IC) with an ICP-QMS. All conditions of element separation by IC and the different steps of the analytical protocol in order to obtain the isotopic and elemental ratios are presented. Relative uncertainties of Cf isotopic ratios range from 0.3% to 0.5% and the uncertainty of the 249 Bk/ 248 Cm and 249 Cf/ 248 Cm elemental ratios are respectively 6.1% and 3.2%.This level of uncertainty for both isotopic and elemental ratios is in perfect agreement with the requirement for transmutation studies. (authors)

  10. Multi-elemental characterization of tunnel and road dusts in Houston, Texas using dynamic reaction cell-quadrupole-inductively coupled plasma–mass spectrometry: Evidence for the release of platinum group and anthropogenic metals from motor vehicles

    International Nuclear Information System (INIS)

    Spada, Nicholas; Bozlaker, Ayse; Chellam, Shankararaman

    2012-01-01

    Highlights: ► Analytical method for PGEs, main group, transition and rare earth metals developed. ► Comprehensive characterization of road and tunnel dust samples was accomplished. ► PGEs in dusts arise from autocatalyst attrition. ► Mobile sources also contributed to Cu, Zn, Ga, As, Mo, Cd, Sn, Sb, Ba, W and Pb. ► All other elements, including rare earths arose from crustal sources. - Abstract: Platinum group elements (PGEs) including Rh, Pd, and Pt are important tracers for vehicular emissions, though their measurement is often challenging and difficult to replicate in environmental campaigns. These challenges arise from sample preparation steps required for PGE quantitation, which often cause severe isobaric interferences and spectral overlaps from polyatomic species of other anthropogenically emitted metals. Consequently, most previous road dust studies have either only quantified PGEs or included a small number of anthropogenic elements. Therefore a novel analytical method was developed to simultaneously measure PGEs, lanthanoids, transition and main group elements to comprehensively characterize the elemental composition of urban road and tunnel dusts. Dust samples collected from the vicinity of high-traffic roadways and a busy underwater tunnel restricted to single-axle (predominantly gasoline-driven) vehicles in Houston, TX were analyzed for 45 metals with the newly developed method using dynamic reaction cell-quadrupole-inductively coupled plasma–mass spectrometry (DRC-q-ICP–MS). Average Rh, Pd and Pt concentrations were 152 ± 52, 770 ± 208 and 529 ± 130 ng g −1 respectively in tunnel dusts while they varied between 6 and 8 ng g −1 , 10 and 88 ng g −1 and 35 and 131 ng g −1 in surface road dusts. Elemental ratios and enrichment factors demonstrated that PGEs in dusts originated from autocatalyst attrition/abrasion. Strong evidence is also presented for mobile source emissions of Cu, Zn, Ga, As, Mo, Cd, Sn, Sb, Ba, W and Pb. However

  11. Silver nanostructures in laser desorption/ionization mass spectrometry and mass spectrometry imaging.

    Science.gov (United States)

    Sekuła, Justyna; Nizioł, Joanna; Rode, Wojciech; Ruman, Tomasz

    2015-09-21

    Silver nanoparticles have been successfully applied as a matrix replacement for the laser desorption/ionization time-of-flight mass spectrometry (LDI-ToF-MS). Nanoparticles, producing spectra with highly reduced chemical background in the low m/z region, are perfectly suited for low-molecular weight compound analysis and imaging. Silver nanoparticles (AgNPs) can efficiently absorb ultraviolet laser radiation, transfer energy to the analyte and promote analyte desorption, but also constitute a source of silver ions suitable for analyte cationisation. This review provides an overview of the literature on silver nanomaterials as non-conventional desorption and ionization promoters in LDI-MS and mass spectrometry imaging.

  12. Solid phase extraction for analysis of biogenic carbonates by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS): an investigation of rare earth element signatures in otolith microchemistry

    International Nuclear Information System (INIS)

    Arslan, Zikri; Paulson, Anthony J.

    2003-01-01

    Uptake of trace elements into fish otoliths is governed by several factors such as life histories and environment in addition to stock and species differences. In an attempt to elucidate the elemental signatures of rare earth elements (REEs) in otoliths, a solid phase extraction (SPE) protocol was used in combination with electrothermal vaporization (ETV) as a sample introduction procedure for the determinations by inductively coupled plasma quadrupole mass spectrometry (ICP-MS). Effects of various parameters, such as carrier gas flow rate, atomization temperature and chemical modification, were examined for optimization of the conditions by ETV-ICP-MS. Atomization was achieved at 2800 deg. C. Lower temperatures (i.e. 2600 deg. C) resulted in severe memory problems due to incomplete atomization. Palladium was used as a chemical modifier. It was found that an increase in Pd concentration up to 0.5 μg in the injection volume (70 μl) led up to four-fold enhancement in the integrated signals. This phenomenon is attributed to the carrier effect of Pd rather than the stabilization since no significant losses were observed for high temperature drying around 700 deg. C even in the absence of Pd. Preconcentration was performed on-line at pH 5 by using a mini-column of Toyopearl AF-Chelate 650M chelating resin, which also eliminated the calcium matrix of otolith solutions. After preconcentration of 6.4 ml of solution, the concentrate was collected in 0.65 ml of 0.5% (v/v) HNO 3 in autosampler cups, and then analyzed by ETV-ICP-MS. The method was validated with the analysis of a fish otolith certified reference material (CRM) of emperor snapper, and then applied to samples. Results obtained from otoliths of fish captured in the same habitat indicated that otolith rare earth element concentrations are more dependent on environmental conditions of the habitat than on species differences

  13. Determination of rare earth, major and trace elements in authigenic fraction of Andaman Sea (Northeastern Indian Ocean) sediments by inductively coupled plasma-mass spectrometry

    Digital Repository Service at National Institute of Oceanography (India)

    Alagarsamy, R.; You, C.-F.; Nath, B.N.; SijinKumar, A.V.

    Downcore variation of rare earth elements (REEs) in the authigenic Fe-Mn oxides of a sediment core (covering a record of last approx. 40 kyr) from the Andaman Sea, a part of the Indian Ocean shows distinctive positive Ce and Eu anomalies...

  14. Analysis of posttranslational modifications of proteins by tandem mass spectrometry

    DEFF Research Database (Denmark)

    Larsen, Martin Røssel; Trelle, Morten B; Thingholm, Tine E

    2006-01-01

    -temporal distribution in cells and tissues. Most PTMs can be detected by protein and peptide analysis by mass spectrometry (MS), either as a mass increment or a mass deficit relative to the nascent unmodified protein. Tandem mass spectrometry (MS/MS) provides a series of analytical features that are highly useful...

  15. Mass spectrometry investigation of magnetron sputtering discharges

    Czech Academy of Sciences Publication Activity Database

    Pokorný, Petr; Musil, Jindřich; Lančok, Ján; Fitl, Přemysl; Novotný, Michal; Bulíř, Jiří; Vlček, Jan

    2017-01-01

    Roč. 143, č. 6 (2017), s. 438-443 ISSN 0042-207X R&D Projects: GA MŠk LO1409; GA MŠk LM2015088; GA TA ČR(CZ) TA03010490; GA ČR GA17-13427S Institutional support: RVO:68378271 Keywords : mass spectrometry * atoms * radicals and ions * RF discharge * contamination * metallic films Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 1.530, year: 2016

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

    Science.gov (United States)

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

    2016-02-12

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

  17. Surface ionization mass spectrometry of opiates

    International Nuclear Information System (INIS)

    Usmanov, D.T.

    2009-07-01

    Key words: surface ionization, adsorption, heterogeneous reactions, surface ionization mass spectrometry, thermodesorption surface ionization spectroscopy, thermoemitter, opiates, extracts of biosamples. Subjects of study. The mass - spectrometric study of thermal - ion emission: surface ionization of opiates by on the surface of oxidized refractory metals. Purpose of work is to establish the regularities of surface ionization (SI) of multi-atomic molecule opiates and their mixtures develop the scientific base of SI methods for high sensitive and selective detection and analysis of these substances in the different objects, including biosamples. Methods of study: surface ionization mass spectrometry, thermodesorption surface ionization spectroscopy. The results obtained and their novelty. For the first time, SI of molecule opiates on the oxidized tungsten surface has been studied and their SI mass-spectra and temperature dependences of ion currents have been obtained, the characteristic heterogeneous reactions of an adsorbed molecules and the channels of monomolecular decays vibrationally-excited ions on their way in mass-spectrometry have been revealed, sublimation energy has been defined, the activation energy of E act , of these decays has been estimated for given period of time. Additivity of the SI mass-spectra of opiate mixtures of has been established under conditions of joint opiate adsorption. High selectivity of SI allows the extracts of biosamples to be analyzed without their preliminary chromatographic separation. The opiates are ionized by SI with high efficiency (from 34 C/mol to 112 C/mol), which provides high sensitivity of opiate detection by SI/MS and APTDSIS methods from - 10 -11 g in the samples under analysis. Practical value. The results of these studies create the scientific base for novel SI methods of high sensitive detection and analysis of the trace amounts of opiates in complicated mixtures, including biosamples without their preliminary

  18. Boundaries of mass resolution in native mass spectrometry.

    Science.gov (United States)

    Lössl, Philip; Snijder, Joost; Heck, Albert J R

    2014-06-01

    Over the last two decades, native mass spectrometry (MS) has emerged as a valuable tool to study intact proteins and noncovalent protein complexes. Studied experimental systems range from small-molecule (drug)-protein interactions, to nanomachineries such as the proteasome and ribosome, to even virus assembly. In native MS, ions attain high m/z values, requiring special mass analyzers for their detection. Depending on the particular mass analyzer used, instrumental mass resolution does often decrease at higher m/z but can still be above a couple of thousand at m/z 5000. However, the mass resolving power obtained on charge states of protein complexes in this m/z region is experimentally found to remain well below the inherent instrument resolution of the mass analyzers employed. Here, we inquire into reasons for this discrepancy and ask how native MS would benefit from higher instrumental mass resolution. To answer this question, we discuss advantages and shortcomings of mass analyzers used to study intact biomolecules and biomolecular complexes in their native state, and we review which other factors determine mass resolving power in native MS analyses. Recent examples from the literature are given to illustrate the current status and limitations.

  19. High-precision analysis on annual variations of heavy metals, lead isotopes and rare earth elements in mangrove tree rings by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Yu Kefu; Kamber, Balz S.; Lawrence, Michael G.; Greig, Alan; Zhao Jianxin

    2007-01-01

    Annual variations from 1982 to 1999 of a wide range of trace elements and reconnaissance Pb isotopes ( 207 Pb/ 206 Pb and 208 Pb/ 206 Pb) were analyzed by solution ICP-MS on digested ash from mangrove Rhizophora apiculata, obtained from Leizhou Peninsula, along northern coast of South China Sea. The concentrations of the majority of elements show a weak declining trend with growth from 1982 to 1999, punctuated by several high concentration spikes. The declining trends are positively correlated with ring width and negatively correlated with inferred water-use efficiency, suggesting a physiological control over metal-uptake in this species. The episodic metal concentration-peaks cannot be interpreted with lateral movement or growth activities and appear to be related to environmental pollution events. Pb isotope ratios for most samples plot along the 'Chinese Pb line' and clearly document the importance of gasoline Pb as a source of contaminant. Shale-normalised REE + Y patterns are relatively flat and consistent across the growth period, with all patterns showing a positive Ce anomaly and elevated Y/Ho ratio. The positive Ce anomaly is observed regardless of the choice of normaliser, in contrast to previously reported REE patterns for terrestrial and marine plants. This pilot study of trace element, REE + Y and Pb isotope distribution in mangrove tree rings indicates the potential use of mangroves as monitors of historical environmental change

  20. Simultaneous determination of major to ultratrace elements in geological samples by fusion-dissolution and inductively coupled plasma mass spectrometry techniques

    Energy Technology Data Exchange (ETDEWEB)

    Madinabeitia, S. Garcia de [Servicio de Geocronologia y Geoquimica Isotopica, Facultad de Ciencia y Tecnologia, Universidad del Pais Vasco/EHU, Sarriena s/n, 48940 Leioa (Spain); Lorda, M.E. Sanchez [Servicio de Geocronologia y Geoquimica Isotopica, Facultad de Ciencia y Tecnologia, Universidad del Pais Vasco/EHU, Sarriena s/n, 48940 Leioa (Spain); Departamento de Mineralogia-Petrologia, Facultad de Ciencia y Tecnologia, Universidad del Pais Vasco/EHU, Sarriena s/n, 48940 Leioa (Spain); Ibarguchi, J.I. Gil [Servicio de Geocronologia y Geoquimica Isotopica, Facultad de Ciencia y Tecnologia, Universidad del Pais Vasco/EHU, Sarriena s/n, 48940 Leioa (Spain)], E-mail: josei.gil@ehu.es

    2008-09-12

    A method has been developed for the simultaneous quantification of major to ultratrace elements in geological samples using quadrupole ICP-MS techniques. The sample preparation involves fusion with LiBO{sub 2} and dilution in HNO{sub 3}-HF which allows complete decomposition of refractory minerals and quantification of the elements of interest. The effects of high Total Dissolved Solids (TDS) and Li in the solution are minimized using a matrix-tolerant interface and conditioning the instrument with LiBO{sub 2} solution. The signal drift is moreover controlled using conventional internal standards and specific Drift Correction Standards (DCS). A key issue of the technique is the external calibration using selected Certified Reference Materials (CRM). Depending on the sample type and analytes of interest three optimized programmable modes are used sequentially: Standard, Collision Cell (CCT) and Kinetic Energy Discrimination (KED) mode. The method allows to quantify more than 40 elements in concentrations from tens-of-percent to <0.1 ppm levels during a single experiment. The method has been validated through the analysis of different CRMs with recovery factors of ca. 100% and typical 2{sigma} errors of <10%.

  1. Simultaneous determination of major to ultratrace elements in geological samples by fusion-dissolution and inductively coupled plasma mass spectrometry techniques

    International Nuclear Information System (INIS)

    Madinabeitia, S. Garcia de; Lorda, M.E. Sanchez; Ibarguchi, J.I. Gil

    2008-01-01

    A method has been developed for the simultaneous quantification of major to ultratrace elements in geological samples using quadrupole ICP-MS techniques. The sample preparation involves fusion with LiBO 2 and dilution in HNO 3 -HF which allows complete decomposition of refractory minerals and quantification of the elements of interest. The effects of high Total Dissolved Solids (TDS) and Li in the solution are minimized using a matrix-tolerant interface and conditioning the instrument with LiBO 2 solution. The signal drift is moreover controlled using conventional internal standards and specific Drift Correction Standards (DCS). A key issue of the technique is the external calibration using selected Certified Reference Materials (CRM). Depending on the sample type and analytes of interest three optimized programmable modes are used sequentially: Standard, Collision Cell (CCT) and Kinetic Energy Discrimination (KED) mode. The method allows to quantify more than 40 elements in concentrations from tens-of-percent to <0.1 ppm levels during a single experiment. The method has been validated through the analysis of different CRMs with recovery factors of ca. 100% and typical 2σ errors of <10%

  2. Study of the interactions between the transuranic elements and some environmental ligands by the hyphenated technique capillary electrophoresis: inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Topin, S.

    2009-09-01

    In this work, the capabilities of the hyphenated Capillary Electrophoresis-ICP-MS technique are used to improve the knowledge on the transuranic element speciation in the environment (nuclear waste management) and in the framework of spent fuel reprocessing. Essential thermodynamical data have been determined for the first time for the interactions of the plutonium at the (5+) oxidation state (main soluble species of Pu of the surface water) in inorganic media (chloride, nitrate, sulfate, carbonate). This study enables to correct the existing model, based on the thermodynamical data of the neptunium at the (5+) oxidation state (analogue of the pentavalent plutonium). Furthermore, the hyphenated CE-ICP-MS technique has also been applied to study the interactions between DTPA, widely used in the nuclear industry, and the elements at the (3+) oxidation state (Pu, Am, Cm, Cf) and at the (4+) oxidation state (Pu, Np, Th). The results show for the first time the formation of mixed An(IV)/DTPA/OH complexes likely to play a key role on the actinide behavior in the field of the waste management. The study on the trivalent elements confirms the selectivity of DTPA versus the actinide in the framework of the actinide/lanthanide separation but proves that the covalency, responsible of the selectivity, are less important than the ionicity in the binding. (author)

  3. Radiocarbon positive-ion mass spectrometry

    International Nuclear Information System (INIS)

    Freeman, Stewart P.H.T.; Shanks, Richard P.; Donzel, Xavier; Gaubert, Gabriel

    2015-01-01

    Proof-of-principle of a new mass spectrometric technique for radiocarbon measurement is demonstrated. Interfering nitrogen and hydrocarbon molecules are largely eliminated in a charge-exchange cell operating on non-metallic gas. The positive-to-negative ion conversion is the reverse of that conventionally used in accelerator mass spectrometry (AMS) and is compatible with plasma ion sources that may be significantly more efficient and capable of greater output than are AMS sputter ion sources. The Nanogan electron cyclotron resonance (ECR) ion source employed exhibited no sample memory and the >50 kyrs age range of AMS was reproduced. A bespoke prototype new instrument is now required to optimise the plasma and cell physics and to realise hypothetical performance gains over AMS.

  4. Radiocarbon positive-ion mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Freeman, Stewart P.H.T.; Shanks, Richard P. [Scottish Universities Environmental Research Centre (SUERC), Scottish Enterprise Technology Park, East Kilbride G75 0QF (United Kingdom); Donzel, Xavier; Gaubert, Gabriel [Pantechnik S.A., 13 Rue de la Résistance, 14400 Bayeux (France)

    2015-10-15

    Proof-of-principle of a new mass spectrometric technique for radiocarbon measurement is demonstrated. Interfering nitrogen and hydrocarbon molecules are largely eliminated in a charge-exchange cell operating on non-metallic gas. The positive-to-negative ion conversion is the reverse of that conventionally used in accelerator mass spectrometry (AMS) and is compatible with plasma ion sources that may be significantly more efficient and capable of greater output than are AMS sputter ion sources. The Nanogan electron cyclotron resonance (ECR) ion source employed exhibited no sample memory and the >50 kyrs age range of AMS was reproduced. A bespoke prototype new instrument is now required to optimise the plasma and cell physics and to realise hypothetical performance gains over AMS.

  5. Mass Spectrometry on Future Mars Landers

    Science.gov (United States)

    Brinckerhoff, W. B.; Mahaffy, P. R.

    2011-01-01

    Mass spectrometry investigations on the 2011 Mars Science Laboratory (MSL) and the 2018 ExoMars missions will address core science objectives related to the potential habitability of their landing site environments and more generally the near-surface organic inventory of Mars. The analysis of complex solid samples by mass spectrometry is a well-known approach that can provide a broad and sensitive survey of organic and inorganic compounds as well as supportive data for mineralogical analysis. The science value of such compositional information is maximized when one appreciates the particular opportunities and limitations of in situ analysis with resource-constrained instrumentation in the context of a complete science payload and applied to materials found in a particular environment. The Sample Analysis at Mars (SAM) investigation on MSL and the Mars Organic Molecule Analyzer (MOMA) investigation on ExoMars will thus benefit from and inform broad-based analog field site work linked to the Mars environments where such analysis will occur.

  6. Lipid imaging by mass spectrometry - a review.

    Science.gov (United States)

    Gode, David; Volmer, Dietrich A

    2013-03-07

    Mass spectrometry imaging (MSI) has proven to be extremely useful for applications such as the spatial analysis of peptides and proteins in biological tissue, the performance assessment of drugs in vivo or the measurement of protein or metabolite expression as tissue classifiers or biomarkers from disease versus control tissue comparisons. The most popular MSI technique is MALDI mass spectrometry. First invented by Richard Caprioli in the mid-1990s, it is the highest performing MSI technique in terms of spatial resolution, sensitivity for intact biomolecules and application range today. The unique ability to identify and spatially resolve numerous compounds simultaneously, based on m/z values has inter alia been applied to untargeted and targeted chemical mapping of biological compartments, revealing changes of physiological states, disease pathologies and metabolic faith and distribution of xenobiotics. Many MSI applications focus on lipid species because of the lipids' diverse roles as structural components of cell membranes, their function in the surfactant cycle, and their involvement as second messengers in signalling cascades of tissues and cells. This article gives a comprehensive overview of lipid imaging techniques and applications using established MALDI and SIMS methods but also other promising MSI techniques such as DESI.

  7. Impact of automation on mass spectrometry.

    Science.gov (United States)

    Zhang, Yan Victoria; Rockwood, Alan

    2015-10-23

    Mass spectrometry coupled to liquid chromatography (LC-MS and LC-MS/MS) is an analytical technique that has rapidly grown in popularity in clinical practice. In contrast to traditional technology, mass spectrometry is superior in many respects including resolution, specificity, multiplex capability and has the ability to measure analytes in various matrices. Despite these advantages, LC-MS/MS remains high cost, labor intensive and has limited throughput. This specialized technology requires highly trained personnel and therefore has largely been limited to large institutions, academic organizations and reference laboratories. Advances in automation will be paramount to break through this bottleneck and increase its appeal for routine use. This article reviews these challenges, shares perspectives on essential features for LC-MS/MS total automation and proposes a step-wise and incremental approach to achieve total automation through reducing human intervention, increasing throughput and eventually integrating the LC-MS/MS system into the automated clinical laboratory operations. Copyright © 2015 Elsevier B.V. All rights reserved.

  8. [Mass spectrometry in the clinical microbiology laboratory].

    Science.gov (United States)

    Jordana-Lluch, Elena; Martró Català, Elisa; Ausina Ruiz, Vicente

    2012-12-01

    Infectious diseases are still a cause of high mortality and morbidity rates. Current microbiological diagnostic methods are based on culture and phenotypic identification of isolated microorganisms, which can be obtained in about 24-48 h. Given that the microbiological identification is of major importance for patient management, new diagnostic methods are needed in order to detect and identify microorganisms in a timely and accurate manner. Over the last few years, several molecular techniques based on the amplification of microbial nucleic acids have been developed with the aim of reducing the time needed for the identification of the microorganisms involved in different infectious processes. On the other hand, mass spectrometry has emerged as a rapid and consistent alternative to conventional methods for microorganism identification. This review describes the most widely used mass spectrometry technologies -matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) and electrospray ionization time-of-flight (ESI-TOF)-, both for protein and nucleic acid analysis, as well as the commercial platforms available. Related publications of most interest in clinical microbiology are also reviewed. Copyright © 2011 Elsevier España, S.L. All rights reserved.

  9. Metrological system for y-ray spectrometry measurement of the specific activity and mass fraction of natural radioactive elements in soil and rock samples

    International Nuclear Information System (INIS)

    Khaikovich, I.M.; Fominykh, V.I.; Kirisyuk, E.M.; Belyachkov, Y.A.

    1994-01-01

    In the last few years a great deal of attention has been devoted to the study of the radiation conditions, which in some regions change markedly as a result of intense human activity. One reason for radioactive contamination of an area is dissemination during extraction and processing of radioactive ores or other minerals of natural radioactive elements with a high content of potassium, uranium (radium), and thorium. Estimation of the level of radioactive contamination is one of the main problems of ecological monitoring, and the quality of the measurements sometimes plays a deciding role in the fate of the object being investigated. This also pertains to, in particular, estimation of radioactive contamination of minerals employed for building homes and factories and other industrial structures. In order to draw unequivocal and well-founded conclusions from measurements of the content of natural radioactive elements in soil and rock samples, collected at the object being investigated, a great deal of attention must be devoted during the organization of the measurements to the metrological system

  10. Validation of a dilute and shoot method for quantification of 12 elements by inductively coupled plasma tandem mass spectrometry in human milk and in cow milk preparations.

    Science.gov (United States)

    Dubascoux, Stéphane; Andrey, Daniel; Vigo, Mario; Kastenmayer, Peter; Poitevin, Eric

    2018-09-01

    Nutritional information about human milk is essential as early human growth and development have been closely linked to the status and requirements of several macro- and micro-elements. However, methods addressing whole mineral profiling in human milk have been scarce due in part to their technical complexities to accurately and simultaneously measure the concentration of micro- and macro-trace elements in low volume of human milk. In the present study, a single laboratory validation has been performed using a "dilute and shoot" approach for the quantification of sodium (Na), magnesium (Mg), phosphorus (P), potassium (K), calcium (Ca), manganese (Mn), iron (Fe), copper (Cu), zinc (Zn), selenium (Se), molybdenum (Mo) and iodine (I), in both human milk and milk preparations. Performances in terms of limits of detection and quantification, of repeatability, reproducibility and trueness have been assessed and verified using various reference or certified materials. For certified human milk sample (NIST 1953), recoveries obtained for reference or spiked values are ranged from 93% to 108% (except for Mn at 151%). This robust method using new technology ICP-MS/MS without high pressure digestion is adapted to both routinely and rapidly analyze human milk micro-sample (i.e. less than 250 μL) in the frame of clinical trials but also to be extended to the mineral profiling of milk preparations like infant formula and adult nutritionals. Copyright © 2018 Elsevier GmbH. All rights reserved.

  11. Elemental analysis of soils using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and laser-induced breakdown spectroscopy (LIBS) with multivariate discrimination: tape mounting as an alternative to pellets for small forensic transfer specimens.

    Science.gov (United States)

    Jantzi, Sarah C; Almirall, José R

    2014-01-01

    Elemental analysis of soil is a useful application of both laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and laser-induced breakdown spectroscopy (LIBS) in geological, agricultural, environmental, archeological, planetary, and forensic sciences. In forensic science, the question to be answered is often whether soil specimens found on objects (e.g., shoes, tires, or tools) originated from the crime scene or other location of interest. Elemental analysis of the soil from the object and the locations of interest results in a characteristic elemental profile of each specimen, consisting of the amount of each element present. Because multiple elements are measured, multivariate statistics can be used to compare the elemental profiles in order to determine whether the specimen from the object is similar to one of the locations of interest. Previous work involved milling and pressing 0.5 g of soil into pellets before analysis using LA-ICP-MS and LIBS. However, forensic examiners prefer techniques that require smaller samples, are less time consuming, and are less destructive, allowing for future analysis by other techniques. An alternative sample introduction method was developed to meet these needs while still providing quantitative results suitable for multivariate comparisons. The tape-mounting method involved deposition of a thin layer of soil onto double-sided adhesive tape. A comparison of tape-mounting and pellet method performance is reported for both LA-ICP-MS and LIBS. Calibration standards and reference materials, prepared using the tape method, were analyzed by LA-ICP-MS and LIBS. As with the pellet method, linear calibration curves were achieved with the tape method, as well as good precision and low bias. Soil specimens from Miami-Dade County were prepared by both the pellet and tape methods and analyzed by LA-ICP-MS and LIBS. Principal components analysis and linear discriminant analysis were applied to the multivariate data

  12. Analysis of soils by glow discharge mass spectrometry

    International Nuclear Information System (INIS)

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

    1993-01-01

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

  13. Electrospray mass spectrometry for actinides and lanthanide speciation

    International Nuclear Information System (INIS)

    Moulin, C.; Amekraz, B.; Colette, S.; Doizi, D.; Jacopin, C.; Lamouroux, C.; Plancque, G.

    2006-01-01

    Electrospray mass spectrometry (ES-MS) is a new speciation technique that has the great interest to be able to probe the element, the ligand and the complex in order to reach the speciation. This paper will focus on the use of ES-MS for the speciation of actinides/lanthanides on several systems of interest in various fields such as the interaction between DTPA (decorporant) and europium, HEBP and uranium, BTP (new extracting agent) and lanthanides with comparison with known chemistry as well as whenever possible with other speciation techniques

  14. Accurate isotope ratio mass spectrometry. Some problems and possibilities

    International Nuclear Information System (INIS)

    Bievre, P. de

    1978-01-01

    The review includes reference to 190 papers, mainly published during the last 10 years. It covers the following: important factors in accurate isotope ratio measurements (precision and accuracy of isotope ratio measurements -exemplified by determinations of 235 U/ 238 U and of other elements including 239 Pu/ 240 Pu; isotope fractionation -exemplified by curves for Rb, U); applications (atomic weights); the Oklo natural nuclear reactor (discovered by UF 6 mass spectrometry at Pierrelatte); nuclear and other constants; isotope ratio measurements in nuclear geology and isotope cosmology - accurate age determination; isotope ratio measurements on very small samples - archaeometry; isotope dilution; miscellaneous applications; and future prospects. (U.K.)

  15. Uncertainty of relative sensitivity factors in glow discharge mass spectrometry

    Science.gov (United States)

    Meija, Juris; Methven, Brad; Sturgeon, Ralph E.

    2017-10-01

    The concept of the relative sensitivity factors required for the correction of the measured ion beam ratios in pin-cell glow discharge mass spectrometry is examined in detail. We propose a data-driven model for predicting the relative response factors, which relies on a non-linear least squares adjustment and analyte/matrix interchangeability phenomena. The model provides a self-consistent set of response factors for any analyte/matrix combination of any element that appears as either an analyte or matrix in at least one known response factor.

  16. 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)

    Guillong, Marcel; Kuhn, Hans-Rudolf; Guenther, Detlef

    2003-01-01

    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

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

    Science.gov (United States)

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

    1996-06-01

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

  18. Ambient ionization mass spectrometry: A tutorial

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Min-Zong; Cheng, Sy-Chi; Cho, Yi-Tzu [Department of Chemistry, National Sun Yat-Sen University, Kaohsiung, Taiwan (China); Shiea, Jentaie, E-mail: jetea@fac.nsysu.edu.tw [Department of Chemistry, National Sun Yat-Sen University, Kaohsiung, Taiwan (China); Cancer Center, Kaohsiung Medical University, Kaohsiung, Taiwan (China)

    2011-09-19

    Highlights: {yields} Ambient ionization technique allows the direct analysis of sample surfaces with little or no sample pretreatment. {yields} We sort ambient ionization techniques into three main analytical strategies, direct ionization, direct desorption/ionization, and two-step ionization. {yields} The underlying principles of operation, ionization processes, detecting mass ranges, sensitivity, and representative applications of these techniques are described and compared. - Abstract: Ambient ionization is a set of mass spectrometric ionization techniques performed under ambient conditions that allows the direct analysis of sample surfaces with little or no sample pretreatment. Using combinations of different types of sample introduction systems and ionization methods, several novel techniques have been developed over the last few years with many applications (e.g., food safety screening; detection of pharmaceuticals and drug abuse; monitoring of environmental pollutants; detection of explosives for antiterrorism and forensics; characterization of biological compounds for proteomics and metabolomics; molecular imaging analysis; and monitoring chemical and biochemical reactions). Electrospray ionization and atmospheric pressure chemical ionization are the two main ionization principles most commonly used in ambient ionization mass spectrometry. This tutorial paper provides a review of the publications related to ambient ionization techniques. We describe and compare the underlying principles of operation, ionization processes, detecting mass ranges, sensitivity, and representative applications of these techniques.

  19. Ambient ionization mass spectrometry: A tutorial

    International Nuclear Information System (INIS)

    Huang, Min-Zong; Cheng, Sy-Chi; Cho, Yi-Tzu; Shiea, Jentaie

    2011-01-01

    Highlights: → Ambient ionization technique allows the direct analysis of sample surfaces with little or no sample pretreatment. → We sort ambient ionization techniques into three main analytical strategies, direct ionization, direct desorption/ionization, and two-step ionization. → The underlying principles of operation, ionization processes, detecting mass ranges, sensitivity, and representative applications of these techniques are described and compared. - Abstract: Ambient ionization is a set of mass spectrometric ionization techniques performed under ambient conditions that allows the direct analysis of sample surfaces with little or no sample pretreatment. Using combinations of different types of sample introduction systems and ionization methods, several novel techniques have been developed over the last few years with many applications (e.g., food safety screening; detection of pharmaceuticals and drug abuse; monitoring of environmental pollutants; detection of explosives for antiterrorism and forensics; characterization of biological compounds for proteomics and metabolomics; molecular imaging analysis; and monitoring chemical and biochemical reactions). Electrospray ionization and atmospheric pressure chemical ionization are the two main ionization principles most commonly used in ambient ionization mass spectrometry. This tutorial paper provides a review of the publications related to ambient ionization techniques. We describe and compare the underlying principles of operation, ionization processes, detecting mass ranges, sensitivity, and representative applications of these techniques.

  20. Mass Spectrometry for Large Undergraduate Laboratory Sections

    Science.gov (United States)

    Illies, A.; Shevlin, P. B.; Childers, G.; Peschke, M.; Tsai, J.

    1995-08-01

    Mass spectrometry is routinely covered in undergraduate organic chemistry courses and a number of valuable laboratory experiments featuring its use have been discussed (1-7). Although such experiments work well at institutions with limited laboratory enrollments, we typically teach laboratories with enrollments of 160 or more in which it is difficult to allow each student to carry out a meaningful "hands on" mass spectrometry experiment. Since we feel that some practical experience with this technique is important, we have designed a simple gas chromatography-mass spectrometry (gc/ms) exercise that allows each student to analyze the products of a simple synthesis that they have performed. The exercise starts with the microscale SN2 synthesis of 1-bromobutane from 1-butanol as described by Williamson (8). The students complete the synthesis and place one drop of the distilled product in a screw capped vial. The vials are then sealed, labeled with the students name and taken to the mass spectrometry laboratory by a teaching assistant. Students are instructed to sign up for a 20-min block of time over the next few days in order to analyze their sample. When the student arrives at the laboratory, he or she adds 1 ml CH2Cl2 to the sample and injects 0.3 microliters of the solution into the gas chromatograph. The samples typically contain the 1-butanol starting material and the 1-bromobutane product along with traces of dibutyl ether. The figure shows a mass chromatogram along with the mass spectra of the starting material and product from an actual student run. For this analysis to be applicable to large numbers of students, the gc separation must be as rapid as possible. We have been able to analyze each sample in 6 minutes on a 30 m DB-5 capillary column with the following temperature program: 70 oC for 1 min, 70-80 oC at 10 oC/min, 86-140 oC at 67.5 oC/min, 140-210 oC at 70 oC/min, and 210 oC for 1 min. A mass range of 20-200 amu is scanned with a solvent delay of 2

  1. High-efficiency thermal ionization sources for mass spectrometry

    International Nuclear Information System (INIS)

    Olivares, Jose A.

    1996-01-01

    A version of the thermal ionization cavity (TIC) source developed specifically for use in mass spectrometry is presented. The performance of this ion source has been characterized extensively both with the use of an isotope separator and a quadrupole mass spectrometer. A detailed description of the TIC source for mass spectrometry is given along with the performance characteristics observed

  2. Cs+ ion source for secondary ion mass spectrometry

    International Nuclear Information System (INIS)

    Bentz, B.L.; Weiss, H.; Liebl, H.

    1981-12-01

    Various types of cesium ionization sources currently used in secondary ion mass spectrometry are briefly reviewed, followed by a description of the design and performance of a novel, thermal surface ionization Cs + source developed in this laboratory. The source was evaluated for secondary ion mass spectrometry applications using the COALA ion microprobe mass analyzer. (orig.)

  3. Indigenous instrumentation for mass spectrometry. PD-5-1

    International Nuclear Information System (INIS)

    Handu, V.K.

    2007-01-01

    Mass Spectrometry is a powerful analytical technique due to its high sensitivity, specificity, selectivity, and wide field of applications in elemental analysis, especially in the determination of trace and ultra trace elements, precise and accurate isotopic ratio measurements. Due to these excellent features, it is a crucial analytical tool for number of Department of Atomic Energy's (DAE) programs. BARC, over the years, has developed several mass spectrometers suitable for needs of a number of programs in DAE and, in this process, technologies have been developed in HV/UHV systems, precision mechanical engineering and fabrication, design and fabrication of electromagnets, ion optics, ultra stable analog and digital electronics, data systems etc. A large number of these mass spectrometers are being used regularly in various units of DAE. Since users are demanding TIMS mass spectrometer with better specifications, efforts are being made in house to develop TIMS with improved specifications. Efforts are also under way to develop a multi collector, plasma source mass spectrometer (MC-ICP-MS) with magnetic sector mass analyzer, since such instrument is increasingly being used to measure isotopic ratios with high precision

  4. The emergence of mass spectrometry in biochemical research

    OpenAIRE

    1995-01-01

    The initial steps toward routinely applying mass spectrometry in the biochemical laboratory have been achieved. In the past, mass spectrometry was confined to the realm of small, relatively stable molecules; large or thermally labile molecules did not survive the desorption and ionization processes intact. Electrospray ionization (ESI) and matrix-assisted laser desorption/ionization (MALDI) mass spectrometry allow for the analysis of both small and large biomolecules through "mild" desorption...

  5. Performance evaluation of elemental analysis/isotope ratio mass spectrometry methods for the determination of the D/H ratio in tetramethylurea and other compounds--results of a laboratory inter-comparison.

    Science.gov (United States)

    Bréas, Olivier; Thomas, Freddy; Zeleny, Reinhard; Calderone, Giovanni; Jamin, Eric; Guillou, Claude

    2007-01-01

    Tetramethylurea (TMU) with a certified D/H ratio is the internal standard for Site-specific Natural Isotope Fractionation measured by Nuclear Magnetic Resonance (SNIF-NMR) analysis of wine ethanol for detection of possible adulterations (Commission Regulation 2676/90). A new batch of a TMU certified reference material (CRM) is currently being prepared. Whereas SNIF-NMR has been employed up to now, Elemental Analysis/Isotope Ratio Mass Spectrometry ((2)H-EA-IRMS) was envisaged as the method of choice for value assignment of the new CRM, as more precise (better repeatable) data might be obtained, resulting in lower uncertainty of the certified value. In order to evaluate the accuracy and intra- and inter-laboratory reproducibility of (2)H-EA-IRMS methods, a laboratory inter-comparison was carried out by analysing TMU and other organic compounds, as well as some waters. The results revealed that experienced laboratories are capable of generating robust and well comparable data, which highlights the emerging potential of IRMS in food authenticity testing. However, a systematic bias between IRMS and SNIF-NMR reference data was observed for TMU; this lack of data consistency rules out the (2)H-IRMS technique for the characterisation measurement of the new TMU CRM.

  6. Mass spectrometry a versatile aid to inorganic analysis

    International Nuclear Information System (INIS)

    Stefani, Rene

    1976-01-01

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

  7. Theory and technique of spark source mass spectrometry; Theorie et technique de la spectrometrie de masse a etincelles

    Energy Technology Data Exchange (ETDEWEB)

    Stefani, R [Commissariat a l' Energie Atomique, Grenoble (France). Centre d' Etudes Nucleaires

    1968-07-01

    Trace analysis in solids by spark source mass spectrometry involves complicated phenomena: element ionization in spark and blacking of sensitive emulsion by focused ion beam. However the principal risk of selectivity lies in analyser system, which realizes double focusing only for a part of the ions. Therefore, each analyst has to known ionic optics of his apparatus, for ensuring the transmission of mean energetic ions, which are representative of sample composition. By a careful photometry of mass spectrum, good reproducibility can be obtained. Thereafter accuracy depends on the knowledge of sensitivity coefficients proper to this apparatus. (author) [French] L'analyse de traces dans les solides par spectrometrie de masse a etincelles met en jeu des phenomenes complexes qui sont l'ionisation des elements dans l'etincelle, et le noircissement de l'emulsion sensible par les faisceaux ioniques focalises. Cependant, le risque majeur de selectivite provient de l'ensemble analyseur, qui realise la double focalisation sur une fraction seulement du faisceau d'ions. L'analyste doit donc connaitre en detail l'optique ionique de son appareil, pour assurer le passage de la bande d'energie moyenne des ions, qui seule caracterise quantitativement la composition chimique de l'echantillon. Une exploitation photometrique soignee du spectrogramme donne alors des resultats reproductibles, dont la justesse ne depend plus que des coefficients de sensibilite propres a ce type d'instrument. (auteur)

  8. Application of Nanodiamonds in Biomolecular Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Ping Cheng

    2010-03-01

    Full Text Available The combination of nanodiamond (ND with biomolecular mass spectrometry (MS makes rapid, sensitive detection of biopolymers from complex biosamples feasible. Due to its chemical inertness, optical transparency and biocompatibility, the advantage of NDs in MS study is unique. Furthermore, functionalization on the surfaces of NDs expands their application in the fields of proteomics and genomics for specific requirements greatly. This review presents methods of MS analysis based on solid phase extraction and elution on NDs and different application examples including peptide, protein, DNA, glycan and others. Owing to the quick development of nanotechnology, surface chemistry, new MS methods and the intense interest in proteomics and genomics, a huge increase of their applications in biomolecular MS analysis in the near future can be predicted.

  9. [Application of mass spectrometry in mycology].

    Science.gov (United States)

    Quiles Melero, Inmaculada; Peláez, Teresa; Rezusta López, Antonio; Garcia-Rodríguez, Julio

    2016-06-01

    MALDI-TOF (matrix-assisted laser desorption ionization time-of-flight) mass spectrometry (MS) is becoming an essential tool in most microbiology laboratories. At present, by using a characteristic fungal profile obtained from whole cells or through simple extraction protocols, MALDI-TOF MS allows the identification of pathogenic fungi with a high performance potential. This methodology decreases the laboratory turnaround time, optimizing the detection of mycoses. This article describes the state-of-the-art of the use of MALDI-TOF MS for the detection of human clinical fungal pathogens in the laboratory and discusses the future applications of this technology, which will further improve routine mycological diagnosis. Copyright © 2016 Elsevier España, S.L.U. All rights reserved.

  10. Calibration samples for accelerator mass spectrometry

    International Nuclear Information System (INIS)

    Hershberger, R.L.; Flynn, D.S.; Gabbard, F.

    1981-01-01

    Radioactive samples with precisely known numbers of atoms are useful as calibration sources for lifetime measurements using accelerator mass spectrometry. Such samples can be obtained in two ways: either by measuring the production rate as the sample is created or by measuring the decay rate after the sample has been obtained. The latter method requires that a large sample be produced and that the decay constant be accurately known. The former method is a useful and independent alternative, especially when the decay constant is not well known. The facilities at the University of Kentucky for precision measurements of total neutron production cross sections offer a source of such calibration samples. The possibilities, while quite extensive, would be limited to the proton rich side of the line of stability because of the use of (p,n) and (α,n) reactions for sample production

  11. Subattomole sensitivity in biological accelerator mass spectrometry.

    Science.gov (United States)

    Salehpour, Mehran; Possnert, Göran; Bryhni, Helge

    2008-05-15

    The Uppsala University 5 MV Pelletron tandem accelerator has been used to study (14)C-labeled biological samples utilizing accelerator mass spectrometry (AMS) technology. We have adapted a sample preparation method for small biological samples down to a few tens of micrograms of carbon, involving among others, miniaturizing of the graphitization reactor. Standard AMS requires about 1 mg of carbon with a limit of quantitation of about 10 amol. Results are presented for a range of small sample sizes with concentrations down to below 1 pM of a pharmaceutical substance in human blood. It is shown that (14)C-labeled molecular markers can be routinely measured from the femtomole range down to a few hundred zeptomole (10 (-21) mol), without the use of any additional separation methods.

  12. Radiocarbon dating with accelerator mass spectrometry

    International Nuclear Information System (INIS)

    Blake, W. Jr.

    1985-01-01

    Radiocarbon dating by means of accelerator mass spectrometry (AMS) has two great advantages over conventional dating: 1) much smaller samples can be handled and 2) counting time is significantly shorter. Three examples are given for Holocene-age material from east-central Ellesmere Island. The results demonstrate the potential use of this technique as a powerful research tool in studies of Quaternary chronology. Individual fragments of marine shells as small as 0.1 g have been dated successfully at the IsoTrace Laboratory, University of Toronto. In the case of an aquatic moss from a lake sediment core, an increment 0.5 cm thick could be used instead of a 5 cm-thick slice, thus allowing a much more precise estimate of the onset of organic sedimentation

  13. Analysis of barium by isotope mass spectrometry

    International Nuclear Information System (INIS)

    Long Kaiming; Jia Baoting; Liu Xuemei

    2004-01-01

    The isotopic abundance ratios for barium at sub-microgram level are analyzed by thermal surface ionization mass spectrometry (TIMS). Rhenium trips used for sample preparation are firstly treated to eliminate possible barium background interference. During the preparation of barium samples phosphoric acid is added as an emitting and stabilizing reagent. The addition of phosphoric acid increases the collection efficiency and ion current strength and stability for barium. A relative standard deviation of 0.02% for the isotopic abundance ratio of 137 Ba to 138 Ba is achieved when the 138 Ba ion current is (1-3) x 10 -12 A. The experimental results also demonstrate that the isotope fractionation effect is negligibly small in the isotopic analysis of barium

  14. High-precision measurement of phenylalanine δ15N values for environmental samples: a new approach coupling high-pressure liquid chromatography purification and elemental analyzer isotope ratio mass spectrometry.

    Science.gov (United States)

    Broek, Taylor A B; Walker, Brett D; Andreasen, Dyke H; McCarthy, Matthew D

    2013-11-15

    Compound-specific isotope analysis of individual amino acids (CSI-AA) is a powerful new tool for tracing nitrogen (N) source and transformation in biogeochemical cycles. Specifically, the δ(15)N value of phenylalanine (δ(15)N(Phe)) represents an increasingly used proxy for source δ(15)N signatures, with particular promise for paleoceanographic applications. However, current derivatization/gas chromatography methods require expensive and relatively uncommon instrumentation, and have relatively low precision, making many potential applications impractical. A new offline approach has been developed for high-precision δ(15)N measurements of amino acids (δ(15)N(AA)), optimized for δ(15)N(Phe) values. Amino acids (AAs) are first purified via high-pressure liquid chromatography (HPLC), using a mixed-phase column and automated fraction collection. The δ(15)N values are determined via offline elemental analyzer-isotope ratio mass spectrometry (EA-IRMS). The combined HPLC/EA-IRMS method separated most protein AAs with sufficient resolution to obtain accurate δ(15)N values, despite significant intra-peak isotopic fractionation. For δ(15)N(Phe) values, the precision was ±0.16‰ for standards, 4× better than gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS; ±0.64‰). We also compared a δ(15)N(Phe) paleo-record from a deep-sea bamboo coral from Monterey Bay, CA, USA, using our method versus GC/C/IRMS. The two methods produced equivalent δ(15)N(Phe) values within error; however, the δ(15)N(Phe) values from HPLC/EA-IRMS had approximately twice the precision of GC/C/IRMS (average stdev of 0.27‰ ± 0.14‰ vs 0.60‰ ± 0.20‰, respectively). These results demonstrate that offline HPLC represents a viable alternative to traditional GC/C/IMRS for δ(15)N(AA) measurement. HPLC/EA-IRMS is more precise and widely available, and therefore useful in applications requiring increased precision for data interpretation (e.g. δ(15)N paleoproxies

  15. Enantioselectivity of mass spectrometry: challenges and promises.

    Science.gov (United States)

    Awad, Hanan; El-Aneed, Anas

    2013-01-01

    With the fast growing market of pure enantiomer drugs and bioactive molecules, new chiral-selective analytical tools have been instigated including the use of mass spectrometry (MS). Even though MS is one of the best analytical tools that has efficiently been used in several pharmaceutical and biological applications, traditionally MS is considered as a "chiral-blind" technique. This limitation is due to the MS inability to differentiate between two enantiomers of a chiral molecule based merely on their masses. Several approaches have been explored to assess the potential role of MS in chiral analysis. The first approach depends on the use of MS-hyphenated techniques utilizing fast and sensitive chiral separation tools such as liquid chromatography (LC), gas chromatography (GC), and capillary electrophoresis (CE) coupled to MS detector. More recently, several alternative separation techniques have been evaluated such as supercritical fluid chromatography (SFC) and capillary electrochromatography (CEC); the latter being a hybrid technique that combines the efficiency of CE with the selectivity of LC. The second approach is based on using the MS instrument solely for the chiral recognition. This method depends on the behavioral differences between enantiomers towards a foreign molecule and the ability of MS to monitor such differences. These behavioral differences can be divided into three types: (i) differences in the enantiomeric affinity for association with the chiral selector, (ii) differences of the enantiomeric exchange rate with a foreign reagent, and (iii) differences in the complex MS dissociation behaviors of the enantiomers. Most recently, ion mobility spectrometry was introduced to qualitatively and quantitatively evaluate chiral compounds. This article provides an overview of MS role in chiral analysis by discussing MS based methodologies and presenting the challenges and promises associated with each approach. © 2013 Wiley Periodicals, Inc.

  16. Evaluation of ultrasound-assisted extraction as sample pre-treatment for quantitative determination of rare earth elements in marine biological tissues by inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Costas, M.; Lavilla, I.; Gil, S.; Pena, F.; Calle, I.; Cabaleiro, N. de la; Bendicho, C.

    2010-01-01

    In this work, the determination of rare earth elements (REEs), i.e. Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu in marine biological tissues by inductively coupled-mass spectrometry (ICP-MS) after a sample preparation method based on ultrasound-assisted extraction (UAE) is described. The suitability of the extracts for ICP-MS measurements was evaluated. For that, studies were focused on the following issues: (i) use of clean up of extracts with a C18 cartridge for non-polar solid phase extraction; (ii) use of different internal standards; (iii) signal drift caused by changes in the nebulization efficiency and salt deposition on the cones during the analysis. The signal drift produced by direct introduction of biological extracts in the instrument was evaluated using a calibration verification standard for bracketing (standard-sample bracketing, SSB) and cumulative sum (CUSUM) control charts. Parameters influencing extraction such as extractant composition, mass-to-volume ratio, particle size, sonication time and sonication amplitude were optimized. Diluted single acids (HNO 3 and HCl) and mixtures (HNO 3 + HCl) were evaluated for improving the extraction efficiency. Quantitative recoveries for REEs were achieved using 5 mL of 3% (v/v) HNO 3 + 2% (v/v) HCl, particle size <200 μm, 3 min of sonication time and 50% of sonication amplitude. Precision, expressed as relative standard deviation from three independent extractions, ranged from 0.1 to 8%. In general, LODs were improved by a factor of 5 in comparison with those obtained after microwave-assisted digestion (MAD). The accuracy of the method was evaluated using the CRM BCR-668 (mussel tissue). Different seafood samples of common consumption were analyzed by ICP-MS after UAE and MAD.

  17. Triethylamine-assisted Mg(OH)2 coprecipitation/preconcentration for determination of trace metals and rare earth elements in seawater by inductively coupled plasma mass spectrometry (ICP-MS).

    Science.gov (United States)

    Arslan, Zikri; Oymak, Tulay; White, Jeremy

    2018-05-30

    In this paper, we report an improved magnesium hydroxide, Mg(OH) 2 , coprecipitation method for the determination of 16 trace elements (Al, V, Cr, Mn, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Sb, Sn and Pb) and 18 rare earth elements (REEs), including Sc, Y, U and Th in seawater and estuarine water samples. The procedure involves coprecipitation of the trace elements and REEs on Mg(OH) 2 upon addition of a small volume of triethylamine (TEA) followed by analysis of the dissolved pellet solutions by inductively coupled plasma mass spectrometry (ICP-MS). Three-step sequential coprecipitation was carried out on 10 mL aliquots of seawater to eliminate the matrix ions and to preconcentrate the analytes of interest into a 1 mL final volume. Spike recoveries varied from 85% (Th) to 105% (Y). Calcium (Ca), sodium (Na) and potassium (K) matrices were virtually eliminated from the analysis solutions. Collision reaction interface (CRI) technology utilizing H 2 and He gases was employed to determine its effectiveness in removing the spectral interferences originating from the residual Mg matrix, TEA and plasma gases. H 2 was more effective than He in reducing spectral interferences from TEA and plasma gases. Limits of detection (LODs) ranged from 0.01 ng L -1 (Ho) to 72 ng L -1  (Al). The method was validated by using certified seawater (CASS-4) and estuarine water (SLEW-3) reference materials. Precision for five (n = 5) replicate measurements were between 1.2% (Pr) and 18% (Lu). Fe, Pb, Sn, and Zn impurities in TEA were significant in comparison to the levels in CASS-4 and SLEW-3, while relatively high background signals impacted determinations of low levels of Sc and Th. The effects of these hurdles on precision and accuracy were alleviated by measuring these elements in spiked CASS-4 and SLEW-3. Copyright © 2018 Elsevier B.V. All rights reserved.

  18. Mass spectrometry of acoustically levitated droplets.

    Science.gov (United States)

    Westphall, Michael S; Jorabchi, Kaveh; Smith, Lloyd M

    2008-08-01

    Containerless sample handling techniques such as acoustic levitation offer potential advantages for mass spectrometry, by eliminating surfaces where undesired adsorption/desorption processes can occur. In addition, they provide a unique opportunity to study fundamental aspects of the ionization process as well as phenomena occurring at the air-droplet interface. Realizing these advantages is contingent, however, upon being able to effectively interface levitated droplets with a mass spectrometer, a challenging task that is addressed in this report. We have employed a newly developed charge and matrix-assisted laser desorption/ionization (CALDI) technique to obtain mass spectra from a 5-microL acoustically levitated droplet containing peptides and an ionic matrix. A four-ring electrostatic lens is used in conjunction with a corona needle to produce bursts of corona ions and to direct those ions toward the droplet, resulting in droplet charging. Analyte ions are produced from the droplet by a 337-nm laser pulse and detected by an atmospheric sampling mass spectrometer. The ion generation and extraction cycle is repeated at 20 Hz, the maximum operating frequency of the laser employed. It is shown in delayed ion extraction experiments that both positive and negative ions are produced, behavior similar to that observed for atmospheric pressure matrix-assisted laser absorption/ionization. No ion signal is observed in the absence of droplet charging. It is likely, although not yet proven, that the role of the droplet charging is to increase the strength of the electric field at the surface of the droplet, reducing charge recombination after ion desorption.

  19. Ultratrace analysis of uranium and plutonium by mass spectrometry

    International Nuclear Information System (INIS)

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

    2002-01-01

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

  20. Liquid chromatography - mass spectrometry analysis of pharmaceuticals

    International Nuclear Information System (INIS)

    Macasek, F.

    2003-01-01

    The drugs represent mostly non-volatile and thermally labile solutes, often available only in small amounts like it is in case of radiopharmaceuticals. Therefor, the favourable separation techniques for such compounds are HPLC, capillary electrophoresis and also TLC 1. Liquid chromatography with mass spectrometric detector (LC/MS) is especially powerful for their microanalysis. Mass spectrometry separating the ions in high vacuum was presumably used as detector for gas chromatography effluent but the on-line coupling with liquid eluant flow 0.1-1 mL/min is far more challenging. New types of ion sources were constructed for simultaneous removal of solvent and ionisation of solutes at atmospheric pressure (API). At present, a relatively wide choice of successfully designed commercial equipment is available either for small organic molecules and larger biomolecules (Perkin-Elmer, Agilent, Jeol, Bruker Daltonics, ThermoQuest, Shimadzu). The features of the LC/MS systems are presented. LC/MS as a new quality control tool for [F-18]fluorodeoxyglucose (FDG) radiopharmaceutical, which has became the most spread radiopharmaceutical for positron emission tomography (PET), was proposed. Other applications of the LC/MS are reviewed. (author)

  1. Radiocarbon mass spectrometry for drug development

    International Nuclear Information System (INIS)

    Ulrich, Schulze-Konig Tim

    2011-01-01

    Full text: Radiocarbon has a huge potential as a tracer for metabolism studies in humans. By using Accelerator Mass Spectrometry (AMS) for its detection, a unique sensitivity is reached reducing required radiation doses to a negligible level. Until recently, a widespread use of AMS in biomedical research was impeded by the high complexity of the instrument, time-consuming sample preparation, and a limited availability of measurement capacity. Over the last few years, tremendous progress has been achieved in the reduction of size and complexity of AMS instruments. It allowed designing a compact AMS system, dubbed BioMICADAS to address the needs of biomedical users. For more than two years, this system is in successful operation at a commercial service provider for the pharmaceutical industry. A further drastic simplification of radiocarbon mass spectrometers seems possible and could establish a regular usage of this technology in drug development. However, to reach this goal a better integration of AMS into the workflow of bioanalytical laboratories will be necessary. For this purpose, CO 2 accepting ion sources may be a key, since they enable an almost automated sample preparation. The status of radiocarbon AMS in biomedical research and its perspective will be discussed

  2. Compressed sensing in imaging mass spectrometry

    International Nuclear Information System (INIS)

    Bartels, Andreas; Dülk, Patrick; Trede, Dennis; Alexandrov, Theodore; Maaß, Peter

    2013-01-01

    Imaging mass spectrometry (IMS) is a technique of analytical chemistry for spatially resolved, label-free and multipurpose analysis of biological samples that is able to detect the spatial distribution of hundreds of molecules in one experiment. The hyperspectral IMS data is typically generated by a mass spectrometer analyzing the surface of the sample. In this paper, we propose a compressed sensing approach to IMS which potentially allows for faster data acquisition by collecting only a part of the pixels in the hyperspectral image and reconstructing the full image from this data. We present an integrative approach to perform both peak-picking spectra and denoising m/z-images simultaneously, whereas the state of the art data analysis methods solve these problems separately. We provide a proof of the robustness of the recovery of both the spectra and individual channels of the hyperspectral image and propose an algorithm to solve our optimization problem which is based on proximal mappings. The paper concludes with the numerical reconstruction results for an IMS dataset of a rat brain coronal section. (paper)

  3. Probing the Composition, Assembly and Activity of Protein Molecular Machines using Native Mass Spectrometry

    NARCIS (Netherlands)

    van de Waterbeemd, M.J.

    2017-01-01

    Native mass spectrometry and mass spectrometry in general, are powerful analytical tools for studying proteins and protein complexes. Native mass spectrometry may provide accurate mass measurements of large macromolecular assemblies enabling the investigation of their composition and stoichiometry.

  4. Statistical methods for mass spectrometry-based clinical proteomics

    NARCIS (Netherlands)

    Kakourou, A.

    2018-01-01

    The work presented in this thesis focuses on methods for the construction of diagnostic rules based on clinical mass spectrometry proteomic data. Mass spectrometry has become one of the key technologies for jointly measuring the expression of thousands of proteins in biological samples.

  5. Applications of accelerator mass spectrometry to nuclear physics and astrophysics

    International Nuclear Information System (INIS)

    Guo Zhiyu; Zhang Chuan

    2002-01-01

    As an ultra high sensitive analyzing method, accelerator mass spectrometry is playing an important role in the studies of nuclear physics and astrophysics. The accelerator mass spectrometry (AMS) applications in searching for violation of Pauli exclusion principle and study on supernovae are discussed as examples

  6. Mass spectrometry for real-time quantitative breath analysis

    Czech Academy of Sciences Publication Activity Database

    Smith, D.; Španěl, Patrik; Herbig, J.; Beauchamp, J.

    2014-01-01

    Roč. 8, č. 2 (2014), 027101 ISSN 1752-7155 Institutional support: RVO:61388955 Keywords : breath analysis * proton transfer reaction mass spectrometry * selected ion flow tube mass spectrometry Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 4.631, year: 2014

  7. Laser Mass Spectrometry in Planetary Science

    International Nuclear Information System (INIS)

    Wurz, P.; Whitby, J. A.; Managadze, G. G.

    2009-01-01

    Knowing the chemical, elemental, and isotopic composition of planetary objects allows the study of their origin and evolution within the context of our solar system. Exploration plans in planetary research of several space agencies consider landing spacecraft for future missions. Although there have been successful landers in the past, more landers are foreseen for Mars and its moons, Venus, the jovian moons, and asteroids. Furthermore, a mass spectrometer on a landed spacecraft can assist in the sample selection in a sample-return mission and provide mineralogical context, or identify possible toxic soils on Mars for manned Mars exploration. Given the resources available on landed spacecraft mass spectrometers, as well as any other instrument, have to be highly miniaturised.

  8. Clinical Mass Spectrometry: Achieving Prominence in Laboratory Medicine

    Energy Technology Data Exchange (ETDEWEB)

    Annesley, Thomas M.; Cooks, Robert G.; Herold, David A.; Hoofnagle, Andrew N.

    2016-01-04

    Each year the journal Clinical Chemistry publishes a January special issue on a topic that is relevant to the laboratory medicine community. In January 2016 the topic is mass spectrometry, and the issue is entitled “Clinical Mass Spectrometry: Achieving Prominence in Laboratory Medicine”. One popular feature in our issues is a Q&A on a topic, clearly in this case mass spectrometry. The journal is assembling a panel of 5-6 experts from various areas of mass spectrometry ranging from instrument manufacturing to practicing clinical chemists. Dick Smith is one of the scientist requested to participate in this special issue Q&A on Mass Spectrometry. The Q&A Transcript is attached

  9. Determination of platinum group elements and gold in reference materials by instrumental neutron activation analysis and inductively coupled plasma-mass spectrometry with nickel sulphide fire-assay collection

    International Nuclear Information System (INIS)

    Morcelli, C.P.R.; Figueiredo, A.M.G.; Sarkis, J.E.S.; Kakazu, M.; Enzweiler, J.

    2002-01-01

    Instrumental Neutron Activation Analysis (INAA) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) after NiS fire assay were used to determine platinum group elements (PGE) and Au in the geological reference materials peridotite GPt-3 and pyroxene peridotite GPt-4 (IGGE, China). INAA has been one of the most useful analytical techniques for PGEs and Au determination, due to its high sensitivity and accuracy. After the fire assay, the NiS button is dissolved in concentrated hydrochloric acid, leaving a residue of insoluble PGE sulphides; the solution is filtered and the filter is directly irradiated with neutrons. In more recent years, ICP-MS with nickel fire assay collection and tellurium coprecipitation has been used as a mean of analysing PGE, with the main advantage of avoiding problems of losses of PGE during the HCl digestion of the NiS button. Buttons were prepared by mixing the sample (10-15 g) with fluxes, nickel and sulphur in a fire clay crucible and fused at temperatures around 1000 deg C. For NAA, the filters containing the PGEs and Au were irradiated at the IEA-R1 research nuclear reactor at IPEN. The measurements of the induced gamma-ray activity were carried out in an hyperpure Ge detector. In general, the results obtained by the two techniques were in good agreement with recommended values. INAA results exhibited higher values than the recommended values for Pd and Pt in GPt-3, while the opposite effect was observed for GPt-4 sample. Ru was not detected by INAA. On the other hand, Rh and Ir were determined more accurately by INAA (relative errors better than 10%). The ICP-MS analytical technique showed better detection limits, and all the PGE were determined. Results obtained for Pt and Pd presented accuracy better than 5% while losses were observed for Os and Ir. (author)

  10. Secondary Ion Mass Spectrometry SIMS XI

    Science.gov (United States)

    Gillen, G.; Lareau, R.; Bennett, J.; Stevie, F.

    2003-05-01

    This volume contains 252 contributions presented as plenary, invited and contributed poster and oral presentations at the 11th International Conference on Secondary Ion Mass Spectrometry (SIMS XI) held at the Hilton Hotel, Walt Disney World Village, Orlando, Florida, 7 12 September, 1997. The book covers a diverse range of research, reflecting the rapid growth in advanced semiconductor characterization, ultra shallow depth profiling, TOF-SIMS and the new areas in which SIMS techniques are being used, for example in biological sciences and organic surface characterization. Papers are presented under the following categories: Isotopic SIMS Biological SIMS Semiconductor Characterization Techniques and Applications Ultra Shallow Depth Profiling Depth Profiling Fundamental/Modelling and Diffusion Sputter-Induced Topography Fundamentals of Molecular Desorption Organic Materials Practical TOF-SIMS Polyatomic Primary Ions Materials/Surface Analysis Postionization Instrumentation Geological SIMS Imaging Fundamentals of Sputtering Ion Formation and Cluster Formation Quantitative Analysis Environmental/Particle Characterization Related Techniques These proceedings provide an invaluable source of reference for both newcomers to the field and experienced SIMS users.

  11. New applications of accelerator mass spectrometry

    International Nuclear Information System (INIS)

    Davis, J.C.

    1991-01-01

    Since its invention in the late 70's, and reduction to near-routine practice by the mid-80's, accelerator mass spectrometry (AMS) has become a powerful tool for archaeological and geochemical measurements in which cosmogenic isotopes such as 10 Be, 14 C, 26 Al, 36 Cl and 129 I are used as either tracers or chronometers. The utility of such measurements is demonstrated by the fact that most accelerators having AMS capabilities have significant backlogs of samples awaiting measurement. In designing and justifying a new accelerator facility in which AMS was to be a major feature, we sought to advance the field and increase the resources available for it by two steps: (1) development of new research applications in which intentionally added isotopic labels were used rather than just naturally present ones; and (2) enhancement of spectrometer throughout, making new classes of experiments possible by greatly increasing the number of samples that could be measured in individual experiments. Results of the effort to date suggest that development of a family of very small spectrometers optimized for just tritium and/or radiocarbon will be attractive in the near future

  12. Accelerator mass spectrometry for radiocarbon dating

    International Nuclear Information System (INIS)

    Bronk, C.R.

    1987-01-01

    Accelerator mass spectrometry (AMS) has been used routinely for radiocarbon measurements for several years. This thesis describes theoretical work to understand the reasons for low accuracy and range and offers practical solutions. The production and transport of the ions used in the measurements are found to be the most crucial stages in the process. The theories behind ion production by sputtering are discussed and applied to the specific case of carbon sputtered by caesium. Experimental evidence is also examined in relation to the theories. The phenomena of space charge and lens aberrations are discussed along with the interaction between ion beams and gas molecules in the vacuum. Computer programs for calculating phase space transformations are then described; these are designed to help investigations of the effects of space charge and aberrations on AMS measurements. Calculations using these programs are discussed in relation both to measured ion beam profiles in phase space and to the current dependent transmission of ions through the Oxford radiocarbon accelerator. Improvements have been made to this accelerator and these are discussed in the context of the calculations. C - ions are produced directly from carbon dioxide at the Middleton High Intensity Sputter Source. Experiments to evaluate the performance of such a source are described and detailed design criteria established. An ion source designed and built specifically for radiocarbon measurements using carbon dioxide is described. Experiments to evaluate its performance and investigate the underlying physical processes are discussed. (author)

  13. 14C Accelerator mass spectrometry in Brazil

    International Nuclear Information System (INIS)

    Macario, K.D.; Gomes, P.R.S.; Anjos, Roberto M.; Linares, R.; Queiroz, E.A.; Oliveira, F.M.; Cardozo, L.; Carvalho, C.R.A.

    2011-01-01

    Radiocarbon Accelerator Mass Spectrometry is an ultra-sensitive technique that enables the direct measurement of carbon isotopes in samples as small as a few milligrams. The possibility of dating or tracing rare or even compound specific carbon samples has application in many fields of science such as Archaeology, Geosciences and Biomedicine. Several kinds of material such as wood, charcoal, carbonate and bone can be chemically treated and converted to graphite to be measured in the accelerator system. The Physics Institute of Universidade Federal Fluminense (UFF), in Brazil will soon be able to perform the complete 14 C-AMS measurement of samples. At the Nuclear Chronology Laboratory (LACRON) samples are prepared and converted to carbon dioxide. A stainless steel vacuum system was constructed for carbon dioxide purification and graphitization is performed in sealed tubes in a muffle oven. Graphite samples will be analyzed in a 250 kV Single Stage Accelerator produced by National Electrostatic Corporation which will be installed in the beginning of 2012. With the sample preparation laboratory at LACRON and the SSAMS system, the Physics Institute of UFF will be the first 14 C-AMS facility in Latin America. (author)

  14. Accelerator mass spectrometry of small biological samples.

    Science.gov (United States)

    Salehpour, Mehran; Forsgard, Niklas; Possnert, Göran

    2008-12-01

    Accelerator mass spectrometry (AMS) is an ultra-sensitive technique for isotopic ratio measurements. In the biomedical field, AMS can be used to measure femtomolar concentrations of labeled drugs in body fluids, with direct applications in early drug development such as Microdosing. Likewise, the regenerative properties of cells which are of fundamental significance in stem-cell research can be determined with an accuracy of a few years by AMS analysis of human DNA. However, AMS nominally requires about 1 mg of carbon per sample which is not always available when dealing with specific body substances such as localized, organ-specific DNA samples. Consequently, it is of analytical interest to develop methods for the routine analysis of small samples in the range of a few tens of microg. We have used a 5 MV Pelletron tandem accelerator to study small biological samples using AMS. Different methods are presented and compared. A (12)C-carrier sample preparation method is described which is potentially more sensitive and less susceptible to contamination than the standard procedures.

  15. Tandem mass spectrometry: analysis of complex mixtures

    International Nuclear Information System (INIS)

    Singleton, K.E.

    1985-01-01

    Applications of tandem mass spectrometry (MS/MS) for the analysis of complex mixtures results in increased specificity and selectivity by using a variety of reagent gases in both negative and positive ion modes. Natural isotopic abundance ratios were examined in both simple and complex mixtures using parent, daughter and neutral loss scans. MS/MS was also used to discover new compounds. Daughter scans were used to identify seven new alkaloids in a cactus species. Three of these alkaloids were novel compounds, and included the first simple, fully aromatic isoquinoline alkaloids reported in Cactaceae. MS/MS was used to characterize the chemical reaction products of coal in studies designed to probe its macromolecular structure. Negative ion chemical ionization was utilized to study reaction products resulting from the oxidation of coal. Possible structural units in the precursor coal were predicted based on the reaction products identified, aliphatic and aromatic acids and their anhydrides. The MS/MS method was also used to characterize reaction products resulting from coal liquefaction and/or extraction. These studies illustrate the types of problems for which MS/MS is useful. Emphasis has been placed on characterization of complex mixtures by selecting experimental parameters which enhance the information obtained. The value of using MS/MS in conjunction with other analytical techniques as well as the chemical pretreatment is demonstrated

  16. Imaging mass spectrometry in drug development and toxicology.

    Science.gov (United States)

    Karlsson, Oskar; Hanrieder, Jörg

    2017-06-01

    During the last decades, imaging mass spectrometry has gained significant relevance in biomedical research. Recent advances in imaging mass spectrometry have paved the way for in situ studies on drug development, metabolism and toxicology. In contrast to whole-body autoradiography that images the localization of radiolabeled compounds, imaging mass spectrometry provides the possibility to simultaneously determine the discrete tissue distribution of the parent compound and its metabolites. In addition, imaging mass spectrometry features high molecular specificity and allows comprehensive, multiplexed detection and localization of hundreds of proteins, peptides and lipids directly in tissues. Toxicologists traditionally screen for adverse findings by histopathological examination. However, studies of the molecular and cellular processes underpinning toxicological and pathologic findings induced by candidate drugs or toxins are important to reach a mechanistic understanding and an effective risk assessment strategy. One of IMS strengths is the ability to directly overlay the molecular information from the mass spectrometric analysis with the tissue section and allow correlative comparisons of molecular and histologic information. Imaging mass spectrometry could therefore be a powerful tool for omics profiling of pharmacological/toxicological effects of drug candidates and toxicants in discrete tissue regions. The aim of the present review is to provide an overview of imaging mass spectrometry, with particular focus on MALDI imaging mass spectrometry, and its use in drug development and toxicology in general.

  17. Correcting mass shifts: A lock mass-free recalibration procedure for mass spectrometry imaging data

    Czech Academy of Sciences Publication Activity Database

    Kulkarni, P.; Kaftan, F.; Kynast, P.; Svatoš, Aleš; Böcker, S.

    2015-01-01

    Roč. 407, č. 25 (2015), s. 7603-7613 ISSN 1618-2642 Institutional support: RVO:61388963 Keywords : mass spectrometry imaging * recalibration * mass shift correction * data processing Subject RIV: CB - Analytical Chemistry , Separation Impact factor: 3.125, year: 2015

  18. Automated spike preparation system for Isotope Dilution Mass Spectrometry (IDMS)

    International Nuclear Information System (INIS)

    Maxwell, S.L. III; Clark, J.P.

    1990-01-01

    Isotope Dilution Mass Spectrometry (IDMS) is a method frequently employed to measure dissolved, irradiated nuclear materials. A known quantity of a unique isotope of the element to be measured (referred to as the ''spike'') is added to the solution containing the analyte. The resulting solution is chemically purified then analyzed by mass spectrometry. By measuring the magnitude of the response for each isotope and the response for the ''unique spike'' then relating this to the known quantity of the ''spike'', the quantity of the nuclear material can be determined. An automated spike preparation system was developed at the Savannah River Site (SRS) to dispense spikes for use in IDMS analytical methods. Prior to this development, technicians weighed each individual spike manually to achieve the accuracy required. This procedure was time-consuming and subjected the master stock solution to evaporation. The new system employs a high precision SMI Model 300 Unipump dispenser interfaced with an electronic balance and a portable Epson HX-20 notebook computer to automate spike preparation

  19. Chemically assisted laser ablation ICP mass spectrometry.

    Science.gov (United States)

    Hirata, Takafumi

    2003-01-15

    A new laser ablation technique combined with a chemical evaporation reaction has been developed for elemental ratio analysis of solid samples using an inductively coupled plasma mass spectrometer (ICPMS). Using a chemically assisted laser ablation (CIA) technique developed in this study, analytical repeatability of the elemental ratio measurement was successively improved. To evaluate the reliability of the CLA-ICPMS technique, Pb/U isotopic ratios were determined for zircon samples that have previously been analyzed by other techniques. Conventional laser ablation for Pb/U shows a serious elemental fractionation during ablation mainly due to the large difference in elemental volatility between Pb and U. In the case of Pb/U ratio measurement, a Freon R-134a gas (1,1,1,2-tetrafluoroethane) was introduced into the laser cell as a fluorination reactant. The Freon gas introduced into the laser cell reacts with the ablated sample U, and refractory U compounds are converted to a volatile U fluoride compound (UF6) under the high-temperature condition at the ablation site. This avoids the redeposition of U around the ablation pits. Although not all the U is reacted with Freon, formation of volatile UF compounds improves the transmission efficiency of U. Typical precision of the 206Pb/238U ratio measurement is 3-5% (2sigma) for NIST SRM 610 and Nancy 91500 zircon standard, and the U-Pb age data obtained here show good agreement within analytical uncertainties with the previously reported values. Since the observed Pb/U ratio for solid samples is relatively insensitive to laser power and ablation time, optimization of ablation conditions or acquisition parameters no longer needs to be performed on a sample-to-sample basis.

  20. Inductively coupled plasma – Tandem mass spectrometry (ICP-MS/MS): A powerful and universal tool for the interference-free determination of (ultra)trace elements – A tutorial review

    Energy Technology Data Exchange (ETDEWEB)

    Balcaen, Lieve; Bolea-Fernandez, Eduardo [Ghent University, Department of Analytical Chemistry, Krijgslaan 281-S12, B-9000 Ghent (Belgium); Resano, Martín [University of Zaragoza, Department of Analytical Chemistry, Pedro Cerbuna 12, E-50009 Zaragoza (Spain); Vanhaecke, Frank, E-mail: Frank.Vanhaecke@UGent.be [Ghent University, Department of Analytical Chemistry, Krijgslaan 281-S12, B-9000 Ghent (Belgium)

    2015-09-24

    This paper is intended as a tutorial review on the use of inductively coupled plasma – tandem mass spectrometry (ICP-MS/MS) for the interference-free quantitative determination and isotope ratio analysis of metals and metalloids in different sample types. Attention is devoted both to the instrumentation and to some specific tools and procedures available for advanced method development. Next to the more typical reaction gases, e.g., H{sub 2}, O{sub 2} and NH{sub 3}, also the use of promising alternative gases, such as CH{sub 3}F, is covered, and the possible reaction pathways with those reactive gases are discussed. A variety of published applications relying on the use of ICP-MS/MS are described, to illustrate the added value of tandem mass spectrometry in (ultra)trace analysis. - Highlights: • First review on tandem ICP-mass spectrometry (ICP-MS/MS). • Clear description of operating principles of ICP-MS/MS. • Description on how to make use of product ion scans, precursor ion scans and neutral gain scans in method development. • Overview of applications published so far.

  1. Inductively coupled plasma – Tandem mass spectrometry (ICP-MS/MS): A powerful and universal tool for the interference-free determination of (ultra)trace elements – A tutorial review

    International Nuclear Information System (INIS)

    Balcaen, Lieve; Bolea-Fernandez, Eduardo; Resano, Martín; Vanhaecke, Frank

    2015-01-01

    This paper is intended as a tutorial review on the use of inductively coupled plasma – tandem mass spectrometry (ICP-MS/MS) for the interference-free quantitative determination and isotope ratio analysis of metals and metalloids in different sample types. Attention is devoted both to the instrumentation and to some specific tools and procedures available for advanced method development. Next to the more typical reaction gases, e.g., H_2, O_2 and NH_3, also the use of promising alternative gases, such as CH_3F, is covered, and the possible reaction pathways with those reactive gases are discussed. A variety of published applications relying on the use of ICP-MS/MS are described, to illustrate the added value of tandem mass spectrometry in (ultra)trace analysis. - Highlights: • First review on tandem ICP-mass spectrometry (ICP-MS/MS). • Clear description of operating principles of ICP-MS/MS. • Description on how to make use of product ion scans, precursor ion scans and neutral gain scans in method development. • Overview of applications published so far.

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

    DEFF Research Database (Denmark)

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

    2010-01-01

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

  3. Interpretation of Tandem Mass Spectrometry (MSMS) Spectra for Peptide Analysis

    DEFF Research Database (Denmark)

    Hjernø, Karin; Højrup, Peter

    2015-01-01

    The aim of this chapter is to give a short introduction to peptide analysis by mass spectrometry (MS) and interpretation of fragment mass spectra. Through examples and guidelines we demonstrate how to understand and validate search results and how to perform de novo sequencing based on the often...... very complex fragmentation pattern obtained by tandem mass spectrometry (also referred to as MSMS). The focus is on simple rules for interpretation of MSMS spectra of tryptic as well as non-tryptic peptides....

  4. 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)

    Pedreira Filho, Walter dos Reis

    2000-01-01

    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 (La 2 O 3 ; CeO 2 ; Pr 6 O 11 ; Nd 2 O 3 ; Sm 2 O 3 ; Gd 2 O 3 ; Y 2 O 3 ) 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

  5. Redox speciation of final repository relevant elements using separation methods in combination with ICP mass spectrometry; Redoxspeziation von endlagerrelevanten Elementen mit Hilfe von Trennmethoden gekoppelt an ein Massenspektrometer mit induktiv gekoppeltem Plasma

    Energy Technology Data Exchange (ETDEWEB)

    Graser, Carl-Heinrich

    2015-12-18

    The long-term safety assessment for nuclear waste repositories requires a detailed understanding of the chemistry of actinide elements in the geosphere. The development of advanced analytical tools is required to gain detailed insights into actinide redox speciation in a given system. The mobility of radionuclides is mostly determined by the geochemical conditions which control the redox state of radionuclides. Besides the longlived radionuclides plutonium (Pu) and neptunium (Np), which are key elements in high level nuclear waste, iron (Fe) represents a main component in natural systems controlling redox related geochemical processes. Analytical techniques for determining oxidation state distribution for redox sensitive radionuclides and other metal ions often have a lack of sensitivity. The detection limits of these methods (i.e. UV/vis, TRLFS, XANES) are in general in the range of ≥ 10{sup -6} mol.L{sup -1}. As a consequence ultrasensitive new analytical techniques are required. Capillary electrophoresis (CE) and ion chromatography (IC) are powerful separation methods for metal ions. In the course of this thesis different speciation method for iron, neptunium and plutonium were optimized. With the optimized setup redox speciation analysis of these elements in different samples were done. Furthermore CE hyphenated to inductively coupled plasma sector field mass spectrometry (CE - ICP - SF - MS) was used to measure the redox speciation of Pu (III, IV, V, VI), Np (IV, V, VI) and Fe (II, III) at concentrations lower than 10{sup -7} mol.L{sup -1}. CE coupling and separation parameters such as sample gas pressure, make up flow rate, capillary position, auxiliary gas flow, as well as the electrolyte system were optimized to obtain the maximum sensitivity. The methodes detection limits are 10{sup -12} mol.L{sup -1} for Np and Pu. The various oxidation state species of Pu and Np in different samples were separated by application of an acetate based electrolyte system

  6. [Advances in mass spectrometry-based approaches for neuropeptide analysis].

    Science.gov (United States)

    Ji, Qianyue; Ma, Min; Peng, Xin; Jia, Chenxi; Ji, Qianyue

    2017-07-25

    Neuropeptides are an important class of endogenous bioactive substances involved in the function of the nervous system, and connect the brain and other neural and peripheral organs. Mass spectrometry-based neuropeptidomics are designed to study neuropeptides in a large-scale manner and obtain important molecular information to further understand the mechanism of nervous system regulation and the pathogenesis of neurological diseases. This review summarizes the basic strategies for the study of neuropeptides using mass spectrometry, including sample preparation and processing, qualitative and quantitative methods, and mass spectrometry imagining.

  7. Mass spectrometry for characterizing plant cell wall polysaccharides

    Directory of Open Access Journals (Sweden)

    Stefan eBauer

    2012-03-01

    Full Text Available Mass spectrometry is a selective and powerful technique to obtain identification and structural information on compounds present in complex mixtures. Since it requires only small sample amount it is an excellent tool for researchers interested in detecting changes in composition of complex carbohydrates of plants. This mini-review gives an overview of common mass spectrometry techniques applied to the analysis of plant cell wall carbohydrates. It presents examples in which mass spectrometry has been used to elucidate the structure of oligosaccharides derived from hemicelluloses and pectins and illustrates how information on sequence, linkages, branching and modifications are obtained from characteristic fragmentation patterns.

  8. [Latest development in mass spectrometry for clinical application].

    Science.gov (United States)

    Takino, Masahiko

    2013-09-01

    Liquid chromatography-tandem mass spectrometry (LC-MS/MS) has seen enormous growth in special clinical chemistry laboratories. It significantly increases the analytic potential in clinical chemistry, especially in the field of low molecular weight biomarker analysis. This review summarizes the state of the art in mass spectrometry and related techniques for clinical application with a main focus on recent developments in LC-MS. Current trends in ionization techniques, automated online sample preparation techniques coupled with LC-MS, and ion mobility spectrometry are discussed. Emerging mass spectrometric approaches complementary to LC-MS are discussed as well.

  9. Proteomic Mass Spectrometry Imaging for Skin Cancer Diagnosis.

    Science.gov (United States)

    Lazova, Rossitza; Seeley, Erin H

    2017-10-01

    Mass spectrometry imaging can be successfully used for skin cancer diagnosis, particularly for the diagnosis of challenging melanocytic lesions. This method analyzes proteins within benign and malignant melanocytic tumor cells and, based on their differences, which constitute a unique molecular signature of 5 to 20 proteins, can render a diagnosis of benign nevus versus malignant melanoma. Mass spectrometry imaging may assist in the differentiation between metastases and nevi as well as between proliferative nodules in nevi and melanoma arising in a nevus. In the difficult area of atypical Spitzoid neoplasms, mass spectrometry diagnosis can predict clinical outcome better than histopathology. Copyright © 2017 Elsevier Inc. All rights reserved.

  10. Application of inorganic mass spectrometry to problems in atmospheric chemistry

    International Nuclear Information System (INIS)

    Kelly, W.R.

    1990-01-01

    The measurement of isotopes by thermal ionization mass spectrometry is a highly sensitive and accurate technique which can be used to determine the concentration of specific nuclides as well as the isotopic composition in environmental samples. The first application uses isotope dilution which makes possible the determination of all elements with two or more stable isotopes in all types of matrices. The second application is a very powerful and useful application in atmospheric chemistry because it permits the use of stable isotopes as definitive intentional tracers of emissions from high temperature combustion sources. The use of stable isotopes of S, Nd, Sm, and U in the study of visibility, deposition, and definitive tracing of emissions will be presented

  11. Translational imaging mass spectrometry: From CERN to the surgeon

    CERN Multimedia

    CERN. Geneva

    2018-01-01

    A comprehensive understanding of molecular patterns of health and disease is needed to pave the way for personalized medicine and tissue regeneration. New Mass Spectrometry based chemical microscopes that target biomedical tissue analysis in various diseases as well as other chemically complex surfaces have now firmly established themselves in translational research. In concert they elucidate the way in which local environments can influence molecular signaling pathways on various scales, from molecule to man. The integration of this pathway information in a surgical setting is imminent, but innovations that push the boundaries of the technology and its application are still needed. In particular, researchers investigate comprehensive and isolated biomolecular molecular patterns of health and disease. This is a key element needed to pave the way for personalized medicine and tissue regeneration. One barrier to predictive, personalized medicine is the lack of a comprehensive molecular understanding at the ti...

  12. Resonance ionization mass spectrometry using tunable diode lasers

    International Nuclear Information System (INIS)

    Shaw, R.W.; Young, J.P.; Smith, D.H.

    1990-01-01

    Tunable semiconductor diode lasers will find many important applications in atomic spectroscopy. They exhibit the desirable attributes of lasers: narrow bandwidth, tunability, and spatial coherence. At the same time, they possess few of the disadvantages of other tunable lasers. They require no alignment, are simple to operate, and are inexpensive. Practical laser spectroscopic instruments can be envisioned. The authors have applied diode lasers to resonance ionization mass spectrometry (RIMS) of some of the lanthanide elements. Sub-Doppler resolution spectra have been recorded and have been used for atomic hyperfine structure analysis. Isotopically-selective ionization has been accomplished, even in cases where photons from a broadband dye laser are part of the overall ionization process and where the isotopic spectral shift is very small. A convenient RIMS instrument for isotope ratio measurements that employs only diode lasers, along with electric field ionization, should be possible

  13. UV and IR laser ablation for inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Smith, M.R.; Koppenaal, D.W.; Farmer, O.T.

    1993-06-01

    Laser ablation particle plume compositions are characterized using inductively coupled plasma mass spectrometry (ICP/MS). This study evaluates the mass response characteristics peculiar to ICP/MS detection as a function of laser fluence and frequency. Evaluation of the ICP/MS mass response allows deductions to be made concerning how representative the laser ablation produced particle plume composition is relative to the targeted sample. Using a black glass standard, elemental fractionation was observed, primarily for alkalis and other volatile elements. The extent of elemental fractionation between the target sample and the sampled plume varied significantly as a function of laser fluences and IR and UV laser frequency

  14. New developments in glow discharge optical emission and mass spectrometry

    International Nuclear Information System (INIS)

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

    2000-01-01

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

  15. imzML: Imaging Mass Spectrometry Markup Language: A common data format for mass spectrometry imaging.

    Science.gov (United States)

    Römpp, Andreas; Schramm, Thorsten; Hester, Alfons; Klinkert, Ivo; Both, Jean-Pierre; Heeren, Ron M A; Stöckli, Markus; Spengler, Bernhard

    2011-01-01

    Imaging mass spectrometry is the method of scanning a sample of interest and generating an "image" of the intensity distribution of a specific analyte. The data sets consist of a large number of mass spectra which are usually acquired with identical settings. Existing data formats are not sufficient to describe an MS imaging experiment completely. The data format imzML was developed to allow the flexible and efficient exchange of MS imaging data between different instruments and data analysis software.For this purpose, the MS imaging data is divided in two separate files. The mass spectral data is stored in a binary file to ensure efficient storage. All metadata (e.g., instrumental parameters, sample details) are stored in an XML file which is based on the standard data format mzML developed by HUPO-PSI. The original mzML controlled vocabulary was extended to include specific parameters of imaging mass spectrometry (such as x/y position and spatial resolution). The two files (XML and binary) are connected by offset values in the XML file and are unambiguously linked by a universally unique identifier. The resulting datasets are comparable in size to the raw data and the separate metadata file allows flexible handling of large datasets.Several imaging MS software tools already support imzML. This allows choosing from a (growing) number of processing tools. One is no longer limited to proprietary software, but is able to use the processing software which is best suited for a specific question or application. On the other hand, measurements from different instruments can be compared within one software application using identical settings for data processing. All necessary information for evaluating and implementing imzML can be found at http://www.imzML.org .

  16. Use of mass spectrometry for study of coordination compounds

    International Nuclear Information System (INIS)

    Gehrbehlehu, N.V.; Indrichan, K.M.

    1981-01-01

    A review on mass-spectrometry of coordination compounds including the works published up to 1979 inclusive is provided. Mainly the products of metals with bi- and tetradentate ligands are considered using the method. Mo and Be carboxylates for which molecular ions lines are found in mass-spectra are studied. The study of mass-spectra for VO chelates with thiosemicarbazone of salicyl aldehyde is carried out. Application of the mass-spectrometry method permits to establish the mass of coordination compounds, the structure of complexes, dentate structure and the way of ligand coordination, the bond strength [ru

  17. The allure of mass spectrometry: From an earlyday chemist's perspective.

    Science.gov (United States)

    Tőkés, László

    2017-07-01

    This reminiscing review article is an account of the author's fascination and involvements with mass spectrometry from the perspective of an organic chemist with an interest in natural product chemistry. It covers a period from 1961 through the mid 1990s as mass spectrometry evolved form a novelty technique to become a most widely used analytical technique. Following a brief synopsis of my pathway to mass spectrometry, my research efforts in this field are presented with a focus mainly on evolving principles and technologies which I had personal involvements with. To provide historical perspectives, discussions of these developments are accompanied by brief outlines of the relevant state-of-the-art, shedding light on the technical and conceptual challenges encountered during those early days in mass spectrometry. Examples are presented of my involvements with basic and applied research in mass spectrometry during graduate studies at Stanford University and close to three decade tenure in pharmaceutical research at Syntex Research. My basic research interests focused mainly on principles of electron ionization induced fragmentation mechanisms, with an emphasis on steroids and other model compounds. Extensive deuterium labeling evidence was used to determine the fragmentation mechanisms of the diagnostically significant ions in the spectra of numerous model compounds, uncovering examples of wide-ranging hydrogen transfers, skeletal rearrangements, methyl and phenyl migrations, stereoselective fragmentations and low and high energy fragmentation processes. Depiction of the industrial research phase of my career includes comments on the pivotal role mass spectrometry played on advancing modern pharmaceutical research. Examples are presented of involvements with instrumental developments and a few select cases of applied research, including studies of bile mechanisms in vertebrates, identification of bisphenol-A leaching from sterilized polycarbonate containers, high

  18. Microbial metabolomics with gas chromatography/mass spectrometry

    NARCIS (Netherlands)

    Koek, M.M.; Muilwijk, B.; Werf, M.J. van der; Hankemeier, T.

    2006-01-01

    An analytical method was set up suitable for the analysis of microbial metabolomes, consisting of an oximation and silylation derivatization reaction and subsequent analysis by gas chromatography coupled to mass spectrometry. Microbial matrixes contain many compounds that potentially interfere with

  19. Sampling and analyte enrichment strategies for ambient mass spectrometry.

    Science.gov (United States)

    Li, Xianjiang; Ma, Wen; Li, Hongmei; Ai, Wanpeng; Bai, Yu; Liu, Huwei

    2018-01-01

    Ambient mass spectrometry provides great convenience for fast screening, and has showed promising potential in analytical chemistry. However, its relatively low sensitivity seriously restricts its practical utility in trace compound analysis. In this review, we summarize the sampling and analyte enrichment strategies coupled with nine modes of representative ambient mass spectrometry (desorption electrospray ionization, paper vhspray ionization, wooden-tip spray ionization, probe electrospray ionization, coated blade spray ionization, direct analysis in real time, desorption corona beam ionization, dielectric barrier discharge ionization, and atmospheric-pressure solids analysis probe) that have dramatically increased the detection sensitivity. We believe that these advances will promote routine use of ambient mass spectrometry. Graphical abstract Scheme of sampling stretagies for ambient mass spectrometry.

  20. Analytical strategies in mass spectrometry-based phosphoproteomics

    DEFF Research Database (Denmark)

    Rosenqvist, Heidi; Ye, Juanying; Jensen, Ole N

    2011-01-01

    then discuss various tandem mass spectrometry approaches for phosphopeptide sequencing and quantification, and we consider aspects of phosphoproteome data analysis and interpretation. Efficient integration of these stages of phosphoproteome analysis is highly important to ensure a successful outcome of large...

  1. Biomarker discovery in high grade sarcomas by mass spectrometry imaging

    OpenAIRE

    Lou, S.

    2017-01-01

    This thesis demonstrates a detailed biomarker discovery Mass Spectrometry Imaging workflow for histologically heterogeneous high grade sarcomas. Panels of protein and metabolite signatures were discovered either distinguishing different histological subtypes or stratifying high risk patients with poor survival.

  2. A theory of stable-isotope dilution mass spectrometry

    International Nuclear Information System (INIS)

    Pickup, J.F.; McPherson, C.K.

    1977-01-01

    In order to perform quantitative analysis using stable isotope dilution with mass spectrometry, an equation is derived which describes the relationship between the relative proportions of natural and labelled material and measured isotope ratios

  3. Chemical ionisation mass spectrometry: a survey of instrument technology

    International Nuclear Information System (INIS)

    Mather, R.E.; Todd, J.F.J.

    1979-01-01

    The purpose of this review is to survey the innovations and improvements which have been made in both instrumentation and methodology in chemical ionization mass spectrometry in the past ten years. (Auth.)

  4. 13th International Mass Spectrometry Conference. Book of Abstracts

    International Nuclear Information System (INIS)

    1994-01-01

    The collection contains abstracts of several hundred papers presented at the international conference on new research and development results and applications of mass spectrometry. Abstracts falling into the INIS scope were indexed separately in the INIS database. (Roboz, P.)

  5. OBT measurement of vegetation by mass spectrometry and radiometry

    International Nuclear Information System (INIS)

    Tamari, T.; Kakiuchi, H.; Momoshima, N.; Sugihara, S.; Baglan, N.; Uda, T.

    2011-01-01

    We carried out OBT (organically bound tritium) measurement by two different methods those are radiometry and mass spectrometry and compared the applicability of these methods for environmental tritium analysis. The dried grass sample was used for the experiments. To eliminate the exchangeable OBT, the sample was washed with tritium free water before analysis. Three times washing reduced the tritium activity in the labile sites below the detectable level. In radiometry the sample was combusted to convert the OBT as well as other hydrogen isotopes to. water and tritium activity in the water was measured by liquid scintillation counting (LSC). In mass spectrometry, the sample was kept in a glass container and 3 He produced by tritium decay was measured by mass spectrometry. The results were in good agreement suggesting applicability of these methods for environmental tritium analysis. The mass spectrometry is more suitable for environmental tritium research because of a lower detection limit than that of the LSC. (authors)

  6. Laser mass spectrometry for DNA sequencing, disease diagnosis, and fingerprinting

    Energy Technology Data Exchange (ETDEWEB)

    Winston Chen, C.H.; Taranenko, N.I.; Zhu, Y.F.; Chung, C.N.; Allman, S.L.

    1997-03-01

    Since laser mass spectrometry has the potential for achieving very fast DNA analysis, the authors recently applied it to DNA sequencing, DNA typing for fingerprinting, and DNA screening for disease diagnosis. Two different approaches for sequencing DNA have been successfully demonstrated. One is to sequence DNA with DNA ladders produced from Snager`s enzymatic method. The other is to do direct sequencing without DNA ladders. The need for quick DNA typing for identification purposes is critical for forensic application. The preliminary results indicate laser mass spectrometry can possibly be used for rapid DNA fingerprinting applications at a much lower cost than gel electrophoresis. Population screening for certain genetic disease can be a very efficient step to reducing medical costs through prevention. Since laser mass spectrometry can provide very fast DNA analysis, the authors applied laser mass spectrometry to disease diagnosis. Clinical samples with both base deletion and point mutation have been tested with complete success.

  7. Recent applications of mass spectrometry in forensic toxicology

    Science.gov (United States)

    Foltz, Rodger L.

    1992-09-01

    This review encompasses applications of mass spectrometry reported during the years 1989, 1990 and 1991 for the analysis of cannabinoids, cocaine, opiates, amphetamines, lysergic acid diethylamide (LSD), and their metabolites in physiological specimens.

  8. Dehydrodimerization of pterostilbene during electrospray ionization mass spectrometry

    KAUST Repository

    Raji, Misjudeen; Amad, Maan H.; Emwas, Abdul-Hamid M.

    2013-01-01

    RATIONALE Pterostilbene is a member of the hydroxystilbene family of compounds commonly found in plants such as blueberry and grapes. During the analysis of this compound by electrospray ionization mass spectrometry (ESI-MS), an ion was observed

  9. 13th International Mass Spectrometry Conference. Book of Abstracts

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1994-12-31

    The collection contains abstracts of several hundred papers presented at the international conference on new research and development results and applications of mass spectrometry. Abstracts falling into the INIS scope were indexed separately in the INIS database. (Roboz, P.).

  10. Gas Chromatography Mass Spectrometry of Quassia undulata Seed ...

    African Journals Online (AJOL)

    Prof. Ogunji

    The use of gas chromatography mass spectrometry (GC MS) as a sensitive and specific technique ... cold flow properties and stability of the fuel to oxidation, peroxidation and polymerization .... determinants of both the physical and chemical ...

  11. Practical aspects and trends in analytical organic mass spectrometry

    International Nuclear Information System (INIS)

    Schlunegger, U.P.

    1981-01-01

    Proceeding from the fundamentals of mass spectrometry (MS), some more recent developments of analytical organic MS are shown in comparison with conventional MS. Sections are headed: the vacuum, production of ions in the mass spectrometer, ions in the analyzer of a mass spectrometer, general considerations, practice of modern MS: selected examples

  12. Optimization of on-line hydrogen stable isotope ratio measurements of halogen- and sulfur-bearing organic compounds using elemental analyzer-chromium/high-temperature conversion isotope ratio mass spectrometry (EA-Cr/HTC-IRMS).

    Science.gov (United States)

    Gehre, Matthias; Renpenning, Julian; Geilmann, Heike; Qi, Haiping; Coplen, Tyler B; Kümmel, Steffen; Ivdra, Natalija; Brand, Willi A; Schimmelmann, Arndt

    2017-03-30

    Accurate hydrogen isotopic analysis of halogen- and sulfur-bearing organics has not been possible with traditional high-temperature conversion (HTC) because the formation of hydrogen-bearing reaction products other than molecular hydrogen (H 2 ) is responsible for non-quantitative H 2 yields and possible hydrogen isotopic fractionation. Our previously introduced, new chromium-based EA-Cr/HTC-IRMS (Elemental Analyzer-Chromium/High-Temperature Conversion Isotope Ratio Mass Spectrometry) technique focused primarily on nitrogen-bearing compounds. Several technical and analytical issues concerning halogen- and sulfur-bearing samples, however, remained unresolved and required further refinement of the reactor systems. The EA-Cr/HTC reactor was substantially modified for the conversion of halogen- and sulfur-bearing samples. The performance of the novel conversion setup for solid and liquid samples was monitored and optimized using a simultaneously operating dual-detection system of IRMS and ion trap MS. The method with several variants in the reactor, including the addition of manganese metal chips, was evaluated in three laboratories using EA-Cr/HTC-IRMS (on-line method) and compared with traditional uranium-reduction-based conversion combined with manual dual-inlet IRMS analysis (off-line method) in one laboratory. The modified EA-Cr/HTC reactor setup showed an overall H 2 -recovery of more than 96% for all halogen- and sulfur-bearing organic compounds. All results were successfully normalized via two-point calibration with VSMOW-SLAP reference waters. Precise and accurate hydrogen isotopic analysis was achieved for a variety of organics containing F-, Cl-, Br-, I-, and S-bearing heteroelements. The robust nature of the on-line EA-Cr/HTC technique was demonstrated by a series of 196 consecutive measurements with a single reactor filling. The optimized EA-Cr/HTC reactor design can be implemented in existing analytical equipment using commercially available material and

  13. Subcellular analysis by laser ablation electrospray ionization mass spectrometry

    Science.gov (United States)

    Vertes, Akos; Stolee, Jessica A; Shrestha, Bindesh

    2014-12-02

    In various embodiments, a method of laser ablation electrospray ionization mass spectrometry (LAESI-MS) may generally comprise micro-dissecting a cell comprising at least one of a cell wall and a cell membrane to expose at least one subcellular component therein, ablating the at least one subcellular component by an infrared laser pulse to form an ablation plume, intercepting the ablation plume by an electrospray plume to form ions, and detecting the ions by mass spectrometry.

  14. Automated, parallel mass spectrometry imaging and structural identification of lipids

    DEFF Research Database (Denmark)

    Ellis, Shane R.; Paine, Martin R.L.; Eijkel, Gert B.

    2018-01-01

    We report a method that enables automated data-dependent acquisition of lipid tandem mass spectrometry data in parallel with a high-resolution mass spectrometry imaging experiment. The method does not increase the total image acquisition time and is combined with automatic structural assignments....... This lipidome-per-pixel approach automatically identified and validated 104 unique molecular lipids and their spatial locations from rat cerebellar tissue....

  15. Quantification of steroid conjugates using fast atom bombardment mass spectrometry

    International Nuclear Information System (INIS)

    Gaskell, S.J.

    1990-01-01

    Fast atom bombardment/mass spectrometry or liquid secondary ion mass spectrometry provides the capability for direct analysis of steroid conjugates (sulfates, glucuronides) without prior hydrolysis or derivatization. During the analysis of biologic extracts, limitations on the sensitivity of detection arise from the presence of co-extracted material which may suppress or obscure the analyte signal. A procedure is described for the quantitative determination of dehydroepiandrosterone sulfate in serum which achieved selective isolation of the analyte using immunoadsorption extraction and highly specific detection using tandem mass spectrometry. A stable isotope-labeled analog [( 2H2]dehydroepiandrosterone sulfate) was used as internal standard. Fast atom bombardment of dehydroepiandrosterone sulfate yielded abundant [M-H]- ions that fragmented following collisional activation to give HSO4-; m/z 97. During fast atom bombardment/tandem mass spectrometry of serum extracts, a scan of precursor ions fragmenting to give m/z 97 detected dehydroepiandrosterone sulfate and the [2H2]-labeled analog with a selectivity markedly superior to that observed using conventional mass spectrometry detection. Satisfactory agreement was observed between quantitative data obtained in this way and data obtained by gas chromatography/mass spectrometry of the heptafluorobutyrates of dehydroepiandrosterone sulfate and [2H2]dehydroepiandrosterone sulfate obtained by direct derivatization. 21 refs

  16. New approaches for metabolomics by mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Vertes, Akos [George Washington Univ., Washington, DC (United States)

    2017-07-10

    Small molecules constitute a large part of the world around us, including fossil and some renewable energy sources. Solar energy harvested by plants and bacteria is converted into energy rich small molecules on a massive scale. Some of the worst contaminants of the environment and compounds of interest for national security also fall in the category of small molecules. The development of large scale metabolomic analysis methods lags behind the state of the art established for genomics and proteomics. This is commonly attributed to the diversity of molecular classes included in a metabolome. Unlike nucleic acids and proteins, metabolites do not have standard building blocks, and, as a result, their molecular properties exhibit a wide spectrum. This impedes the development of dedicated separation and spectroscopic methods. Mass spectrometry (MS) is a strong contender in the quest for a quantitative analytical tool with extensive metabolite coverage. Although various MS-based techniques are emerging for metabolomics, many of these approaches include extensive sample preparation that make large scale studies resource intensive and slow. New ionization methods are redefining the range of analytical problems that can be solved using MS. This project developed new approaches for the direct analysis of small molecules in unprocessed samples, as well as pushed the limits of ultratrace analysis in volume limited complex samples. The projects resulted in techniques that enabled metabolomics investigations with enhanced molecular coverage, as well as the study of cellular response to stimuli on a single cell level. Effectively individual cells became reaction vessels, where we followed the response of a complex biological system to external perturbation. We established two new analytical platforms for the direct study of metabolic changes in cells and tissues following external perturbation. For this purpose we developed a novel technique, laser ablation electrospray

  17. Bayesian Integration and Characterization of Composition C-4 Plastic Explosives Based on Time-of-Flight Secondary Ion Mass Spectrometry and Laser Ablation-Inductively Coupled Plasma Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mahoney, Christine M.; Kelly, Ryan T.; Alexander, M. L.; Newburn, Matthew K.; Bader, Sydney P.; Ewing, Robert G.; Fahey, Albert J.; Atkinson, David A.; Beagley, Nathaniel

    2016-02-25

    Key elements regarding the use of non-radioactive ionization sources will be presented as related to explosives detection by mass spectrometry and ion mobility spectrometry. Various non-radioactive ionization sources will be discussed along with associated ionization mechanisms pertaining to specific sample types.

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

    International Nuclear Information System (INIS)

    De Villiers, W. van Z.

    1983-11-01

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

  19. Isotope dilution mass spectrometry for nuclear material accountability measurements: dreams and reality

    International Nuclear Information System (INIS)

    Deron, S.; )

    1996-01-01

    Gravimetry, titration, coulometry and isotope dilution mass spectrometry are alternative techniques which can be used to obtain elemental assays of the desirable accuracy. The communication briefly describes the characteristics of the procedure and summarizes a wealth of experience accumulated during actual accountability verification activities

  20. Applications of inductively coupled plasma mass spectrometry and laser ablation inductively coupled plasma mass spectrometry in materials science

    International Nuclear Information System (INIS)

    Becker, Johanna Sabine

    2002-01-01

    Inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation ICP-MS (LA-ICP-MS) have been applied as the most important inorganic mass spectrometric techniques having multielemental capability for the characterization of solid samples in materials science. ICP-MS is used for the sensitive determination of trace and ultratrace elements in digested solutions of solid samples or of process chemicals (ultrapure water, acids and organic solutions) for the semiconductor industry with detection limits down to sub-picogram per liter levels. Whereas ICP-MS on solid samples (e.g. high-purity ceramics) sometimes requires time-consuming sample preparation for its application in materials science, and the risk of contamination is a serious drawback, a fast, direct determination of trace elements in solid materials without any sample preparation by LA-ICP-MS is possible. The detection limits for the direct analysis of solid samples by LA-ICP-MS have been determined for many elements down to the nanogram per gram range. A deterioration of detection limits was observed for elements where interferences with polyatomic ions occur. The inherent interference problem can often be solved by applying a double-focusing sector field mass spectrometer at higher mass resolution or by collision-induced reactions of polyatomic ions with a collision gas using an ICP-MS fitted with collision cell. The main problem of LA-ICP-MS is quantification if no suitable standard reference materials with a similar matrix composition are available. The calibration problem in LA-ICP-MS can be solved using on-line solution-based calibration, and different procedures, such as external calibration and standard addition, have been discussed with respect to their application in materials science. The application of isotope dilution in solution-based calibration for trace metal determination in small amounts of noble metals has been developed as a new calibration strategy. This review discusses new

  1. Use of a discharge in an hollow cathode as neutral atom source for resonant ionization mass spectrometry

    International Nuclear Information System (INIS)

    Berthoud, T.; Briand, A.; Khelifa, N.; Mauchien, P.

    1987-01-01

    The resonance ionization mass spectrometry in our laboratory is aimed at simplification of isotope measurements of elements present in mixtures and at measurement of very small isotopes. An atomization source which produces an atomic beam collimated from a discharge in a hollow cathode has been developed. First results of this spectrometry with an uranium atomic jet are presented [fr

  2. MPAI (mass probes aided ionization) method for total analysis of biomolecules by mass spectrometry.

    Science.gov (United States)

    Honda, Aki; Hayashi, Shinichiro; Hifumi, Hiroki; Honma, Yuya; Tanji, Noriyuki; Iwasawa, Naoko; Suzuki, Yoshio; Suzuki, Koji

    2007-01-01

    We have designed and synthesized various mass probes, which enable us to effectively ionize various molecules to be detected with mass spectrometry. We call the ionization method using mass probes the "MPAI (mass probes aided ionization)" method. We aim at the sensitive detection of various biological molecules, and also the detection of bio-molecules by a single mass spectrometry serially without changing the mechanical settings. Here, we review mass probes for small molecules with various functional groups and mass probes for proteins. Further, we introduce newly developed mass probes for proteins for highly sensitive detection.

  3. Extending Penning trap mass measurements with SHIPTRAP to the heaviest elements

    International Nuclear Information System (INIS)

    Block, M.; Ackermann, D.; Herfurth, F.; Hofmann, S.; Blaum, K.; Droese, C.; Marx, G.; Schweikhard, L.; Düllmann, Ch. E.; Eibach, M.; Eliseev, S.; Haettner, E.; Plaß, W. R.; Scheidenberger, C.; Heßberger, F. P.; Ramirez, E. Minaya; Nesterenko, D.

    2013-01-01

    Penning-trap mass spectrometry of radionuclides provides accurate mass values and absolute binding energies. Such mass measurements are sensitive indicators of the nuclear structure evolution far away from stability. Recently, direct mass measurements have been extended to the heavy elements nobelium (Z=102) and lawrencium (Z=103) with the Penning-trap mass spectrometer SHIPTRAP. The results probe nuclear shell effects at N=152. New developments will pave the way to access even heavier nuclides.

  4. Incorporating Biological Mass Spectrometry into Undergraduate Teaching Labs, Part 2: Peptide Identification via Molecular Mass Determination

    Science.gov (United States)

    Arnquist, Isaac J.; Beussman, Douglas J.

    2009-01-01

    Mass spectrometry has become a routine analytical tool in the undergraduate curriculum in the form of GC-MS. While relatively few undergraduate programs have incorporated biological mass spectrometry into their programs, the importance of these techniques, as demonstrated by their recognition with the 2002 Nobel Prize, will hopefully lead to…

  5. Data recording and processing in mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    McKown, H. [International Atomic Energy Agency, Vienna (Austria)

    1978-12-15

    When a mass spectrometer is going to be obtained, it must be specified to do a particular task. It follows that the data recording system must be designed to work satisfactorily with hardware that produces the ion current or currents. The author describes two systems: the AVCO mass spectrometer and the tandem mass spectrometer.

  6. Mass spectrometry of stardust : experimental tests of nucleosynthesis

    International Nuclear Information System (INIS)

    Clayton, R.N.

    1997-01-01

    Primitive meteorites contain grains of diamond, graphite and silicon carbide which condensed from the outflows of red-giant stars, which existed before the formation of our Sun and Solar System. Nuclear processes within the parent star have modified the isotopic compositions of all elements in the grains. By means of a very sensitive and selective microanalytical technique, Resonant Ionization Mass Spectrometry, we can measure isotopic abundances of trace metals in individual 3-micrometer-sized crystals. The technique uses multi-photon photoionization with tuned lasers to ionize a single element selectively and efficiently. This allows isotopic measurements of trace constituents in complex systems. Results from zirconium and molybdenum in presolar silicon carbide grains show large enhancements in the s-process isotopes, and depletion by factors >2 in the r-process and p-process isotopes. The observations are in good agreement with recent calculations of s-process nucleosynthesis in Asymptotic Giant Branch stars. These results confirm the classical subdivision of nucleo-synthetic processes into p-, r-, and s-processes and show that the principal site of the s-process is in carbon-rich red giant stars. (author)

  7. ELEMENT MASSES IN THE CRAB NEBULA

    Energy Technology Data Exchange (ETDEWEB)

    Sibley, Adam R.; Katz, Andrea M.; Satterfield, Timothy J.; Vanderveer, Steven J.; MacAlpine, Gordon M. [Department of Physics and Astronomy, Trinity University, San Antonio, TX 78212 (United States)

    2016-10-01

    Using our previously published element abundance or mass-fraction distributions in the Crab Nebula, we derived actual mass distributions and estimates for overall nebular masses of hydrogen, helium, carbon, nitrogen, oxygen and sulfur. As with the previous work, computations were carried out for photoionization models involving constant hydrogen density and also constant nuclear density. In addition, employing new flux measurements for [Ni ii]  λ 7378, along with combined photoionization models and analytic computations, a nickel abundance distribution was mapped and a nebular stable nickel mass estimate was derived.

  8. Towards airborne nanoparticle mass spectrometry with nanomechanical string resonators

    DEFF Research Database (Denmark)

    Schmid, Silvan; Kurek, Maksymilian; Boisen, Anja

    2013-01-01

    airborne nanoparticle sensors. Recently, nanomechanical mass spectrometry was established. One of the biggest challenges of nanomechanical sensors is the low efficiency of diffusion-based sampling. We developed an inertial-based sampling method that enables the efficient sampling of airborne nanoparticles...... mode. Mass spectrometry of airborne nanoparticles requires the simultaneous operation in the first and second mode, which can be implemented in the transduction scheme of the resonator. The presented results lay the cornerstone for the realization of a portable airborne nanoparticle mass spectrometer....

  9. AM1 and electron impact mass spectrometry study of the ...

    African Journals Online (AJOL)

    Recently, in electron impact mass spectrometry (EIMS), it has been found a good correlation between the fragmentation processes of coumarins and the electronic charges of the atoms of their skeleton. In this paper, the same analytical method has been applied to 4-acyl isochroman-1,3-diones, whose mass spectra had ...

  10. A Review of the Emerging Field of Underwater Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Emily Chua

    2016-11-01

    Full Text Available Mass spectrometers are versatile sensor systems, owing to their high sensitivity and ability to simultaneously measure multiple chemical species. Over the last two decades, traditional laboratory-based membrane inlet mass spectrometers have been adapted for underwater use. Underwater mass spectrometry has drastically improved our capability to monitor a broad suite of gaseous compounds (e.g., dissolved atmospheric gases, light hydrocarbons, and volatile organic compounds in the aquatic environment. Here we provide an overview of the progress made in the field of underwater mass spectrometry since its inception in the 1990s to the present. In particular, we discuss the approaches undertaken by various research groups in developing in situ mass spectrometers. We also provide examples to illustrate how underwater mass spectrometers have been used in the field. Finally, we present future trends in the field of in situ mass spectrometry. Most of these efforts are aimed at improving the quality and spatial and temporal scales of chemical measurements in the ocean. By providing up-to-date information on underwater mass spectrometry, this review offers guidance for researchers interested in adapting this technology as well as goals for future progress in the field.

  11. Using the ion microprobe mass analyser for trace element analysis

    International Nuclear Information System (INIS)

    Schilling, J.H.

    1978-01-01

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

  12. Plutonium determination in urine by techniques of mass spectrometry

    International Nuclear Information System (INIS)

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

    2013-10-01

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

  13. Mass spectrometry in nuclear technology - a review of application of thermal ionization mass spectrometry in fuel reprocessing plants. PD-7-1

    International Nuclear Information System (INIS)

    Dakshinamoorthy, A.

    2007-01-01

    Mass spectrometry finds the widespread application in nuclear science and technology due to the fact that it can be employed for isotope composition measurements of different elements of interest and also concentration measurements of these elements using isotope dilution techniques. Thermal ionization mass spectrometer (TIMS), Inductively coupled plasma mass spectrometer (ICP-MS) and gas chromatography mass spectrometer (GC-MS) are the different types of mass spectrometers used in nuclear industry for the analyses of isotope composition of special nuclear material, trace impurities in nuclear fuels and components and characterization of various solvents respectively. Among them, TIMS plays a vital role in the nuclear fuel cycle in determining precisely the isotope composition of uranium, plutonium, D/H ratio in heavy water etc. TIMS is an indispensable analytical tool for nuclear material accounting at the input stage of a reprocessing plant by carrying out precise and accurate concentration measurement of plutonium and uranium by isotope dilution mass spectrometry (IDMS). It is the only accepted measurement technique for the purpose because of its high precision, better sensitivity and no quantitative separation is needed. The isotope abundance measurements of uranium and plutonium at this point are also useful for burn-up studies and isotope correlations. Mass spectrometric analysis of uranium and plutonium is also required for nuclear data measurements and calibrating other chemical methods

  14. Knudsen effusion mass spectrometry. Chapter 20

    International Nuclear Information System (INIS)

    Sai Baba, M.

    1997-01-01

    The Knudsen effusion mass spectrometric method for the determination of vapour pressures and thermodynamic properties is described. The aim of the article is to give a general introduction to the method rather than to give a critical review of the technique. The latest developments in this area of research are reviewed by the peers in the field during the triennial international mass spectrometric conferences. The Knudsen effusion mass spectrometric method is being applied for thermodynamic measurements. In recent times, laser vaporisation mass spectrometric methods have emerged as a source of determination of vapour pressures at very high temperatures and beyond the pressure regime far exceeding Knudsen effusion range

  15. Development of stereotactic mass spectrometry for brain tumor surgery.

    Science.gov (United States)

    Agar, Nathalie Y R; Golby, Alexandra J; Ligon, Keith L; Norton, Isaiah; Mohan, Vandana; Wiseman, Justin M; Tannenbaum, Allen; Jolesz, Ferenc A

    2011-02-01

    Surgery remains the first and most important treatment modality for the majority of solid tumors. Across a range of brain tumor types and grades, postoperative residual tumor has a great impact on prognosis. The principal challenge and objective of neurosurgical intervention is therefore to maximize tumor resection while minimizing the potential for neurological deficit by preserving critical tissue. To introduce the integration of desorption electrospray ionization mass spectrometry into surgery for in vivo molecular tissue characterization and intraoperative definition of tumor boundaries without systemic injection of contrast agents. Using a frameless stereotactic sampling approach and by integrating a 3-dimensional navigation system with an ultrasonic surgical probe, we obtained image-registered surgical specimens. The samples were analyzed with ambient desorption/ionization mass spectrometry and validated against standard histopathology. This new approach will enable neurosurgeons to detect tumor infiltration of the normal brain intraoperatively with mass spectrometry and to obtain spatially resolved molecular tissue characterization without any exogenous agent and with high sensitivity and specificity. Proof of concept is presented in using mass spectrometry intraoperatively for real-time measurement of molecular structure and using that tissue characterization method to detect tumor boundaries. Multiple sampling sites within the tumor mass were defined for a patient with a recurrent left frontal oligodendroglioma, World Health Organization grade II with chromosome 1p/19q codeletion, and mass spectrometry data indicated a correlation between lipid constitution and tumor cell prevalence. The mass spectrometry measurements reflect a complex molecular structure and are integrated with frameless stereotaxy and imaging, providing 3-dimensional molecular imaging without systemic injection of any agents, which can be implemented for surgical margins delineation of

  16. Optimal sample to tracer ratio for isotope dilution mass spectrometry: the polyisotopic case

    International Nuclear Information System (INIS)

    Laszlo, G.; Ridder, P. de; Goldman, A.; Cappis, J.; Bievre, P. de

    1991-01-01

    The Isotope Dilution Mass Spectrometry (IDMS) measurement technique provides a means for determining the unknown amount of various isotopes of an element in a sample solution of known mass. The sample solution is mixed with an auxiliary solution, or tracer, containing a known amount of the same element having the same isotopes but of different relative abundances or isotopic composition and the induced change in the isotopic composition measured by isotope mass spectrometry. The technique involves the measurement of the abundance ratio of each isotope to a (same) reference isotope in the sample solution, in the tracer solution and in the blend of the sample and tracer solution. These isotope ratio measurements, the known element amount in the tracer and the known mass of sample solution are used to calculate the unknown amount of one isotope in the sample solution. Subsequently the unknown amount of element is determined. The purpose of this paper is to examine the optimization of the ratio of the estimated unknown amount of element in the sample solution to the known amount of element in the tracer solution in order to minimize the relative uncertainty in the determination of the unknown amount of element

  17. Emerging mass spectrometry techniques for the direct analysis of microbial colonies

    OpenAIRE

    Fang, Jinshu; Dorrestein, Pieter C.

    2014-01-01

    One of the emerging areas in microbiology is detecting specialized metabolites produced by microbial colonies and communities with mass spectrometry. In this review/perspective, we illustrate the emerging mass spectrometry methodologies that enable the interrogation of specialized metabolites directly from microbial colonies. Mass spectrometry techniques such as imaging mass spectrometry and real-time mass spectrometry allow two and three dimensional visualization of the distri...

  18. The matrix effect in secondary ion mass spectrometry

    Science.gov (United States)

    Seah, M. P.; Shard, A. G.

    2018-05-01

    Matrix effects in the secondary ion mass spectrometry (SIMS) of selected elemental systems have been analyzed to investigate the applicability of a mathematical description of the matrix effect, called here the charge transfer (CT) model. This model was originally derived for proton exchange and organic positive secondary ions, to characterise the enhancement or suppression of intensities in organic binary systems. In the systems considered in this paper protons are specifically excluded, which enables an assessment of whether the model applies for electrons as well. The present importance is in organic systems but, here we analyse simpler inorganic systems. Matrix effects in elemental systems cannot involve proton transfer if there are no protons present but may be caused by electron transfer and so electron transfer may also be involved in the matrix effects for organic systems. There are general similarities in both the magnitudes of the ion intensities as well as the matrix effects for both positive and negative secondary ions in both systems and so the CT model may be more widely applicable. Published SIMS analyses of binary elemental mixtures are analyzed. The data of Kim et al., for the Pt/Co system, provide, with good precision, data for such a system. This gives evidence for the applicability of the CT model, where electron, rather than proton, transfer is the matrix enhancing and suppressing mechanism. The published data of Prudon et al., for the important Si/Ge system, provides further evidence for the effects for both positive and negative secondary ions and allows rudimentary rules to be developed for the enhancing and suppressing species.

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  20. Mass Spectrometry Imaging of Drugs of Abuse in Hair.

    Science.gov (United States)

    Flinders, Bryn; Cuypers, Eva; Porta, Tiffany; Varesio, Emmanuel; Hopfgartner, Gérard; Heeren, Ron M A

    2017-01-01

    Hair testing is a powerful tool routinely used for the detection of drugs of abuse. The analysis of hair is highly advantageous as it can provide prolonged drug detectability versus that in biological fluids and chronological information about drug intake based on the average growth of hair. However, current methodology requires large amounts of hair samples and involves complex time-consuming sample preparation followed by gas or liquid chromatography coupled with mass spectrometry. Mass spectrometry imaging is increasingly being used for the analysis of single hair samples, as it provides more accurate and visual chronological information in single hair samples.Here, two methods for the preparation of single hair samples for mass spectrometry imaging are presented.The first uses an in-house built cutting apparatus to prepare longitudinal sections, the second is a method for embedding and cryo-sectioning hair samples in order to prepare cross-sections all along the hair sample.

  1. Proceedings of twelfth ISMAS symposium cum workshop on mass spectrometry

    International Nuclear Information System (INIS)

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

    2007-03-01

    Mass Spectrometry is an important analytical tool and has encompassed almost all branches of science and technology including Agricultural, biology, Chemistry, Earth sciences, environment, Forensic Science, Medical Sciences, Hydrology, Nuclear Technology, Oceanography, Physics etc. Recent advancements in the instrumentation of Mass Spectrometry have further strengthened its role for various applications. It is indeed a matter of great pleasure to present this special Issue of ISMAS Bulletin which is brought out on the occasion of the 12th ISMAS Symposium cum Workshop on Mass spectrometry (12th ISMAS-WS 2007) being held at Cidade-de-Goa, Dona Paula, Goa from March 25 to 30, 2007 in association with National Institute of Oceanography, Goa. This Symposium cum Workshop is co-sponsored by Scientific Departments of Government of India. Papers relevant to INIS are indexed separately

  2. High efficiency nebulization for helium inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Jorabchi, Kaveh; McCormick, Ryan; Levine, Jonathan A.; Liu Huiying; Nam, S.-H.; Montaser, Akbar

    2006-01-01

    A pneumatically-driven, high efficiency nebulizer is explored for helium inductively coupled plasma mass spectrometry. The aerosol characteristics and analyte transport efficiencies of the high efficiency nebulizer for nebulization with helium are measured and compared to the results obtained with argon. Analytical performance indices of the helium inductively coupled plasma mass spectrometry are evaluated in terms of detection limits and precision. The helium inductively coupled plasma mass spectrometry detection limits obtained with the high efficiency nebulizer at 200 μL/min are higher than those achieved with the ultrasonic nebulizer consuming 2 mL/min solution, however, precision is generally better with high efficiency nebulizer (1-4% vs. 3-8% with ultrasonic nebulizer). Detection limits with the high efficiency nebulizer at 200 μL/min solution uptake rate approach those using ultrasonic nebulizer upon efficient desolvation with a heated spray chamber followed by a Peltier-cooled multipass condenser

  3. Laser desorption mass spectrometry for biomolecule detection and its applications

    Science.gov (United States)

    Winston Chen, C. H.; Sammartano, L. J.; Isola, N. R.; Allman, S. L.

    2001-08-01

    During the past few years, we developed and used laser desorption mass spectrometry for biomolecule detections. Matrix-assisted laser desorption/ionization (MALDI) was successfully used to detect DNA fragments with the size larger than 3000 base pairs. It was also successfully used to sequence DNA with both enzymatic and chemical degradation methods to produce DNA ladders. We also developed MALDI with fragmentation for direct DNA sequencing for short DNA probes. Since laser desorption mass spectrometry for DNA detection has the advantages of fast speed and no need of labeling, it has a great potential for molecular diagnosis for disease and person identification by DNA fingerprinting. We applied laser desorption mass spectrometry to succeed in the diagnosis of cystic fibrosis and several other nerve degenerative diseases such as Huntington's disease. We also succeeded in demonstrating DNA typing for forensic applications.

  4. Laser desorption mass spectrometry for biomolecule detection and its applications

    International Nuclear Information System (INIS)

    Winston Chen, C.H.; Allman, S.L.; Sammartano, L.J.; Isola, N.R.

    2001-01-01

    During the past few years, we developed and used laser desorption mass spectrometry for biomolecule detections. Matrix-assisted laser desorption/ionization (MALDI) was successfully used to detect DNA fragments with the size larger than 3000 base pairs. It was also successfully used to sequence DNA with both enzymatic and chemical degradation methods to produce DNA ladders. We also developed MALDI with fragmentation for direct DNA sequencing for short DNA probes. Since laser desorption mass spectrometry for DNA detection has the advantages of fast speed and no need of labeling, it has a great potential for molecular diagnosis for disease and person identification by DNA fingerprinting. We applied laser desorption mass spectrometry to succeed in the diagnosis of cystic fibrosis and several other nerve degenerative diseases such as Huntington's disease. We also succeeded in demonstrating DNA typing for forensic applications

  5. Accelerator mass spectrometry-current status in techniques and applications

    International Nuclear Information System (INIS)

    Imamura, Mineo; Nagai, Hisao; Kobayashi, Koichi.

    1991-01-01

    Accelerator mass spectrometry (AMS) is the mass spectrometry by incorporating an accelerator. After samples are ionized, they are accelerated to a certain energy, and mass, energy, nuclear charge (atomic number) are distinguished, and ion counting is made one by one with a heavy ion detector. For the measurement of long half-life radioisotopes, mass spectrometry has been used because of the high sensitivity, but in low energy mass spectrometry, there are the difficulties due to the mixing of the molecular ions having nearly same mass and the existence of isobars. One of the methods solving these difficulties is an accelerator which enables background-free measurement. The progress of AMS is briefly described, and at present, it is carried out in about 30 facilities in the world. In AMS, the analysis is carried out in the order of the ionization of samples, the acceleration of beam, the electron stripping with a thin film, the sorting of the momentum and energy of beam and the identification of particles. The efficiency, sensitivity and accuracy of detection and the application are reported. (K.I.)

  6. Structural analyses of sucrose laurate regioisomers by mass spectrometry techniques

    DEFF Research Database (Denmark)

    Lie, Aleksander; Stensballe, Allan; Pedersen, Lars Haastrup

    2015-01-01

    6- And 6′-O-lauroyl sucrose were isolated and analyzed by matrix-assisted laser desorption/ionisation (MALDI) time-of-flight (TOF) mass spectrometry (MS), Orbitrap high-resolution (HR) MS, and electrospray-ionization (ESI) tandem mass spectrometry (MS/MS). The analyses aimed to explore the physic......6- And 6′-O-lauroyl sucrose were isolated and analyzed by matrix-assisted laser desorption/ionisation (MALDI) time-of-flight (TOF) mass spectrometry (MS), Orbitrap high-resolution (HR) MS, and electrospray-ionization (ESI) tandem mass spectrometry (MS/MS). The analyses aimed to explore.......8, respectively, and Orbitrap HRMS confirmed the mass of [M+Na]+ (m/z 547.2712). ESI-MS/MS on the precursor ion [M+Na]+ resulted in product ion mass spectra showing two high-intensity signals for each sample. 6-O-Lauroyl sucrose produced signals located at m/z 547.27 and m/z 385.21, corresponding to the 6-O...

  7. Application of secondary ions mass spectrometry (SIMS) in studies of internal contamination

    International Nuclear Information System (INIS)

    Amaral, Ademir; Galle, Pierre; Colas-Linhart, Nicole

    2000-01-01

    Secondary Ion Mass Spectrometry (SIMS) permits the detection of stable and radioactive nuclides. Based on the ablation of specimens by ion bombardment this mass spectrometry method allows a rapid assessment of trace elements in biological samples. Its resolving mass power provides an efficient analytical method and, in particular, it makes possible accurate isotopic ratio determination. In this work, the application of SIMS has been investigated in studies of internal contamination. In vivo studies were carried out using duodenal tissue sections from rats contaminated with cerium. Tests were performed to localize this element as a result of the contamination. In this report, analytical procedures and the potential of SIMS in biological research are presented and discussed. (author)

  8. Radiogas chromatography mass spectrometry in the selected ion monitoring mode

    International Nuclear Information System (INIS)

    Doerfler, D.L.; Rosenblum, E.R.; Malloy, J.M.; Naworal, J.D.; McManus, I.R.; Campbell, I.M.

    1980-01-01

    The value of selected ion monitoring in analyzing biological radio isotope incorporation experiments by radiogas chromatography mass spectrometry is illustrated with reference to the biosynthesis of the mycotoxin mycophenolic acid in Penicillium brevicompactum and the mode of action of the anticholesterolemic drug 20,25-diazacholesterol. Both examples used 1-[ 14 C]acetate precursors. It is shown that the increased sensitivity and specificity of the selected ion monitoring mode detector permits straightforward detection and identification of the relatively small cellular pools associated with metabolic intermediates. The computer program RADSIM is described. Problems that still exist in using radiogas gas chromatography mass spectrometry technology to analyse isotope incorporation experiments are discussed. (author)

  9. Analysis of chirality by femtosecond laser ionization mass spectrometry.

    Science.gov (United States)

    Horsch, Philipp; Urbasch, Gunter; Weitzel, Karl-Michael

    2012-09-01

    Recent progress in the field of chirality analysis employing laser ionization mass spectrometry is reviewed. Emphasis is given to femtosecond (fs) laser ionization work from the author's group. We begin by reviewing fundamental aspects of determining circular dichroism (CD) in fs-laser ionization mass spectrometry (fs-LIMS) discussing an example from the literature (resonant fs-LIMS of 3-methylcyclopentanone). Second, we present new data indicating CD in non-resonant fs-LIMS of propylene oxide. Copyright © 2012 Wiley Periodicals, Inc., A Wiley Company.

  10. Native Mass Spectrometry in Fragment-Based Drug Discovery.

    Science.gov (United States)

    Pedro, Liliana; Quinn, Ronald J

    2016-07-28

    The advent of native mass spectrometry (MS) in 1990 led to the development of new mass spectrometry instrumentation and methodologies for the analysis of noncovalent protein-ligand complexes. Native MS has matured to become a fast, simple, highly sensitive and automatable technique with well-established utility for fragment-based drug discovery (FBDD). Native MS has the capability to directly detect weak ligand binding to proteins, to determine stoichiometry, relative or absolute binding affinities and specificities. Native MS can be used to delineate ligand-binding sites, to elucidate mechanisms of cooperativity and to study the thermodynamics of binding. This review highlights key attributes of native MS for FBDD campaigns.

  11. Quantitating subcellular metabolism with multi-isotope imaging mass spectrometry

    OpenAIRE

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

    2012-01-01

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

  12. Major roles for minor bacterial lipids identified by mass spectrometry.

    Science.gov (United States)

    Garrett, Teresa A

    2017-11-01

    Mass spectrometry of lipids, especially those isolated from bacteria, has ballooned over the past two decades, affirming in the process the complexity of the lipidome. With this has come the identification of new and interesting lipid structures. Here is an overview of several novel lipids, from both Gram-negative and Gram-positive bacteria with roles in health and disease, whose structural identification was facilitated using mass spectrometry. This article is part of a Special Issue entitled: Bacterial Lipids edited by Russell E. Bishop. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Identifying modifications in RNA by MALDI mass spectrometry

    DEFF Research Database (Denmark)

    Douthwaite, Stephen; Kirpekar, Finn

    2007-01-01

    as RNA modifications added in cell-free in vitro systems. MALDI-MS is particularly useful in cases in which other techniques such as those involving primer extension or chromatographic analyses are not practicable. To date, MALDI-MS has been used to localize rRNA modifications that are involved......Posttranscriptional modifications on the base or sugar of ribonucleosides generally result in mass increases that can be measured by mass spectrometry. Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) is a direct and accurate means of determining the masses of RNAs. Mass...... spectra produced by MALDI are relatively straightforward to interpret, because they are dominated by singly charged ions, making it possible to analyze complex mixtures of RNA oligonucleotides ranging from trinucleotides up to 20-mers. Analysis of modifications within much longer RNAs, such as ribosomal...

  14. Current use of high-resolution mass spectrometry in drug screening relevant to clinical and forensic toxicology and doping control.

    Science.gov (United States)

    Ojanperä, Ilkka; Kolmonen, Marjo; Pelander, Anna

    2012-05-01

    Clinical and forensic toxicology and doping control deal with hundreds or thousands of drugs that may cause poisoning or are abused, are illicit, or are prohibited in sports. Rapid and reliable screening for all these compounds of different chemical and pharmaceutical nature, preferably in a single analytical method, is a substantial effort for analytical toxicologists. Combined chromatography-mass spectrometry techniques with standardised reference libraries have been most commonly used for the purpose. In the last ten years, the focus has shifted from gas chromatography-mass spectrometry to liquid chromatography-mass spectrometry, because of progress in instrument technology and partly because of the polarity and low volatility of many new relevant substances. High-resolution mass spectrometry (HRMS), which enables accurate mass measurement at high resolving power, has recently evolved to the stage that is rapidly causing a shift from unit-resolution, quadrupole-dominated instrumentation. The main HRMS techniques today are time-of-flight mass spectrometry and Orbitrap Fourier-transform mass spectrometry. Both techniques enable a range of different drug-screening strategies that essentially rely on measuring a compound's or a fragment's mass with sufficiently high accuracy that its elemental composition can be determined directly. Accurate mass and isotopic pattern acts as a filter for confirming the identity of a compound or even identification of an unknown. High mass resolution is essential for improving confidence in accurate mass results in the analysis of complex biological samples. This review discusses recent applications of HRMS in analytical toxicology.

  15. Mass Spectrometry Imaging, an Emerging Technology in Neuropsychopharmacology

    Science.gov (United States)

    Shariatgorji, Mohammadreza; Svenningsson, Per; Andrén, Per E

    2014-01-01

    Mass spectrometry imaging is a powerful tool for directly determining the distribution of proteins, peptides, lipids, neurotransmitters, metabolites and drugs in neural tissue sections in situ. Molecule-specific imaging can be achieved using various ionization techniques that are suited to different applications but which all yield data with high mass accuracies and spatial resolutions. The ability to simultaneously obtain images showing the distributions of chemical species ranging from metal ions to macromolecules makes it possible to explore the chemical organization of a sample and to correlate the results obtained with specific anatomical features. The imaging of biomolecules has provided new insights into multiple neurological diseases, including Parkinson's and Alzheimer's disease. Mass spectrometry imaging can also be used in conjunction with other imaging techniques in order to identify correlations between changes in the distribution of important chemical species and other changes in the properties of the tissue. Here we review the applications of mass spectrometry imaging in neuroscience research and discuss its potential. The results presented demonstrate that mass spectrometry imaging is a useful experimental method with diverse applications in neuroscience. PMID:23966069

  16. Mass spectrometry imaging, an emerging technology in neuropsychopharmacology.

    Science.gov (United States)

    Shariatgorji, Mohammadreza; Svenningsson, Per; Andrén, Per E

    2014-01-01

    Mass spectrometry imaging is a powerful tool for directly determining the distribution of proteins, peptides, lipids, neurotransmitters, metabolites and drugs in neural tissue sections in situ. Molecule-specific imaging can be achieved using various ionization techniques that are suited to different applications but which all yield data with high mass accuracies and spatial resolutions. The ability to simultaneously obtain images showing the distributions of chemical species ranging from metal ions to macromolecules makes it possible to explore the chemical organization of a sample and to correlate the results obtained with specific anatomical features. The imaging of biomolecules has provided new insights into multiple neurological diseases, including Parkinson's and Alzheimer's disease. Mass spectrometry imaging can also be used in conjunction with other imaging techniques in order to identify correlations between changes in the distribution of important chemical species and other changes in the properties of the tissue. Here we review the applications of mass spectrometry imaging in neuroscience research and discuss its potential. The results presented demonstrate that mass spectrometry imaging is a useful experimental method with diverse applications in neuroscience.

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

  18. Ion source memory in {sup 36}Cl accelerator mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Pavetich, Stefan; Akhmadaliev, Shavkat; Merchel, Silke; Rugel, Georg [HZDR, Dresden (Germany); Arnold, Maurice; Aumaitre, Georges; Bourles, Didier; Martschini, Martin [ASTER, Aix-en-Provence (France); Buchriegler, Josef; Golser, Robin; Keddadouche, Karim; Steier, Peter [VERA, Vienna (Austria)

    2013-07-01

    Since the DREAMS (Dresden Accelerator Mass Spectrometry) facility went operational in 2011, constant effort was put into enabling routine measurements of long-lived radionuclides as {sup 10}Be, {sup 26}Al and {sup 41}Ca. For precise AMS-measurements of the volatile element Cl the key issue is the minimization of the long term memory effect. For this purpose one of the two original HVE sources was mechanically modified, allowing the usage of bigger cathodes with individual target apertures. Additionally a more open geometry was used to improve the vacuum level. To evaluate this improvement in comparison to other up-to-date ion sources, a small inter-laboratory comparison had been initiated. The long-term memory effect in the Cs sputter ion sources of the AMS facilities VERA, ASTER and DREAMS had been investigated by running samples of natural {sup 35}Cl/{sup 37}Cl-ratio and samples containing highly enriched {sup 35}Cl({sup 35}Cl/{sup 37}Cl > 500). Primary goals of the research are the time constants of the recovery from the contaminated sample ratio to the initial ratio of the sample and the level of the long-term memory effect in the sources.

  19. Principles of isotopic analysis by mass spectrometry

    International Nuclear Information System (INIS)

    Herrmann, M.

    1980-01-01

    The use of magnetic sector field mass spectrometers in isotopic analysis, especially for nitrogen gas, is outlined. Two measuring methods are pointed out: the scanning mode for significantly enriched samples and the double collector method for samples near the natural abundance of 15 N. The calculation formulas are derived and advice is given for corrections. (author)

  20. A New Accelerator-Based Mass Spectrometry.

    Science.gov (United States)

    Gove, H. E.

    1983-01-01

    Tandem electrostatic accelerators produce beams of positive ions which are used to penetrate atomic nuclei in a target, inducing nuclear reactions whose study elucidates varied properties of the nucleus. Uses of the system, which acts like a mass spectrometer, are discussed. These include radiocarbon dating measurements. (JN)

  1. Characterizing the lipid and metabolite changes associated with placental function and pregnancy complications using ion mobility spectrometry-mass spectrometry and mass spectrometry imaging

    Energy Technology Data Exchange (ETDEWEB)

    Burnum-Johnson, Kristin E.; Baker, Erin S.; Metz, Thomas O.

    2017-12-01

    Successful pregnancy is dependent upon discrete biological events, which include embryo implantation, decidualization, and placentation. Problems associated with each of these events can cause infertility or conditions such as preeclampsia. A greater understanding of the molecular changes associated with these complex processes is necessary to aid in identifying treatments for each condition. Previous nuclear magnetic resonance spectroscopy and mass spectrometry studies have been used to identify metabolites and lipids associated with pregnancy-related complications. However, due to limitations associated with conventional implementations of both techniques, novel technology developments are needed to more fully understand the initiation and development of pregnancy related problems at the molecular level. In this perspective, we describe current analytical techniques for metabolomic and lipidomic characterization of pregnancy complications and discuss the potential for new technologies such as ion mobility spectrometry-mass spectrometry and mass spectrometry imaging to contribute to a better understanding of the molecular changes that affect the placenta and pregnancy outcomes.

  2. Ion Mobility Mass Spectrometry Direct Isotope Abundance Analysis

    International Nuclear Information System (INIS)

    Manard, Manuel J.; Weeks, Stephan; Kyle, Kevin

    2010-01-01

    The nuclear forensics community is currently engaged in the analysis of illicit nuclear or radioactive material for the purposes of non-proliferations and attribution. One technique commonly employed for gathering nuclear forensics information is isotope analysis. At present, the state-of-the-art methodology for obtaining isotopic distributions is thermal ionization mass spectrometry (TIMS). Although TIMS is highly accurate at determining isotope distributions, the technique requires an elementally pure sample to perform the measurement. The required radiochemical separations give rise to sample preparation times that can be in excess of one to two weeks. Clearly, the nuclear forensics community is in need of instrumentation and methods that can expedite their decision making process in the event of a radiological release or nuclear detonation. Accordingly, we are developing instrumentation that couples a high resolution IM drift cell to the front end of a MS. The IM cell provides a means of separating ions based upon their collision cross-section and mass-to-charge ratio (m/z). Two analytes with the same m/z, but with different collision cross-sections (shapes) would exit the cell at different times, essentially enabling the cell to function in a similar manner to a gas chromatography (GC) column. Thus, molecular and atomic isobaric interferences can be effectively removed from the ion beam. The mobility selected chemical species could then be introduced to a MS for high-resolution mass analysis to generate isotopic distributions of the target analytes. The outcome would be an IM/MS system capable of accurately measuring isotopic distributions while concurrently eliminating isobaric interferences and laboratory radiochemical sample preparation. The overall objective of this project is developing instrumentation and methods to produce near real-time isotope distributions with a modular mass spectrometric system that performs the required gas-phase chemistry and

  3. Trace amount analysis using spark mass spectrometry

    International Nuclear Information System (INIS)

    Stefani, Rene

    1975-01-01

    Characteristics of spark mass spectrometers (ion source, properties of the ion beam, ion optics, and performance) and their use in qualitative and quantitative analysis are described. This technique is very interesting for the semi-quantitative analysis of trace amounts, down to 10 -8 atoms. Examples of applications such as the analysis of high purity materials and non-conducting mineral samples, and determination of carbon and gas trace amounts are presented. (50 references) [fr

  4. Hydrogen isotope analysis by quadrupole mass spectrometry

    International Nuclear Information System (INIS)

    Ellefson, R.E.; Moddeman, W.E.; Dylla, H.F.

    1981-03-01

    The analysis of isotopes of hydrogen (H, D, T) and helium ( 3 He, 4 He) and selected impurities using a quadrupole mass spectrometer (QMS) has been investigated as a method of measuring the purity of tritium gas for injection into the Tokamak Fusion Test Reactor (TFTR). A QMS was used at low resolution, m/Δm 3 He, and 4 He in HT/D 2

  5. Total evaporation in thermal ionization mass spectrometry

    International Nuclear Information System (INIS)

    Callis, E.L.; Cappis, J.H.

    1996-01-01

    Experiments were conducted to assess the effects of impurities on the total evaporation method for mass spectrometric measurement of the isotope ratio of uranium. Standard samples were spiked with Na, Ca, Fe, Zr and Ba. The results indicated that only Fe, and possible Na, displayed any interference, and then only at high concentrations. One problem limiting the accuracy of the method is the determination of the relative efficiency of the collectors in the multicollector system. 3 refs., 1 tab

  6. Radio-tracing 'without' radioactivity: accelerator mass spectrometry in biomedicine

    International Nuclear Information System (INIS)

    Vogel, J.S.

    2005-01-01

    Accelerator mass spectrometry (AMS) is a form of isotope-ratio mass spectrometry that quantifies concentrations of certain long-lived radioisotopes independently of their radioactive decay. AMS is primarily used in the geosciences for determining the age of a material that contains naturally occurring radioisotopes. AMS uses the same high specificity for enriched levels of these radioisotopes in tracing low chemical doses for long periods in biological systems, including humans. AMS provides the safety of low radiative exposure to experimental subjects and investigators, while obtaining attomole sensitivities that are not possible with stable isotope tracers because of their natural isotopic abundances. AMS isotope tracing was first applied to quantifying the genotoxicity of low level environmental chemicals in animals and later in humans. Physiologic concentrations of 14 C-labeled trace nutrients (folate, carotene, and tocopherol) are now measured directly in humans without concern about radiation. The radiative exposure is less than the commonly accepted risks of natural background radiation or the radiation fields found in high altitude air flights. AMS measures very small biological samples (such as 20 microliters of blood) that are easily obtained from human volunteers or model animals at frequent intervals for detailed analysis of kinetic profiles. This high data density enables the construction of compartmental models that elucidate nutrient behavior in tissues that cannot be directly sampled. The pharmaceutical industry is enthusiastic about AMS as a detector for 'micro-dosing' in which the human kinetics of an assuredly non-toxic dose of a candidate drug is tested early in a development project. Molecular tracing uses 3 H or 14 C as common isotopic labels, but AMS contributes to elemental tracing with certain radioisotopes having very long lives, such as 26 AL or 41 Ca. Calcium-41 is a particularly useful isotope in biomedical research because it is used

  7. Calcium Isotope Analysis by Mass Spectrometry

    Science.gov (United States)

    Boulyga, S.; Richter, S.

    2010-12-01

    The variations in the isotopic composition of calcium caused by fractionation in heterogeneous systems and by nuclear reactions can provide insight into numerous biological, geological, and cosmic processes, and therefore isotopic analysis finds a wide spectrum of applications in cosmo- and geochemistry, paleoclimatic, nutritional, and biomedical studies. The measurement of calcium isotopic abundances in natural samples has challenged the analysts for more than three decades. Practically all Ca isotopes suffer from significant isobaric interferences, whereas low-abundant isotopes can be particularly affected by neighboring major isotopes. The extent of natural variations of stable isotopes appears to be relatively limited, and highly precise techniques are required to resolve isotopic effects. Isotope fractionation during sample preparation and measurements and instrumental mass bias can significantly exceed small isotope abundance variations in samples, which have to be investigated. Not surprisingly, a TIMS procedure developed by Russell et al. (Russell et al., 1978. Geochim Cosmochim Acta 42: 1075-1090) for Ca isotope measurements was considered as revolutionary for isotopic measurements in general, and that approach is used nowadays (with small modifications) for practically all isotopic systems and with different mass spectrometric techniques. Nevertheless, despite several decades of calcium research and corresponding development of mass spectrometers, the available precision and accuracy is still not always sufficient to achieve the challenging goals. This presentation discusses figures of merits of presently used analytical methods and instrumentation, and attempts to critically assess their limitations. Additionally, the availability of Ca isotope reference materials will be discussed.

  8. Statistical design of mass spectrometry calibration procedures

    International Nuclear Information System (INIS)

    Bayne, C.K.

    1996-11-01

    The main objective of this task was to agree on calibration procedures to estimate the system parameters (i.e., dead-time correction, ion-counting conversion efficiency, and detector efficiency factors) for SAL's new Finnigan MAT-262 mass spectrometer. SAL will use this mass spectrometer in a clean-laboratory which was opened in December 1995 to measure uranium and plutonium isotopes on environmental samples. The Finnigan MAT-262 mass spectrometer has a multi-detector system with seven Faraday cup detectors and one ion- counter for the measurement of very small signals (e.g. 10 -17 Ampere range). ORNL has made preliminary estimates of the system parameters based on SAL's experimental data measured in late 1994 when the Finnigan instrument was relatively new. SAL generated additional data in 1995 to verify the calibration procedures for estimating the dead-time correction factor, the ion-counting conversion factor and the Faraday cup detector efficiency factors. The system parameters estimated on the present data will have to be reestablished when the Finnigan MAT-262 is moved-to the new clean- laboratory. Different methods will be used to analyzed environmental samples than the current measurement methods being used. For example, the environmental samples will be electroplated on a single filament rather than using the current two filament system. An outline of the calibration standard operating procedure (SOP) is included

  9. Absorption Mode FT-ICR Mass Spectrometry Imaging

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Donald F.; Kilgour, David P.; Konijnenburg, Marco; O' Connor, Peter B.; Heeren, Ronald M.

    2013-12-03

    Fourier transform ion cyclotron resonance mass spectrometry offers the highest mass resolving power for molecular imaging experiments. This high mass resolving power ensures that closely spaced peaks at the same nominal mass are resolved for proper image generation. Typically higher magnetic fields are used to increase mass resolving power. However, a gain in mass resolving power can also be realized by phase correction of the data for absorption mode display. In addition to mass resolving power, absorption mode offers higher mass accuracy and signal-to-noise ratio over the conventional magnitude mode. Here we present the first use of absorption mode for Fourier transform ion cyclotron resonance mass spectrometry imaging. The Autophaser algorithm is used to phase correct each spectrum (pixel) in the image and then these parameters are used by the Chameleon work-flow based data processing software to generate absorption mode ?Datacubes? for image and spectral viewing. Absorption mode reveals new mass and spatial features that are not resolved in magnitude mode and results in improved selected ion image contrast.

  10. Inductively-coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Dale, L.

    1990-01-01

    The instrument in operation at the Lucas Heights Research Laboratories is a VG Plasma-quad PQ 2. A schematic diagram of the instrument components is presented along with its applicability to various fields of research and its perceived limitations. Apart from its high sensitivity the capability for rapid multi-element analysis in one of its major advantages over other instrumental method analysis. The necessity to present the sample in the form of a solution is probably its major drawback. 4 tabs, 7 figs

  11. Accelerator mass spectrometry - accomplishments and challenges

    International Nuclear Information System (INIS)

    Elmore, David

    2002-01-01

    Full text: AMS techniques and applications have advanced significantly since the first radiocarbon measurements in 1977. The list of nuclides in routine use includes 10 Be, 14 C, 26 Al, 36 Cl, 41 Ca, and 129 I. Cosmogenic radionuclides now have important applications in the study of earth surface processes and events. Recent biomedical studies include tracing aluminum as a toxic element and as an adjuvant in vaccines, radiocarbon as a tracer for tissue implants, and calcium loss from bones. Improvements in AMS performance for these and new nuclides result from automation, better ion sources, higher energies, and better isobar separation techniques

  12. The combined measurement of uranium by alpha spectrometry and secondary ion mass spectrometry (SIMS)

    International Nuclear Information System (INIS)

    Harvan, D.

    2009-01-01

    The aim of thesis was to found the dependence between radiometric method - alpha spectrometry and surface sensitive method - Secondary Ion Mass Spectrometry (SIMS). Uranium or naturally occurring uranium isotopes were studied. Samples (high polished stainless steel discs) with uranium isotopes were prepared by electrodeposition. Samples were measured by alpha spectrometry after electrodeposition and treatment. It gives surface activities. Weights, as well as surface's weights of uranium isotopes were calculated from their activities, After alpha spectrometry samples were analyzed by TOF-SIMS IV instrument in International Laser Centre in Bratislava. By the SIMS analysis intensities of uranium-238 were obtained. The interpretation of SIMS intensities vs. surface activity, or surface's weights of uranium isotopes indicates the possibility to use SIMS in quantitative analysis of surface contamination by uranium isotopes, especially 238 U. (author)

  13. Specialized Gas Chromatography--Mass Spectrometry Systems for Clinical Chemistry.

    Science.gov (United States)

    Gochman, Nathan; And Others

    1979-01-01

    A discussion of the basic design and characteristics of gas chromatography-mass spectrometry systems used in clinical chemistry. A comparison of three specific systems: the Vitek Olfax IIA, Hewlett-Packard HP5992, and Du Pont DP-102 are included. (BB)

  14. Role of mass spectrometry in nuclear forensic science

    International Nuclear Information System (INIS)

    Joseph, M.; Sivaraman, N.

    2016-01-01

    The present talk will focus on the role of mass spectrometry in NFS in general; besides that, the various chromatographic methods developed towards separation of actinides and lanthanide fission products and characterization of dissolver solutions of nuclear reactor fuels using TIMS and some applications of using ICP-MS as well

  15. Identification of Secreted Candida Proteins Using Mass Spectrometry

    NARCIS (Netherlands)

    Gómez-Molero, E.; Dekker, H.L.; de Boer, A.D.; de Groot, P.W.; Calderone, R.; Cihlar, R.

    2016-01-01

    Analysis of fungal secretomes using mass spectrometry is a useful technique in cell biology. Knowledge of the secretome of a human fungal pathogen may yield important information of host-pathogen interactions and may be useful for identifying vaccines candidates or diagnostic markers for antifungal

  16. On-Line Synthesis and Analysis by Mass Spectrometry

    Science.gov (United States)

    Bain, Ryan M.; Pulliam, Christopher J.; Raab, Shannon A.; Cooks, R. Graham

    2015-01-01

    In this laboratory experiment, students learn how to use ESI to accelerate chemical synthesis and to couple it with on-line mass spectrometry for structural analysis. The Hantzsch synthesis of symmetric 1,4-dihydropyridines is a classic example of a one-pot reaction in which multiple intermediates can serve to indicate the progress of the reaction…

  17. Biomedical applications of mass spectrometry. Clinical uses of stable isotopes

    International Nuclear Information System (INIS)

    Krahmer, U.I.; McCloskey, J.A.

    1978-01-01

    The review covers typical or important examples of stable isotope usage in clinical fields during the period since the last triennial mass spectrometry conference in 1973. Items are included which involve uses of stable isotopes in human or clinically oriented studies, including measurements carried out on materials of human origin. 163 references. (U.K.)

  18. Recent research and progress of laser mass spectrometry

    International Nuclear Information System (INIS)

    Li Jinying; Wang Fan; Zhao Yonggang; Xiao Guoping; Guo Dongfa; Cui Haiping

    2012-01-01

    The progress of laser mass spectrometry (LMS) was introduced. Its history and principle characteristics were reviewed. The research and applications of LMS in geology, mining, organics, biochemistry, environment and nuclear industry were given. The trend of LMS in the future was outlined, and the main issue and the available solutions were discussed. (authors)

  19. Advances in characterizing ubiquitylation sites by mass spectrometry

    DEFF Research Database (Denmark)

    Sylvestersen, K.B.; Young, C.; Nielsen, M.L.

    2013-01-01

    of ubiquitylation is a two-fold challenge that involves the mapping of ubiquitylation sites and the determination of ubiquitin chain topology. This review focuses on the technical advances in the mass spectrometry-based characterization of ubiquitylation sites, which have recently involved the large...

  20. The use of mass spectrometry in peptide chemistry

    NARCIS (Netherlands)

    Leclercq, P.A.; White, P.A.; Hägele, K.; Desiderio, D.M.; Meienhofer, J.

    1972-01-01

    A review with 16 refs. Methods are detailed for derivatizing peptides (mg quantities) in order to provide sufficient volatility for mass spectrometry (at least 10-5 mm vapor pressure at 300 Deg is required). Three steps are used in producing the desired derivs.: (a) arginine side chains are

  1. Gas chromatography mass spectrometry : key technology in metabolomics

    NARCIS (Netherlands)

    Koek, Maud Marijtje

    2009-01-01

    Metabolomics involves the unbiased quantitative and qualitative analysis of the complete set of metabolites present in cells, body fluids and tissues. Gas chromatography coupled to mass spectrometry (GC-MS) is very suitable for metabolomics analysis, as it combines high separation power with

  2. Fusion of mass spectrometry-based metabolomics data

    NARCIS (Netherlands)

    Smilde, Age K.; van der Werf, Mariët J.; Bijlsma, Sabina; van der Werff-van der Vat, Bianca J. C.; Jellema, Renger H.

    2005-01-01

    A general method is presented for combining mass spectrometry-based metabolomics data. Such data are becoming more and more abundant, and proper tools for fusing these types of data sets are needed. Fusion of metabolomics data leads to a comprehensive view on the metabolome of an organism or

  3. Discovery based and targeted Mass Spectrometry in farm animal proteomics

    DEFF Research Database (Denmark)

    Bendixen, Emøke

    2013-01-01

    for investigating farm animal biology. SRM is particularly important for validation biomarker candidates This talk will introduce the use of different mass spectrometry approaches through examples related to food quality and animal welfare, including studies of gut health in pigs, host pathogen interactions...

  4. Thermal ionisation mass spectrometry: recent developments and future prospects

    International Nuclear Information System (INIS)

    Aggarwal, S.K.

    1996-01-01

    This paper presents the current state of art of thermal ionization mass spectrometry (TIMS) instrumentation and highlights some of the recent applications of TIMS in geological, biological and nuclear sciences with special emphasis on some of the recent work undertaken in the area of nuclear science and technology. A few examples from the published literature are also discussed here

  5. Yeast expression proteomics by high-resolution mass spectrometry

    DEFF Research Database (Denmark)

    Walther, Tobias C; Olsen, Jesper Velgaard; Mann, Matthias

    2010-01-01

    -translational controls contribute majorly to regulation of protein abundance, for example in heat shock stress response. The development of new sample preparation methods, high-resolution mass spectrometry and novel bioinfomatic tools close this gap and allow the global quantitation of the yeast proteome under different...

  6. High-Performance Liquid Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Vestal, Marvin L.

    1984-01-01

    Reviews techniques for online coupling of high-performance liquid chromatography with mass spectrometry, emphasizing those suitable for application to nonvolatile samples. Also summarizes the present status, strengths, and weaknesses of various techniques and discusses potential applications of recently developed techniques for combined liquid…

  7. Mass Spectrometry Imaging for the Classification of Tumor Tissue

    NARCIS (Netherlands)

    Mascini, N.E.

    2016-01-01

    Mass spectrometry imaging (MSI) can detect and identify many different molecules without the need for labeling. In addition, it can provide their spatial distributions as ‘molecular maps’. These features make MSI well suited for studying the molecular makeup of tumor tissue. Currently, there is an

  8. Applications of accelerator mass spectrometry: advances and innovation

    International Nuclear Information System (INIS)

    Fifield, L.K.

    2004-01-01

    Emerging trends in the applications of accelerator mass spectrometry (AMS) are identified and illustrated with specific examples. Areas of application covered include rapid landscape evolution, calibration of the radiocarbon time scale, compound-specific radiocarbon studies, tracing of nuclear discharges, and searches for extraterrestrial isotopes

  9. Biomedical mass spectrometry in today's and tomorrow's clinical microbiology laboratories

    NARCIS (Netherlands)

    A.F. van Belkum (Alex); M. Welker (Martin); M. Erhard (Marcel); S. Chatellier (Sonia)

    2012-01-01

    textabstractClinical microbiology is a conservative laboratory exercise where base technologies introduced in the 19th century remained essentially unaltered. High-tech mass spectrometry (MS) has changed that. Within a few years following its adaptation to microbiological diagnostics, MS has been

  10. Capillary filling of miniaturized sources for electrospray mass spectrometry

    International Nuclear Information System (INIS)

    Arscott, Steve; Gaudet, Matthieu; Brinkmann, Martin; Ashcroft, Alison E; Blossey, Ralf

    2006-01-01

    Capillary slot-based emitter tips are a novel tool for use in electrospray ionization-mass spectrometry of large biomolecules. We have performed a combined theoretical and experimental study of capillary filling in micron-sized slots with the aim of developing a rational design procedure for miniaturized electrospray sources, ultimately enabling the integration of ESI into laboratory-on-a-chip devices

  11. Mass spectrometry. Environment, biology, oenology, medicine, geology, chemistry, archaeology, mechanisms

    International Nuclear Information System (INIS)

    1999-01-01

    This document provides the papers (communications and posters) presented at the 16. French days of mass spectrometry, held September 6-9, 1999 in Nancy, France. 5 papers are interesting for the INIS database and are analyzed separately. (O.M.)

  12. Automatic Compound Annotation from Mass Spectrometry Data Using MAGMa.

    NARCIS (Netherlands)

    Ridder, L.O.; Hooft, van der J.J.J.; Verhoeven, S.

    2014-01-01

    The MAGMa software for automatic annotation of mass spectrometry based fragmentation data was applied to 16 MS/MS datasets of the CASMI 2013 contest. Eight solutions were submitted in category 1 (molecular formula assignments) and twelve in category 2 (molecular structure assignment). The MS/MS

  13. Fast atom bombardment mass spectrometry of condensed tannin sulfonate derivatives

    Science.gov (United States)

    J.J. Karchesy; L.Y. Foo; Richard W. Hemingway; E. Barofsky; D.F. Barofsky

    1989-01-01

    Condensed tannin sulfonate derivatives were studied by fast atom bombardment mass spectrometry (FAB-MS) to assess the feasibility of using this technique for determining molecular weight and structural information about these compounds. Both positive- and negative-ion spectra provided useful data with regard to molecular weight, cation species present, and presence of...

  14. Molecular mass spectrometry imaging in biomedical and life science research

    Czech Academy of Sciences Publication Activity Database

    Pól, Jaroslav; Strohalm, Martin; Havlíček, Vladimír; Volný, Michael

    2010-01-01

    Roč. 134, č. 5 (2010), s. 423-443 ISSN 0948-6143 R&D Projects: GA MŠk LC545; GA ČR GPP206/10/P018 Institutional research plan: CEZ:AV0Z50200510 Keywords : Mass spectrometry * Chemical imaging * Molecular imaging Subject RIV: EE - Microbiology, Virology Impact factor: 4.727, year: 2010

  15. 14 C dating by using mass spectrometry with particle accelerator

    International Nuclear Information System (INIS)

    Santos, G.M.; Gomes, P.R.S.; Yokoyama, Y.; Tada, M.L. di; Cresswell, R.G.; Fifield, L.K.

    1999-01-01

    The different aspects concerning the 14 C dating are described, including the cosmogenic origin of 14 C, its production and absorption by matter, the procedures to be followed for the age determination and the associated errors, particularly by the Accelerator Mass Spectrometry (AMS) technique, and the different steps of the sample preparation process. (author)

  16. Traveling-wave ion mobility mass spectrometry of protein complexes

    DEFF Research Database (Denmark)

    Salbo, Rune; Bush, Matthew F; Naver, Helle

    2012-01-01

    The collision cross-section (Ω) of a protein or protein complex ion can be measured using traveling-wave (T-wave) ion mobility (IM) mass spectrometry (MS) via calibration with compounds of known Ω. The T-wave Ω-values depend strongly on instrument parameters and calibrant selection. Optimization ...

  17. Mass spectrometry with ionization induced by 252Cf fission fragments

    International Nuclear Information System (INIS)

    Sysoev, A.A.; Artaev, V.B.

    1991-01-01

    The review deals with mass-spectrometry with ionization induced by 252 Cf fission fragments. Equipment and technique of the analysis, analytic possibilities of the method are considered. The method permits to determine molecular masses of large nonvolatile biological molecules. The method is practically nondestructive, it possesses a high resolution over the depth and surface, which permits to use it for the analysis of surface of semiconductors, dielectrics, catalysts, for the study of formation kinetics of complex unstable molecules on the surface

  18. Mass spectrometry of submicrogram quantities of lead and cadmium

    International Nuclear Information System (INIS)

    Moraes, Noemia M.P. de; Kakazu, M.H.; Iyer, S.S.

    1980-01-01

    Isotope analyses of submicrogram quantities of lead and cadmium are carried out by single filament solid source mass spectrometry. Thermionic emission of Pb and Cd is enhanced using silica gel as an emitter. Details of the chemical and mass spectrometric techniques are described. The low blank levels are maintained by extra purification of the reagents. The applications of isotope ratios of Pb and Cd in environmental sciences and geochemistry are discussed. (Author) [pt

  19. High Resolution Mass Spectrometry of Polyfluorinated Polyether-Based Formulation

    DEFF Research Database (Denmark)

    Dimzon, Ian Ken; Trier, Xenia; Frömel, Tobias

    2016-01-01

    High resolution mass spectrometry (HRMS) was successfully applied to elucidate the structure of a polyfluorinated polyether (PFPE)-based formulation. The mass spectrum generated from direct injection into the MS was examined by identifying the different repeating units manually and with the aid o......-fluorinated polymers. The information from MS is essential in studying the physico-chemical properties of PFPEs and can help in assessing the risks they pose to the environment and to human health. Graphical Abstract ᅟ....

  20. Focusing procedures in time-of-flight mass spectrometry

    International Nuclear Information System (INIS)

    Ioanoviciu, D.

    2002-01-01

    Time-of-flight mass spectrometry is a fast growing field due to its ability to handle very fast processes and due to its theoretically unlimited mass range. The performances of the time-of-flight mass analysers are heavily dependent on the progress in ion optics, a periodically reviewed field. In this presentation the various focusing procedures in time-of-flight mass spectrometry are reviewed. For ions of the same charge and mass flight time differences result from different potentials at the location of formation and from the initial velocity spread. There is no simultaneous space and velocity focusing in time-of-flight mass spectrometry. Space focusing of first and second order can be reached in time-of-flight mass analysers having two homogeneous electric field ion sources followed by a field free space in front of the detector. Single and double stage homogeneous electric field mirrors can focus in time ions of different energies. These different energies result when ions leaving different initial sites and arriving simultaneously to an intermediate space focus. Convenient mass dispersion can be obtained by including a mirror. Initial velocity focusing is obtained by the delayed extraction procedure in drift space and mirror time-of-flight mass analysers. Post source pulse focusing aims at the same purpose. Ion source electrodes of hyperbolic shape, operated by high voltage pulses can bring major improvements of the resolution, especially at high masses. For each focusing procedure the geometric and/or electric conditions are given as well as the aberrations allowing the mass resolution determination. The various focusing procedures are compared and a prediction of their future performances was tempted. (author)

  1. Mass spectrometry of fluorocarbon-labeled glycosphingolipids

    DEFF Research Database (Denmark)

    Li, Yunsen; Arigi, Emma; Eichert, Heather

    2010-01-01

    ceramide N-deacylase (SCDase) is used to remove the fatty acid from the ceramide moiety, after which a fluorocarbon-rich substituent (F-Tag) is incorporated at the free amine of the sphingoid. In initial trials, a neutral GSL, globotriaosylceramide (Gb(3)Cer), three purified bovine brain gangliosides...... with subsequent per-N,O-methylation was established for the F-tagged Gb(3) Cer and purified gangliosides, and extensive mass spectra (MS(1) and MS(2)) consistent with all of the expected products were acquired. The potential use of F-tagged derivatives for a comprehensive MS based profiling application...

  2. Automated Intelligent Assistant for mass spectrometry operation

    International Nuclear Information System (INIS)

    Filby, E.E.; Rankin, R.A.; Yoshida, D.E.

    1991-01-01

    The Automated Intelligent Assistant is designed to insure that our mass spectrometers produce timely, high-quality measurement data. The design combines instrument interfacing and expert system technology to automate an adaptable set-point damage prevention strategy. When shutdowns occur, the Assistant can help guide troubleshooting efforts. Stored real-time data will help our development program upgrade and improve the system, and also make it possible to re-run previously-observed instrument problems as ''live'' training exercises for the instrument operators. Initial work has focused on implementing the Assistant for the instrument ultra-high vacuum components. 14 refs., 5 figs

  3. Application of Laser Mass Spectrometry to Art and Archaeology

    Science.gov (United States)

    Gulian, Lase Lisa E.; Callahan, Michael P.; Muliadi, Sarah; Owens, Shawn; McGovern, Patrick E.; Schmidt, Catherine M.; Trentelman, Karen A.; deVries, Mattanjah S.

    2011-01-01

    REMPI laser mass spectrometry is a combination of resonance enhanced multiphoton ionization spectroscopy and time of flight mass spectrometry, This technique enables the collection of mass specific optical spectra as well as of optically selected mass spectra. Analytes are jet-cooled by entrainment in a molecular beam, and this low temperature gas phase analysis has the benefit of excellent vibronic resolution. Utilizing this method, mass spectrometric analysis of historically relevant samples can be simplified and improved; Optical selection of targets eliminates the need for chromatography while knowledge of a target's gas phase spectroscopy allows for facile differentiation of molecules that are in the aqueous phase considered spectroscopically indistinguishable. These two factors allow smaller sample sizes than commercial MS instruments, which in turn will require less damage to objects of antiquity. We have explored methods to optimize REMPI laser mass spectrometry as an analytical tool to archaeology using theobromine and caffeine as molecular markers in Mesoamerican pottery, and are expanding this approach to the field of art to examine laccaic acid in shellacs.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-10-17

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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  6. Accelerator mass spectrometry in biomedical research

    International Nuclear Information System (INIS)

    Vogel, J.S.; Turteltaub, K.W.

    1993-01-01

    Biological effects occur in natural systems at chemical concentrations of parts per billion (1:10 9 ) or less. Affected biomolecules may be separable in only milligram or microgram quantities. Quantification at attomole sensitivity is needed to study these interactions. AMS measures isotope concentrations to parts per 10 13--15 on milligram-sized samples and is ideal for quantifying long-lived radioisotopic labels that are commonly used to trace biochemical pathways in natural systems. 14 C-AMS has now been coupled to a variety of organic separation and definition technologies. The primary research investigates pharmacokinetics and genotoxicities of toxins and drugs at very low doses. Human subject research using AMS includes nutrition, toxicity and elemental balance studies. 3 H, 41 Ca and 26 Al are also traced by AMS for fundamental biochemical kinetic research. Expansion of biomedical AMS awaits further development of biochemical and accelerator technologies designed specifically for these applications

  7. Paleodiet characterisation of an Etrurian population of Pontecagnano (Italy) by Isotope Ratio Mass Spectrometry (IRMS) and Atomic Absorption Spectrometry (AAS)(#).

    Science.gov (United States)

    Scarabino, Carla; Lubritto, Carmine; Proto, Antonio; Rubino, Mauro; Fiengo, Gilda; Marzaioli, Fabio; Passariello, Isabella; Busiello, Gaetano; Fortunato, Antonietta; Alfano, Davide; Sabbarese, Carlo; Rogalla, Detlef; De Cesare, Nicola; d'Onofrio, Antonio; Terrasi, Filippo

    2006-06-01

    Human bones recovered from the archaeological site of Pontecagnano (Salerno, Italy) have been studied to reconstruct the diet of an Etrurian population. Two different areas were investigated, named Library and Sant' Antonio, with a total of 44 tombs containing human skeletal remains, ranging in age from the 8th to the 3rd century B.C. This time span was confirmed by 14C dating obtained using Accelerator Mass Spectrometry (AMS) on one bone sample from each site. Atomic Absorption Spectrometry (AAS) was used to extract information about the concentration of Sr, Zn, Ca elements in the bone inorganic fraction, whilst stable isotope ratio measurements (IRMS) were carried out on bone collagen to obtain the delta13C and delta15N. A reliable technique has been used to extract and separate the inorganic and organic fractions of the bone remains. Both IRMS and AAS results suggest a mixed diet including C3 plant food and herbivore animals, consistent with archaeological indications.

  8. Inter-laboratory comparison of elemental analysis and gas chromatography combustion isotope ratio mass spectrometry (GC-C-IRMS). Part I: delta13C measurements of selected compounds for the development of an isotopic Grob-test.

    Science.gov (United States)

    Serra, F; Janeiro, A; Calderone, G; Rojas, J M Moreno; Rhodes, C; Gonthier, L A; Martin, F; Lees, M; Mosandl, A; Sewenig, S; Hener, U; Henriques, B; Ramalho, L; Reniero, F; Teixeira, A J; Guillou, C

    2007-03-01

    This study was directed towards investigating suitable compounds to be used as stable isotope reference materials for gas chromatography combustion isotope ratio mass spectrometry (GC-C-IRMS) calibration. Several compounds were selected from those used in the 'Grob-test' mixture. Oxygen- and nitrogen-containing substances were added to these compounds to allow the mixture to be used as a possible multi-isotopic calibration tool for 2H/1H, 13C/12C, 15N/14N and 18O/16O ratio determinations. In this paper we present the results of delta13C measurements performed by the consortium of the five laboratories taking part in this inter-calibration exercise. All the compounds were individually assessed for homogeneity, short-term stability and long-term stability by means of EA-IRMS, as required by the bureau communitaire de reference (BCR) Guide for Production of Certified Reference Materials. The results were compared then with the GC-C-IRMS measurements using both polar and non-polar columns, and the final mixture of selected compounds underwent a further certification exercise assessing limits of accuracy and reproducibility under specified GC-C-IRMS conditions. Copyright 2007 John Wiley & Sons, Ltd.

  9. Liquid chromatography-mass spectrometry in forensic toxicology.

    Science.gov (United States)

    Van Bocxlaer, J F; Clauwaert, K M; Lambert, W E; Deforce, D L; Van den Eeckhout, E G; De Leenheer, A P

    2000-01-01

    Liquid chromatography-mass spectrometry has evolved from a topic of mainly research interest into a routinely usable tool in various application fields. With the advent of new ionization approaches, especially atmospheric pressure, the technique has established itself firmly in many areas of research. Although many applications prove that LC-MS is a valuable complementary analytical tool to GC-MS and has the potential to largely extend the application field of mass spectrometry to hitherto "MS-phobic" molecules, we must recognize that the use of LC-MS in forensic toxicology remains relatively rare. This rarity is all the more surprising because forensic toxicologists find themselves often confronted with the daunting task of actually searching for evidence materials on a scientific basis without any indication of the direction in which to search. Through the years, mass spectrometry, mainly in the GC-MS form, has gained a leading role in the way such quandaries are tackled. The advent of robust, bioanalytically compatible combinations of liquid chromatographic separation with mass spectrometric detection really opens new perspectives in terms of mass spectrometric identification of difficult molecules (e.g., polar metabolites) or biopolymers with toxicological relevance, high throughput, and versatility. Of course, analytical toxicologists are generally mass spectrometry users rather than mass spectrometrists, and this difference certainly explains the slow start of LC-MS in this field. Nevertheless, some valuable applications have been published, and it seems that the introduction of the more universal atmospheric pressure ionization interfaces really has boosted interests. This review presents an overview of what has been realized in forensic toxicological LC-MS. After a short introduction into LC-MS interfacing operational characteristics (or limitations), it covers applications that range from illicit drugs to often abused prescription medicines and some

  10. Photoionization mass spectrometry of UF6

    International Nuclear Information System (INIS)

    Berkowitz, J.

    1979-01-01

    The photoionization mass spectrum of 238 UF 6 was obtained. At 600 A = 20.66 eV, the relative ionic abundances were as follows: UF 6 + , 1.4; UF 5 + , 100; UF + , 17; UF 3 + , approx. 0.7; UF 2 + , very weak; UF + , very weak; U + , essentially zero. The adiabatic ionization potential for UF 6 was 13.897 +- 0.005 eV. The production of UF 5 + begins at approx. 887 A = 13.98 eV, at which energy the UF 6 + partial cross section abruptly declines and then levels off. This behavior suggests the vague possibility of an isotope effect. The UF 4 + signal begins at approx. 725 A = 17.10 eV, at which energy the UF 5 + signal reaches a plateau value. The UF 5 + photoionization yield curve displays some autoionization structure from its threshold to approx. 750 A

  11. Complete Hexose Isomer Identification with Mass Spectrometry

    Science.gov (United States)

    Nagy, Gabe; Pohl, Nicola L. B.

    2015-04-01

    The first analytical method is presented for the identification and absolute configuration determination of all 24 aldohexose and 2-ketohexose isomers, including the D and L enantiomers for allose, altrose, galactose, glucose, gulose, idose, mannose, talose, fructose, psicose, sorbose, and tagatose. Two unique fixed ligand kinetic method combinations were discovered to create significant enough energetic differences to achieve chiral discrimination among all 24 hexoses. Each of these 24 hexoses yields unique ratios of a specific pair of fragment ions that allows for simultaneous determination of identification and absolute configuration. This mass spectrometric-based methodology can be readily employed for accurate identification of any isolated monosaccharide from an unknown biological source. This work provides a key step towards the goal of complete de novo carbohydrate analysis.

  12. Intact glycopeptide characterization using mass spectrometry.

    Science.gov (United States)

    Cao, Li; Qu, Yi; Zhang, Zhaorui; Wang, Zhe; Prytkova, Iya; Wu, Si

    2016-05-01

    Glycosylation is one of the most prominent and extensively studied protein post-translational modifications. However, traditional proteomic studies at the peptide level (bottom-up) rarely characterize intact glycopeptides (glycosylated peptides without removing glycans), so no glycoprotein heterogeneity information is retained. Intact glycopeptide characterization, on the other hand, provides opportunities to simultaneously elucidate the glycan structure and the glycosylation site needed to reveal the actual biological function of protein glycosylation. Recently, significant improvements have been made in the characterization of intact glycopeptides, ranging from enrichment and separation, mass spectroscopy (MS) detection, to bioinformatics analysis. In this review, we recapitulated currently available intact glycopeptide characterization methods with respect to their advantages and limitations as well as their potential applications.

  13. Precise atomic mass measurements by deflection mass spectrometry

    CERN Document Server

    Barber, R C

    2003-01-01

    Since its inception nearly 90 years ago by J.J. Thomson, the precise determination of atomic masses by the classical technique of deflecting charged particles in electric and magnetic fields has provided a large body of data on naturally occurring nuclides. Currently, such measurements on stable nuclides have frequently achieved a precision of better than two parts in 10 sup 9 of the mass. A review of the technique, together with a brief summary of the important historical developments in the field of precise atomic mass measurements, will be given. The more recent contributions to this field by the deflection mass spectrometer at the University of Manitoba will be provided as illustrations of the culmination of the techniques used and the applications that have been studied. A brief comparison between this and newer techniques using Penning traps will be presented.

  14. Hands-on Electrospray Ionization-Mass Spectrometry for Upper-Level Undergraduate and Graduate Students

    Science.gov (United States)

    Stock, Naomi L.; March, Raymond E.

    2014-01-01

    Electrospray ionization-mass spectrometry (ESI-MS) is a powerful technique for the detection, identification, and quantification of organic compounds. As mass spectrometers have become more user-friendly and affordable, many students--often with little experience in mass spectrometry--find themselves needing to incorporate mass spectrometry into…

  15. Meet interesting abbreviations in clinical mass spectrometry: from compound classification by REIMS to multimodal and mass spectrometry imaging (MSI)

    Czech Academy of Sciences Publication Activity Database

    Luptáková, Dominika; Pluháček, Tomáš; Palyzová, Andrea; Přichystal, Jakub; Balogh, J.; Lemr, Karel; Juránek, I.; Havlíček, Vladimír

    2017-01-01

    Roč. 61, č. 3 (2017), s. 353-360 ISSN 0001-723X R&D Projects: GA MŠk(CZ) LO1509; GA ČR(CZ) GA16-20229S Institutional support: RVO:61388971 Keywords : REIMS * multimodal * mass spectrometry imaging Subject RIV: EE - Microbiology, Virology OBOR OECD: Microbiology Impact factor: 0.673, year: 2016

  16. T cells recognizing a peptide contaminant undetectable by mass spectrometry

    DEFF Research Database (Denmark)

    Brezar, Vedran; Culina, Slobodan; Østerbye, Thomas

    2011-01-01

    Synthetic peptides are widely used in immunological research as epitopes to stimulate their cognate T cells. These preparations are never completely pure, but trace contaminants are commonly revealed by mass spectrometry quality controls. In an effort to characterize novel major histocompatibility...... complex (MHC) Class I-restricted ß-cell epitopes in non-obese diabetic (NOD) mice, we identified islet-infiltrating CD8+ T cells recognizing a contaminating peptide. The amount of this contaminant was so small to be undetectable by direct mass spectrometry. Only after concentration by liquid...... chromatography, we observed a mass peak corresponding to an immunodominant islet-specific glucose-6-phosphatase catalytic subunit-related protein (IGRP)(206-214) epitope described in the literature. Generation of CD8+ T-cell clones recognizing IGRP(206-214) using a novel method confirmed the identity...

  17. Analytical applications of resonance ionization mass spectrometry (RIMS)

    International Nuclear Information System (INIS)

    Fassett, J.D.; Travis, J.C.

    1988-01-01

    A perspective on the role of resonance ionization mass spectrometry (RIMS) in the field of analytical chemistry is presented. RIMS provides new, powerful, and complementary capabilities relative to traditional methods of inorganic mass spectrometry. Much of the initial work in RIMS has been to illustrate these capabilities and define the potential of RIMS in the generalized field of chemical analysis. Three areas of application are reviewed here: (1) noble gas measurements; (2) materials analysis using isotope dilution (IDMS); and, (3) solids analysis using direct sampling. The role of RIMS is discussed relative to the more traditional mass spectrometric methods of analysis in these areas. The applications are meant to illustrate the present state-of-the-art as well as point to the future state-of-the-art of RIMS in chemical analysis. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-10-15

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

  19. LILBID-mass spectrometry of the mitochondrial preprotein translocase TOM

    International Nuclear Information System (INIS)

    Mager, Frauke; Lintzel, Julia; Nussberger, Stephan; Sokolova, Lucie; Brutschy, Bernhard

    2010-01-01

    In the present work we applied a novel mass spectrometry method termed laser-induced liquid bead ion desorption mass spectrometry (LILBID-MS) to the outer mitochondrial membrane protein translocon TOM to analyze its subunit composition and stoichiometry. With TOM core complex, purified at high pH, we demonstrate that a TOM core complex of Neurospora crassa is composed of at least two Tom40 and Tom22 molecules, respectively, and more than five small Tom subunits between 5.5 and 6.4 kDa. We show that the multiprotein complex has a total molecular mass higher than 170 depending on the number of Tom5, Tom6 and Tom7 molecules bound.

  20. LILBID-mass spectrometry of the mitochondrial preprotein translocase TOM

    Science.gov (United States)

    Mager, Frauke; Sokolova, Lucie; Lintzel, Julia; Brutschy, Bernhard; Nussberger, Stephan

    2010-11-01

    In the present work we applied a novel mass spectrometry method termed laser-induced liquid bead ion desorption mass spectrometry (LILBID-MS) to the outer mitochondrial membrane protein translocon TOM to analyze its subunit composition and stoichiometry. With TOM core complex, purified at high pH, we demonstrate that a TOM core complex of Neurospora crassa is composed of at least two Tom40 and Tom22 molecules, respectively, and more than five small Tom subunits between 5.5 and 6.4 kDa. We show that the multiprotein complex has a total molecular mass higher than 170 depending on the number of Tom5, Tom6 and Tom7 molecules bound.

  1. Resonance ionization mass spectrometry system for measurement of environmental samples

    International Nuclear Information System (INIS)

    Pibida, L.; McMahon, C.A.; Noertershaeuser, W.; Bushaw, B.A.

    2002-01-01

    A resonance ionization mass spectrometry (RIMS) system has been developed at the National Institute of Standards and Technology (NIST) for sensitive and selective determination of radio-cesium in the environment. The overall efficiency was determined to be 4x10-7 with a combined (laser and mass spectrometer) selectivity of 108 for both 135Cs and 137Cs with respect to 133Cs. RIMS isotopic ratio measurements of 135Cs/ 137Cs were performed on a nuclear fuel burn-up sample and compared to measurements on a similar system at Pacific Northwest National Laboratory (PNNL) and to conventional thermal ionization mass spectrometry (TIMS). Results of preliminary RIMS investigations on a freshwater lake sediment sample are also discussed

  2. Mass spectrometry of selective androgen receptor modulators.

    Science.gov (United States)

    Thevis, Mario; Schänzer, Wilhelm

    2008-07-01

    Nonsteroidal selective androgen receptor modulators (SARMs) are an emerging class of drugs for treatment of various diseases including osteoporosis and muscle wasting as well as the correction of age-related functional decline such as muscle strength and power. Several SARMs, which have advanced to preclinical and clinical trials, are composed of diverse chemical structures including arylpropionamide-, bicyclic hydantoin-, quinoline-, and tetrahydroquinoline-derived nuclei. Since January 2008, SARMs have been categorized as anabolic agents and prohibited by the World Anti-Doping Agency (WADA). Suitable detection methods for these low-molecular weight drugs were based on mass spectrometric approaches, which necessitated the elucidation of dissociation pathways in order to characterize and identify the target analytes in doping control samples as well as potential metabolic products and synthetic analogs. Fragmentation patterns of representatives of each category of SARMs after electrospray ionization (ESI) and collision-induced dissociation (CID) as well as electron ionization (EI) are summarized. The complexity and structural heterogeneity of these drugs is a daunting challenge for detection methods. Copyright 2008 John Wiley & Sons, Ltd.

  3. Analytical capabilities of laser-probe mass spectrometry

    International Nuclear Information System (INIS)

    Kovalev, I.D.; Madsimov, G.A.; Suchkov, A.I.; Larin, N.V.

    1978-01-01

    The physical bases and quantitative analytical procedures of laser-probe mass spectrometry are considered in this review. A comparison is made of the capabilities of static and dynamic mass spectrometers. Techniques are studied for improving the analytical characteristics of laser-probe mass spectrometers. The advantages, for quantitative analysis, of the Q-switched mode over the normal pulse mode for lasers are: (a) the possibility of analysing metals, semiconductors and insulators without the use of standards; and (b) the possibility of layer-by-layer and local analysis. (Auth.)

  4. Computer automation of an accelerator mass spectrometry system

    International Nuclear Information System (INIS)

    Gressett, J.D.; Maxson, D.L.; Matteson, S.; McDaniel, F.D.; Duggan, J.L.; Mackey, H.J.; North Texas State Univ., Denton, TX; Anthony, J.M.

    1989-01-01

    The determination of trace impurities in electronic materials using accelerator mass spectrometry (AMS) requires efficient automation of the beam transport and mass discrimination hardware. The ability to choose between a variety of charge states, isotopes and injected molecules is necessary to provide survey capabilities similar to that available on conventional mass spectrometers. This paper will discuss automation hardware and software for flexible, high-sensitivity trace analysis of electronic materials, e.g. Si, GaAs and HgCdTe. Details regarding settling times will be presented, along with proof-of-principle experimental data. Potential and present applications will also be discussed. (orig.)

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  6. Cortisol production rates measured by liquid chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    Esteban, N.V.; Yergey, A.L.

    1990-01-01

    Cortisol production rates (FPRs) in physiologic and pathologic states in humans have been investigated over the past 30 years. However, there has been conflicting evidence concerning the validity of the currently accepted value of FPRs in humans (12 to 15 mg/m2/d) as determined by radiotracer methodology. The present study reviews previous methods proposed for the measurement of FPRs in humans and discusses the applications of the first method for the direct determination of 24-hour plasma FPRs during continuous administration of a stable isotope, using a thermospray high-pressure liquid chromatography-mass spectrometry technique. The technique is fast, sensitive, and, unlike gas chromatography-mass spectrometry methods, does not require derivatization, allowing on-line detection and quantification of plasma cortisol after a simple extraction procedure. The results of determination of plasma FPRs by stable tracer/mass spectrometry are directly in units of mass/time and, unlike radiotracer methods, are independent of any determination of volume of distribution or cortisol concentration. Our methodology offers distinct advantages over radiotracer techniques in simplicity and reliability since only single measurements of isotope ratios are required. The technique was validated in adrenalectomized patients. Circadian variations in daily FRPs were observed in normal volunteers, and, to date, results suggest a lower FRP in normal children and adults than previously believed. 88 references

  7. Advances in 193 nm excimer lasers for mass spectrometry applications

    Science.gov (United States)

    Delmdahl, Ralph; Esser, Hans-Gerd; Bonati, Guido

    2016-03-01

    Ongoing progress in mass analysis applications such as laser ablation inductively coupled mass spectrometry of solid samples and ultraviolet photoionization mediated sequencing of peptides and proteins is to a large extent driven by ultrashort wavelength excimer lasers at 193 nm. This paper will introduce the latest improvements achieved in the development of compact high repetition rate excimer lasers and elaborate on the impact on mass spectrometry instrumentation. Various performance and lifetime measurements obtained in a long-term endurance test over the course of 18 months will be shown and discussed in view of the laser source requirements of different mass spectrometry tasks. These sampling type applications are served by excimer lasers delivering pulsed 193 nm output of several mJ as well as fast repetition rates which are already approaching one Kilohertz. In order to open up the pathway from the laboratory to broader market industrial use, sufficient component lifetimes and long-term stable performance behavior have to be ensured. The obtained long-term results which will be presented are based on diverse 193 nm excimer laser tube improvements aiming at e.g. optimizing the gas flow dynamics and have extended the operational life the laser tube for the first time over several billion pulses even under high duty-cycle conditions.

  8. Isotope dilution inductively coupled plasma quadrupole mass spectrometry in connection with a chromatographic separation for ultra trace determinations of platinum group elements (Pt, Pd, Ru, Ir) in environmental samples.

    Science.gov (United States)

    Müller, M; Heumann, K G

    2000-09-01

    An isotope dilution inductively coupled plasma quadrupole mass spectrometric (ID-ICP-QMS) method was developed for the simultaneous determination of the platinum group elements Pt, Pd, Ru, and Ir in environmental samples. Spike solutions, enriched with the isotopes 194Pt, 108Pd, 99Ru, and 191Ir, were used for the isotope dilution step. Interfering elements were eliminated by chromatographic separation using an anion-exchange resin. Samples were dissolved with aqua regia in a high pressure asher. Additional dissolution of possible silicate portions by hydrofluoric acid was usually not necessary. Detection limits of 0.15 ng x g(-1), 0.075 ng x g(-1), and 0.015 ng x g(-1) were achieved for Pt, Pd, Ru, and Ir, respectively, using sample weights of only 0.2 g. The reliability of the ID-ICP-QMS method was demonstrated by analyzing a Canadian geological reference material and by participating in an interlaboratory study for the determination of platinum and palladium in a homogenized road dust sample. Surface soil, sampled at different distances from a highway, showed concentrations in the range of 0.1-87 ng x g(-1). An exponential decrease of the platinum and palladium concentration with increasing distance and a small anthropogenic contribution to the natural background concentration of ruthenium and iridium was found in these samples.

  9. Atmospheric pressure photo ionization hydrogen/deuterium exchange mass spectrometry--a method to differentiate isomers by mass spectrometry.

    Science.gov (United States)

    Ahmed, Arif; Kim, Sunghwan

    2013-12-01

    In this report, a method for in-source hydrogen/deuterium (H/D) exchange at atmospheric pressure is reported. The method was named atmospheric pressure photo ionization hydrogen/deuterium exchange mass spectrometry (APPI HDX MS). H/D exchange was performed by mixing samples dissolved in toluene with CH3OD solvent and analyzing the mixture using atmospheric pressure photo ionization mass spectrometry (APPI-MS). The APPI HDX spectra obtained with contact times between the analyte solution and methanol-OD (CH3OD) of atmospheric pressure. H/D exchange can be performed in any laboratory with a mass spectrometer and a commercial APPI source. Using this method, multiple H/D exchanges of aromatic hydrogen and/or H/D exchange of active hydrogen were observed. These results demonstrated that H/D exchange can be used to distinguish between isomers containing primary, secondary, and tertiary amines, as well as pyridine and pyrrole functional groups.

  10. Accelerator mass spectrometry at IFIN-HH in Bucharest

    International Nuclear Information System (INIS)

    Stan-Sion, C.; Catana, D.; Plostinaru, D.; Radulescu, M.; Enachescu, M.

    1999-01-01

    An AMS (Accelerator Mass Spectrometry) facility was constructed at the FN - 8 MV Tandem Accelerator of the National Institute for Physics and Nuclear Engineering in Bucharest. It represents the first experimental setup of this type in the large geographical area of Eastern Europe. The main components of the facility are: the ion injector deck, the AMS beam line and the detector systems. The injector deck is polarised at 50 kV and contains the high current sputtering ion source (spherical ionizer) followed, for beam transport, by electrostatic devices (single lenses, steerers, quadrupole lenses), a double focussing, 90 angle analysing magnet (Danfysik), a pre-acceleration tube (NEC) and several diagnose and defining elements. The AMS samples are placed in an eight stack magazine attached to the ion source. On the exit side of the Tandem Accelerator tank, a velocity filter and the particle detection system are mounted. The beam line, on the high energy side, is optically achromatic and contains two 90 angle analysing magnets of 150 MEP. For particle detection a Bragg-curve Spectroscopy Detector (ionisation chamber) is used and a multi-anode gas detector with TOF discrimination is under construction. The research programme at this new facility is focused on using 26 Al for medical applications. In future it will be use for 129 I - AMS measurements as a nuclear safeguard. This long lived isotope will be used to monitor and investigate the transport of 129 I in vicinity of three nuclear power plants in Eastern Europe: Kozloduy (Bulgaria), Cernavoda (Romania) and Chernobyl (Ukraine). Measurements will concern soil, precipitation and air samples. Water samples will be collected along the flow of rivers Danube and Dnieper, from the Danube Delta and from coastal areas of the Black Sea. (authors)

  11. Study by Auger spectrometry and mass spectrometry of the chemisorption of carbon monoxide on polycrystalline molybdenum

    International Nuclear Information System (INIS)

    Gillet, E.; Chiarena, J.C.; Gillet, M.

    1976-01-01

    A combination of Auger spectrometry and mass spectrometry was employed to study CO chemisorption on polycrystalline Mo surfaces at room temperature. Five adsorption states were observed and the binding parameters (E,n 0 ,tau 0 ) were calculated for the three important states. The results obtained by the two methods are in accord but the occurence of electronic desorption in Auger experiments was pointed out. Contamination effects by C atoms in such studies were investigated by repeated cycles of adsorption-desorption and a characteristic evolution of flash desorption was observed. The results are discussed in this point of view enhancing the importance of a control of the adsorption surface cleanness by a method of great sensibility like Auger spectrometry. (Auth.)

  12. The Use of Gas Chromatography and Mass Spectrometry to Introduce General Chemistry Students to Percent Mass and Atomic Mass Calculations

    Science.gov (United States)

    Pfennig, Brian W.; Schaefer, Amy K.

    2011-01-01

    A general chemistry laboratory experiment is described that introduces students to instrumental analysis using gas chromatography-mass spectrometry (GC-MS), while simultaneously reinforcing the concepts of mass percent and the calculation of atomic mass. Working in small groups, students use the GC to separate and quantify the percent composition…

  13. Establishing Drug Resistance in Microorganisms by Mass Spectrometry

    Science.gov (United States)

    Demirev, Plamen A.; Hagan, Nathan S.; Antoine, Miquel D.; Lin, Jeffrey S.; Feldman, Andrew B.

    2013-08-01

    A rapid method to determine drug resistance in bacteria based on mass spectrometry is presented. In it, a mass spectrum of an intact microorganism grown in drug-containing stable isotope-labeled media is compared with a mass spectrum of the intact microorganism grown in non-labeled media without the drug present. Drug resistance is determined by predicting characteristic mass shifts of one or more microorganism biomarkers using bioinformatics algorithms. Observing such characteristic mass shifts indicates that the microorganism is viable even in the presence of the drug, thus incorporating the isotopic label into characteristic biomarker molecules. The performance of the method is illustrated on the example of intact E. coli, grown in control (unlabeled) and 13C-labeled media, and analyzed by MALDI TOF MS. Algorithms for data analysis are presented as well.

  14. Fourier Transform Mass Spectrometry: The Transformation of Modern Environmental Analyses

    Science.gov (United States)

    Lim, Lucy; Yan, Fangzhi; Bach, Stephen; Pihakari, Katianna; Klein, David

    2016-01-01

    Unknown compounds in environmental samples are difficult to identify using standard mass spectrometric methods. Fourier transform mass spectrometry (FTMS) has revolutionized how environmental analyses are performed. With its unsurpassed mass accuracy, high resolution and sensitivity, researchers now have a tool for difficult and complex environmental analyses. Two features of FTMS are responsible for changing the face of how complex analyses are accomplished. First is the ability to quickly and with high mass accuracy determine the presence of unknown chemical residues in samples. For years, the field has been limited by mass spectrometric methods that were based on knowing what compounds of interest were. Secondly, by utilizing the high resolution capabilities coupled with the low detection limits of FTMS, analysts also could dilute the sample sufficiently to minimize the ionization changes from varied matrices. PMID:26784175

  15. Fourier Transform Mass Spectrometry: The Transformation of Modern Environmental Analyses

    Directory of Open Access Journals (Sweden)

    Lucy Lim

    2016-01-01

    Full Text Available Unknown compounds in environmental samples are difficult to identify using standard mass spectrometric methods. Fourier transform mass spectrometry (FTMS has revolutionized how environmental analyses are performed. With its unsurpassed mass accuracy, high resolution and sensitivity, researchers now have a tool for difficult and complex environmental analyses. Two features of FTMS are responsible for changing the face of how complex analyses are accomplished. First is the ability to quickly and with high mass accuracy determine the presence of unknown chemical residues in samples. For years, the field has been limited by mass spectrometric methods that were based on knowing what compounds of interest were. Secondly, by utilizing the high resolution capabilities coupled with the low detection limits of FTMS, analysts also could dilute the sample sufficiently to minimize the ionization changes from varied matrices.

  16. Native Mass Spectrometry in Fragment-Based Drug Discovery

    Directory of Open Access Journals (Sweden)

    Liliana Pedro

    2016-07-01

    Full Text Available The advent of native mass spectrometry (MS in 1990 led to the development of new mass spectrometry instrumentation and methodologies for the analysis of noncovalent protein–ligand complexes. Native MS has matured to become a fast, simple, highly sensitive and automatable technique with well-established utility for fragment-based drug discovery (FBDD. Native MS has the capability to directly detect weak ligand binding to proteins, to determine stoichiometry, relative or absolute binding affinities and specificities. Native MS can be used to delineate ligand-binding sites, to elucidate mechanisms of cooperativity and to study the thermodynamics of binding. This review highlights key attributes of native MS for FBDD campaigns.

  17. Mass Spectrometry-Based N-Glycomics of Colorectal Cancer

    Directory of Open Access Journals (Sweden)

    Manveen K. Sethi

    2015-12-01

    Full Text Available Colorectal cancer (CRC is one of the most prevalent cancers worldwide. An increased molecular understanding of the CRC pathology is warranted to gain insights into the underlying molecular and cellular mechanisms of the disease. Altered protein glycosylation patterns are associated with most diseases including malignant transformation. Recent advances in mass spectrometry and bioinformatics have accelerated glycomics research and present a new paradigm for cancer biomarker discovery. Mass spectrometry (MS-based glycoproteomics and glycomics, therefore, hold considerable promise to improve the discovery of novel biomarkers with utility in disease diagnosis and therapy. This review focuses on the emerging field of glycomics to present a comprehensive review of advances in technologies and their application in studies aimed at discovering novel glycan-based biomarkers. We will also discuss some of the challenges associated with using glycans as biomarkers.

  18. Statistical methods for quantitative mass spectrometry proteomic experiments with labeling

    Directory of Open Access Journals (Sweden)

    Oberg Ann L

    2012-11-01

    Full Text Available Abstract Mass Spectrometry utilizing labeling allows multiple specimens to be subjected to mass spectrometry simultaneously. As a result, between-experiment variability is reduced. Here we describe use of fundamental concepts of statistical experimental design in the labeling framework in order to minimize variability and avoid biases. We demonstrate how to export data in the format that is most efficient for statistical analysis. We demonstrate how to assess the need for normalization, perform normalization, and check whether it worked. We describe how to build a model explaining the observed values and test for differential protein abundance along with descriptive statistics and measures of reliability of the findings. Concepts are illustrated through the use of three case studies utilizing the iTRAQ 4-plex labeling protocol.

  19. Statistical methods for quantitative mass spectrometry proteomic experiments with labeling.

    Science.gov (United States)

    Oberg, Ann L; Mahoney, Douglas W

    2012-01-01

    Mass Spectrometry utilizing labeling allows multiple specimens to be subjected to mass spectrometry simultaneously. As a result, between-experiment variability is reduced. Here we describe use of fundamental concepts of statistical experimental design in the labeling framework in order to minimize variability and avoid biases. We demonstrate how to export data in the format that is most efficient for statistical analysis. We demonstrate how to assess the need for normalization, perform normalization, and check whether it worked. We describe how to build a model explaining the observed values and test for differential protein abundance along with descriptive statistics and measures of reliability of the findings. Concepts are illustrated through the use of three case studies utilizing the iTRAQ 4-plex labeling protocol.

  20. Centrosome isolation and analysis by mass spectrometry-based proteomics

    DEFF Research Database (Denmark)

    Jakobsen, Lis; Schrøder, Jacob Morville; Larsen, Katja M

    2013-01-01

    Centrioles are microtubule-based scaffolds that are essential for the formation of centrosomes, cilia, and flagella with important functions throughout the cell cycle, in physiology and during development. The ability to purify centriole-containing organelles on a large scale, combined with advan...... to isolate centrosomes from human cells and strategies to selectively identify and study the properties of the associated proteins using quantitative mass spectrometry-based proteomics.......Centrioles are microtubule-based scaffolds that are essential for the formation of centrosomes, cilia, and flagella with important functions throughout the cell cycle, in physiology and during development. The ability to purify centriole-containing organelles on a large scale, combined...... with advances in protein identification using mass spectrometry-based proteomics, have revealed multiple centriole-associated proteins that are conserved during evolution in eukaryotes. Despite these advances, the molecular basis for the plethora of processes coordinated by cilia and centrosomes is not fully...