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Sample records for spectrometry multi-elemental analysis

  1. Multi-elemental analysis of aqueous geological samples by inductively coupled plasma-optical emission spectrometry

    Science.gov (United States)

    Todorov, Todor I.; Wolf, Ruth E.; Adams, Monique

    2014-01-01

    Typically, 27 major, minor, and trace elements are determined in natural waters, acid mine drainage, extraction fluids, and leachates of geological and environmental samples by inductively coupled plasma-optical emission spectrometry (ICP-OES). At the discretion of the analyst, additional elements may be determined after suitable method modifications and performance data are established. Samples are preserved in 1–2 percent nitric acid (HNO3) at sample collection or as soon as possible after collection. The aqueous samples are aspirated into the ICP-OES discharge, where the elemental emission signals are measured simultaneously for 27 elements. Calibration is performed with a series of matrix-matched, multi-element solution standards.

  2. Multi-elemental analysis of marine sediments of Manila Bay using x-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Rosales, Colleen Marciel Fontelera

    2011-04-01

    An analysis of the marine sediments of Manila Bay was done by employing X-ray fluorescence spectrometry. The general trends observed in sediments are increasing (Ca and Sr), decreasing (Zr), or constant (Cl, Na, S, K) with respect to depth, sometimes, no trend can be observed. These trends are further explained by correlations present among these elements, plus all the other elements. The two X RF data analysis methods Auto Quantify and AXIL were also compared on the basis of the correlation plot obtained. AutoQuantify gave clearer correlations; thus, results from this method were used for constructing correlation plots. Correlations using Microsoft Excel and Stat graphics Centurion X V show that there are naturally occurring [lithogenic (Si, Ti, Al, Mg, Rb, Zn and Fe), biogenic (Ca, Mg), and conservative (Na, Cl)] and non-naturally occurring [mostly anthropogenic, brought to the bodies of water by aeolian or fluvial input (heavy metals Pb-Cu-Zn and Ni-Cr)] correlation present in the sediments. Moreover, pairs of elements that may coexist in a source and not coexist in another (Cr and Mg, Cr and Ni) have also been observed. The heavy metal enrichment was attributed to the burning of fossil fuels, iron and steel manufacturing (present in Valenzuela-Bulacan area), ferry and fishing services and other industrialization activities present in Manila Bay. Marine organisms are affected by the presence of these heavy metals by means of bioaccumulations, and may later on affect humans because of trophic transfer and bio magnification. (author)

  3. 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

  4. 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.

  5. Energy dispersive X-ray fluorescence spectrometry for the direct multi-element analysis of dried blood spots

    Science.gov (United States)

    Marguí, E.; Queralt, I.; García-Ruiz, E.; García-González, E.; Rello, L.; Resano, M.

    2018-01-01

    Home-based collection protocols for clinical specimens are actively pursued as a means of improving life quality of patients. In this sense, dried blood spots (DBS) are proposed as a non-invasive and even self-administered alternative to sampling whole venous blood. This contribution explores the potential of energy dispersive X-ray fluorescence spectrometry for the simultaneous and direct determination of some major (S, Cl, K, Na), minor (P, Fe) and trace (Ca, Cu, Zn) elements in blood, after its deposition onto clinical filter papers, thus giving rise to DBS. For quantification purposes the best strategy was to use matrix-matched blood samples of known analyte concentrations. The accuracy and precision of the method were evaluated by analysis of a blood reference material (Seronorm™ trace elements whole blood L3). Quantitative results were obtained for the determination of P, S, Cl, K and Fe, and limits of detection for these elements were adequate, taking into account their typical concentrations in real blood samples. Determination of Na, Ca, Cu and Zn was hampered by the occurrence of high sample support (Na, Ca) and instrumental blanks (Cu, Zn). Therefore, the quantitative determination of these elements at the levels expected in blood samples was not feasible. The methodology developed was applied to the analysis of several blood samples and the results obtained were compared with those reported by standard techniques. Overall, the performance of the method developed is promising and it could be used to determine the aforementioned elements in blood samples in a simple, fast and economic way. Furthermore, its non-destructive nature enables further analyses by means of complementary techniques to be carried out.

  6. 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

  7. 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

  8. 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.

  9. Multi-element analysis of emeralds and associated rocks by k0 neutron activation analysis

    International Nuclear Information System (INIS)

    Acharya, R.N.; Mondal, R.K.; Burte, P.P.; Nair, A.G.C.; Reddy, N.B.Y.; Reddy, L.K.; Reddy, A.V.R.; Manohar, S.B.

    2000-01-01

    Multi-element analysis was carried out in natural emeralds, their associated rocks and one sample of beryl obtained from Rajasthan, India. The concentrations of 21 elements were assayed by Instrumental Neutron Activation Analysis using the k 0 method (k 0 INAA method) and high-resolution gamma ray spectrometry. The data reveal the segregation of some elements from associated (trapped and host) rocks to the mineral beryl forming the gemstones. A reference rock standard of the US Geological Survey (USGS BCR-1) was also analysed as a control of the method

  10. Low-resolution continuum source simultaneous multi-element electrothermal atomic absorption spectrometry: steps into practice

    Energy Technology Data Exchange (ETDEWEB)

    Katskov, Dmitri, E-mail: katskovda@tut.ac.za

    2015-03-01

    The theory and practical problems of continuum source simultaneous multi-element electrothermal atomic absorption spectrometry (SMET AAS) are discussed by the example of direct analysis of underground water. The experimental methodology is based on pulse vaporization of the sample in a fast heated graphite tube and measurement of transient absorption of continuum spectrum radiation from D{sub 2} and Xe lamps within 200–400 nm wavelengths range with a low resolution spectral instrument and linear charge-coupled device. The setup permits the acquisition of 200 spectra during 1 s atomization pulse. Respective data matrix absorbance vs wavelength/time is employed for the quantification of elements in the sample. The calculation algorithm developed includes broad band and continuum background correction, linearization of function absorbance vs. concentration of atomic vapor and integration of thus modified absorbance at the resonance lines of the elements to be determined. Practical application shows that the method can be employed for the direct simultaneous determination of about 20 elements above microgram per liter level within 3–5 orders of the magnitude concentration range. The investigated sources of measurement errors are mainly associated with the atomization and vapor transportation problems, which are aggravated for the simultaneous release of major and minor sample constituents. Respective corrections concerning the selection of analytical lines, optimal sampling volume, matrix modification and cleaning of the atomizer have been introduced in the SMET AAS analytical technology. Under the optimized experimental conditions the calibration curves in Log-Log coordinates for all the investigated analytes in the single or multi-element reference solutions are approximated by the first order equations. The use of these equations as permanent characteristics of the setup enables instant quantification of Al, Ca, Co, Cr, Cu, Fe, Mg, Mn and Ni in the underground

  11. Low-resolution continuum source simultaneous multi-element electrothermal atomic absorption spectrometry: steps into practice

    International Nuclear Information System (INIS)

    Katskov, Dmitri

    2015-01-01

    The theory and practical problems of continuum source simultaneous multi-element electrothermal atomic absorption spectrometry (SMET AAS) are discussed by the example of direct analysis of underground water. The experimental methodology is based on pulse vaporization of the sample in a fast heated graphite tube and measurement of transient absorption of continuum spectrum radiation from D 2 and Xe lamps within 200–400 nm wavelengths range with a low resolution spectral instrument and linear charge-coupled device. The setup permits the acquisition of 200 spectra during 1 s atomization pulse. Respective data matrix absorbance vs wavelength/time is employed for the quantification of elements in the sample. The calculation algorithm developed includes broad band and continuum background correction, linearization of function absorbance vs. concentration of atomic vapor and integration of thus modified absorbance at the resonance lines of the elements to be determined. Practical application shows that the method can be employed for the direct simultaneous determination of about 20 elements above microgram per liter level within 3–5 orders of the magnitude concentration range. The investigated sources of measurement errors are mainly associated with the atomization and vapor transportation problems, which are aggravated for the simultaneous release of major and minor sample constituents. Respective corrections concerning the selection of analytical lines, optimal sampling volume, matrix modification and cleaning of the atomizer have been introduced in the SMET AAS analytical technology. Under the optimized experimental conditions the calibration curves in Log-Log coordinates for all the investigated analytes in the single or multi-element reference solutions are approximated by the first order equations. The use of these equations as permanent characteristics of the setup enables instant quantification of Al, Ca, Co, Cr, Cu, Fe, Mg, Mn and Ni in the underground water

  12. Design considerations regarding an atomizer for multi-element electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Katskov, Dmitri A., E-mail: katskovda@tut.ac.za [Department of Chemistry, Tshwane University of Technology, Private Bag X680, Pretoria 0001 (South Africa); Sadagov, Yuri M. [All-Russian Scientific Research Institute of Optical and Physical Measurements (VNIIOFI), Ozernaya St. 46, Moscow 119361 (Russian Federation)

    2011-06-15

    The methodology of simultaneous multi-element electrothermal atomic absorption spectrometry (ETAAS-Electrothermal Atomic Absorption Spectrometry) stipulates rigid requirements to the design and operation of the atomizer. It must provide high degree of atomization for the group of analytes, invariant respective to the vaporization kinetics and heating ramp residence time of atoms in the absorption volume and absence of memory effects from major sample components. For the low resolution spectrometer with a continuum radiation source the reduced compared to traditional ETAAS (Electrothermal Atomic Absorption Spectrometry) sensitivity should be, at least partially, compensated by creating high density of atomic vapor in the absorption pulse. The sought-for characteristics were obtained for the 18 mm in length and 2.5 mm in internal diameter longitudinally heated graphite tube atomizer furnished with 2-4.5 mg of ring shaped carbon fiber yarn collector. The collector located next to the sampling port provides large substrate area that helps to keep the sample and its residue in the central part of the tube after drying. The collector also provides a 'platform' effect that delays the vaporization and stipulates vapor release into absorption volume having already stabilized gas temperature. Due to the shape of external surface of the tube, presence of collector and rapid (about 10 {sup o}C/ms) heating, an inverse temperature distribution along the tube is attained at the beginnings of the atomization and cleaning steps. The effect is employed for cleaning of the atomizer using the set of short maximum power heating pulses. Preparation, optimal maintenance of the atomizer and its compliance to the multi-element determination requirements are evaluated and discussed. The experimental setup provides direct simultaneous determination of large group of element within 3-4 order concentration range. Limits of detection are close to those for sequential single element

  13. Multi-Element Composition of Honey as a Suitable Tool for Its Authenticity Analysis

    Directory of Open Access Journals (Sweden)

    Oroian Mircea

    2015-06-01

    Full Text Available The aim of this study was to evaluate the composition of 36 honey samples of 4 different botanical origins (acacia, sun flower, tilia and honeydew from the North East region of Romania. An inductively coupled plasma-mass spectrometry (ICP-MS method was used to determine 27 elements in honey (Ag, Al, As, Ba, Be, Ca, Cd, Co, Cr, Cs, Cu, Fe, Ga, K, Li, Mg, Mn, Na, Ni, Pb, Rb, Se, Sr, Tl, U, V and Zn. We would like to achieve the following goal: to demonstrate that the qualitative and quantitative multi-element composition determination of honey can be used as a suitable tool to classify honey according to its botanical origin. The principal component analysis allowed the reduction of the 27 variables to 2 principal components which explained 74% of the total variance. The dominant elements which were strongly associated with the principal component were K, Mg and Ca. Discriminant models obtained for each kind of botanical honey confirmed that the differentiation of honeys according to their botanical origin was mainly based on multi-element composition. A correct classification of all samples was achieved with the exception of 11.1% of honeydew honeys.

  14. Multi-element analysis of emeralds and associated rocks by k{sub 0} neutron activation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Acharya, R.N.; Mondal, R.K.; Burte, P.P.; Nair, A.G.C.; Reddy, N.B.Y.; Reddy, L.K.; Reddy, A.V.R.; Manohar, S.B

    2000-12-15

    Multi-element analysis was carried out in natural emeralds, their associated rocks and one sample of beryl obtained from Rajasthan, India. The concentrations of 21 elements were assayed by Instrumental Neutron Activation Analysis using the k{sub 0} method (k{sub 0} INAA method) and high-resolution gamma ray spectrometry. The data reveal the segregation of some elements from associated (trapped and host) rocks to the mineral beryl forming the gemstones. A reference rock standard of the US Geological Survey (USGS BCR-1) was also analysed as a control of the method.

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

    International Nuclear Information System (INIS)

    Sri-Wardani

    2004-01-01

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

  16. Multi-element analysis of lubricant oil by WDXRF technique using thin-film sample preparation

    International Nuclear Information System (INIS)

    Scapin, M. A.; Salvador, V. L. R.; Lopes, C. D.; Sato, I. M.

    2006-01-01

    The quantitative analysis of the chemical elements in matrices like oils or gels represents a challenge for the analytical chemists. The classics methods or instrumental techniques such as atomic absorption spectrometry (AAS) and plasma optical emission spectrometry (ICP-OES) need chemical treatments, mainly sample dissolution and degradation processes. X-ray fluorescence technique allows a direct and multi-element analysis without previous sample treatments. In this work, a sensible method for the determination of elements Mg, Al, Si, P, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Mo, Ag, Sn, Ba and Pb in lubricating oil is presented. The x-ray fluorescence (WDXRF) technique using linear regression method and thin film sample preparation was used. The validation of the methodology (repeatability and accuracy) was obtained by the analysis of the standard reference materials SRM Alpha AESAR lot 703527D, applying the Chauvenet, Cochrane, ANOVA and Z-score statistical tests. The method presents a relative standard deviation lower than 10% for all the elements, except for Pb determination (RSD Pb 15%). The Z-score values for all the elements were in the range -2 < Z < 2, indicating a very good accuracy.(Full text)

  17. Micro-scaled high-throughput digestion of plant tissue samples for multi-elemental analysis

    Directory of Open Access Journals (Sweden)

    Husted Søren

    2009-09-01

    Full Text Available Abstract Background Quantitative multi-elemental analysis by inductively coupled plasma (ICP spectrometry depends on a complete digestion of solid samples. However, fast and thorough sample digestion is a challenging analytical task which constitutes a bottleneck in modern multi-elemental analysis. Additional obstacles may be that sample quantities are limited and elemental concentrations low. In such cases, digestion in small volumes with minimum dilution and contamination is required in order to obtain high accuracy data. Results We have developed a micro-scaled microwave digestion procedure and optimized it for accurate elemental profiling of plant materials (1-20 mg dry weight. A commercially available 64-position rotor with 5 ml disposable glass vials, originally designed for microwave-based parallel organic synthesis, was used as a platform for the digestion. The novel micro-scaled method was successfully validated by the use of various certified reference materials (CRM with matrices rich in starch, lipid or protein. When the micro-scaled digestion procedure was applied on single rice grains or small batches of Arabidopsis seeds (1 mg, corresponding to approximately 50 seeds, the obtained elemental profiles closely matched those obtained by conventional analysis using digestion in large volume vessels. Accumulated elemental contents derived from separate analyses of rice grain fractions (aleurone, embryo and endosperm closely matched the total content obtained by analysis of the whole rice grain. Conclusion A high-throughput micro-scaled method has been developed which enables digestion of small quantities of plant samples for subsequent elemental profiling by ICP-spectrometry. The method constitutes a valuable tool for screening of mutants and transformants. In addition, the method facilitates studies of the distribution of essential trace elements between and within plant organs which is relevant for, e.g., breeding programmes aiming at

  18. Multi-element analysis for environmental characterization and its future trends

    International Nuclear Information System (INIS)

    Sansoni, B.

    1987-04-01

    Before starting to characterize the environment by its elemental composition, it may be useful to ask about the objective of these efforts. This includes questions about the scope of environmental protection, the definition of the environment and the limitations of its characterization by elemental composition alone. In the second part of this lecture, examples are given of the elemental composition of well analysed samples from the atmosphere, hydrosphere, lithosphere and biosphere. The third part introduces the principle of multi-element analysis and the fourth part gives examples. Finally, future aspects of modern chemical analysis are outlined with respect to the multi-element principle. (orig.)

  19. Multi-element analysis of unidentified fallen objects from Tatale in ...

    African Journals Online (AJOL)

    A multi-element analysis has been carried out on two fallen objects, # 01 and # 02, using instrumental neutron activation analysis technique. A total of 17 elements were identified in object # 01 while 21 elements were found in object # 02. The two major elements in object # 01 were Fe and Mg, which together constitute ...

  20. Multi-element RIMS Analysis of Genesis Solar Wind Collectors

    Science.gov (United States)

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

    2009-12-01

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

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

    DEFF Research Database (Denmark)

    Götze, Ramona; Astrup, Thomas Fruergaard

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

  2. Multi-element analysis of small biological samples

    International Nuclear Information System (INIS)

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

    1983-01-01

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

  3. Head of detector for multi-element analysis

    International Nuclear Information System (INIS)

    Frynta, Z.

    1983-01-01

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

  4. Multi-element neutron activation analysis of Brazilian coal samples

    International Nuclear Information System (INIS)

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

    1982-09-01

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

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

    International Nuclear Information System (INIS)

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

    1998-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2003-09-01

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

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

    Science.gov (United States)

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

    2018-01-01

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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

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

    International Nuclear Information System (INIS)

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

    1983-01-01

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

  10. 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)

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

    Science.gov (United States)

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

    2015-01-07

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

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

    CERN Document Server

    Lin Yan Chang; Lai Wan Chang; Zhou Si Chun

    2002-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-07-01

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

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

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

    Science.gov (United States)

    Xiao, Heng; Gou, Xiaolong; Yang, Suwen

    2011-05-01

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

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

    Science.gov (United States)

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

    2015-06-01

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

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

    International Nuclear Information System (INIS)

    Wall, G.J.

    1985-01-01

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

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

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

    International Nuclear Information System (INIS)

    Hilpert, K.; Waidmann, E.

    1988-01-01

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-05-15

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

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

    Directory of Open Access Journals (Sweden)

    Michael O’Connor

    2010-05-01

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

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    International Nuclear Information System (INIS)

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

    1997-01-01

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

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

  7. 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)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-09-03

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

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

    International Nuclear Information System (INIS)

    Foo, Jasmine; Wan Xiaoliang; Karniadakis, George Em

    2008-01-01

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

  10. Multi-element analysis of the obese subject by in vivo neutron activation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Siwek, R A; Burkinshaw, L; Oxby, C B [Leeds General Infirmary (UK); Robinson, P A.J. [Saint James' s University Hospital, Leeds (UK)

    1984-06-01

    The Leeds facility for in vivo neutron activation analysis has been modified and calibrated for the simultaneous measurement of nitrogen, potassium, sodium, chlorine, phosphorus and calcium in obese patients weighing up to 210 kg. The effects of body size and shape were incorporated into the calibration by measuring 14 anthropomorphic phantoms of known composition representing individual patients being treated for obesity. The phantoms were constructed from tissue substitutes representing lean skeletal and adipose tissues, arranged to simulate the distributions of the corresponding tissues within the patients, as visualised by CT scanning. The precision of the method, determined by measuring a single phantom ten times over a period of ten weeks, is between two and three per cent for all elements except calcium, for which it is 11.3%. Accuracy is estimated to be similar to precision. The procedure has been used to study changes in body composition of patients undergoing therapeutic starvation.

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

    International Nuclear Information System (INIS)

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

    2016-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-07-01

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

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

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

    International Nuclear Information System (INIS)

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

    2017-01-01

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

  15. Applications of total reflection X-ray fluorescence in multi-element analysis

    International Nuclear Information System (INIS)

    Michaelis, W.; Prange, A.; Knoth, J.

    1985-01-01

    Although Total Reflection X-Ray Fluorescence Analysis (TXRF) became available for practical applications and routine measurements only few years ago, the number of programmes that make use of this method is increasing rapidly. The scope of work is widespread over environmental research and monitoring, mineralogy, mineral exploration, oceanography, biology, medicine and biochemistry. The present paper gives a brief survey of these applications and summarizes some of them which are typical for quite different matrices. (orig.)

  16. Performance evaluation of the ORNL multi-elemental XRF analysis algorithms

    Energy Technology Data Exchange (ETDEWEB)

    McElroy, Robert Dennis [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2016-11-01

    Hybrid K-Edge Densitometer (HKED) systems integrate both K-Edge Densitometry (KED) and X-Ray Fluorescence (XRF) analyses to provide accurate rapid, assay results of the uranium and plutonium content of dissolver solution samples from nuclear fuel reprocessing facilities. Introduced for international safeguards applications in the late 1980s, the XRF component of the hybrid analyses is limited to quantification of U and Pu over a narrow range of U:Pu concentration ratios in the vicinity of ≈100. The analysis was further limited regarding the presence of minor actinide components where only a single minor actinide (typically Am) is included in the analysis and then only treated as an interference. The evolving nuclear fuel cycle has created the need to assay more complex dissolver solutions where uranium may no longer be the dominant actinide in the solution and the concentrations of the so called minor actinides (e.g., Th, Np, Am, and Cm) are sufficiently high that they can no longer be treated as impurities and ignored. Extension of the traditional HKED Region of Interest (ROI) based analysis to include these additional actinides is not possible due to the increased complexity of the XRF spectra. Oak Ridge National Laboratory (ORNL) has developed a spectral fitting approach to the HKED XRF measurement with an enhanced algorithm set to accommodate these complex XRF spectra. This report provides a summary of the spectral fitting methodology and examines the performance of these algorithms using data obtained from the ORNL HKED system, as well as data provided by the International Atomic Energy Agency (IAEA) on actual dissolver solutions.

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

    International Nuclear Information System (INIS)

    Godinez A, M.A.

    1994-01-01

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

  18. Aspects of cleaning environmental materials for multi-element analysis, e.g. plant samples

    International Nuclear Information System (INIS)

    Markert, B.

    1992-01-01

    Cleaning of samples is often the first step in the entire procedure of sample preparation in environmental trace element research. The question must generally be raised of whether cleaning is meaningful before chemical investigations with plant material (e.g. for the determination of transfer factors in the soil/plant system) or not (e.g. for food chain analysis in the plant/animal system). The most varied cleaning procedures for plant samples are currently available ranging from dry and wet wiping of the leaf or needle surface up to the complete removal of the cuticule with the aid of chlorofom. There is at present no standardized cleaning procedure for plant samples so that it is frequently not possible to compare analytical data from different working groups studying the same plant species. (orig.)

  19. Tracking transformation processes of organic micropollutants in aquatic environments using multi-element isotope fractionation analysis

    International Nuclear Information System (INIS)

    Hofstetter, Thomas B.; Bolotin, Jakov; Skarpeli-Liati, Marita; Wijker, Reto; Kurt, Zohre; Nishino, Shirley F.; Spain, Jim C.

    2011-01-01

    The quantitative description of enzymatic or abiotic transformations of man-made organic micropollutants in rivers, lakes, and groundwaters is one of the major challenges associated with the risk assessment of water resource contamination. Compound-specific isotope analysis enables one to identify (bio)degradation pathways based on changes in the contaminants' stable isotope ratios even if multiple reactive and non-reactive processes cause concentrations to decrease. Here, we investigated how the magnitude and variability of isotope fractionation in some priority pollutants is determined by the kinetics and mechanisms of important enzymatic and abiotic redox reactions. For nitroaromatic compounds and substituted anilines, we illustrate that competing transformation pathways can be assessed via trends of N and C isotope signatures.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-11-23

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

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    International Nuclear Information System (INIS)

    Rossini, I.

    1991-06-01

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

  3. Authentication of organically grown plants - advantages and limitations of atomic spectroscopy for multi-element and stable isotope analysis

    DEFF Research Database (Denmark)

    Laursen, Kristian Holst; Schjørring, Jan Kofod; Kelly, S.D.

    2014-01-01

    Organic food products are believed to be healthier, safer and more environment-friendly than their conventional counterparts and are sold at premium prices. Consequently, adulteration of organic plants and fraudulent activities for economic profit are increasing. This has spurred the development...... plant tissue, and compound-specific isotope analysis based on isotope ratio-mass spectrometry are promising tools for documenting the fertilization history of organic plants. However, these techniques are challenged by the potential diversity of fertilization practices of organic and conventional plant...

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-05-01

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

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

    International Nuclear Information System (INIS)

    Zhuravleva, E.L.

    1980-01-01

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

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

    Science.gov (United States)

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

    2018-04-01

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

  8. 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

  9. 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...

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

    International Nuclear Information System (INIS)

    Vermaercke, P.

    2007-01-01

    determined by the nuclear cross sections. The cross sections depend on the neutron energy E and also these physical properties are parameterised in the k0-NAA method resulting in the so-called k0-factors for each element and for the different isotopes of an element. The quantification of an element then involves the use of a ratio of k0-factors in which one k0-factor is the one for 198Au. In practice, ratios of k0-factors accounting for the energy spectrum of the neutrons (f, a) are used in an analysis. These ratios are called the comparator factor FC. It is clear that the quality assurance of the k0-NAA method requires the control of the parameters f and a for each irradiation of samples. This is generally realised by using several flux monitors e.g. a set of Zr and Au monitors which are co-irradiated with the samples to analyse. However, this approach is quite labour intensive and recently we started investigating an approach based on co-irradiation of Synthetic Multi-Element Standards (SMELS) for this purpose. SMELS contain different elements in known concentrations, and three types of materials exist: Type I (elements forming short-lived radionuclides), Type II (elements forming medium lived radionuclides) and Type III (elements forming long lived radionuclides). Au was added to all three SMELS types and Zr in type III. The objectives are to optimise the ratio of quality of analysis to workload by appropriate quality control methods to determine and monitor the irradiation parameters (f, a) using SMELS and to set up a Quality Control (QC) system for the complete measurement and analysis process for k0-NAA

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

    International Nuclear Information System (INIS)

    Adeyemo, D.J.

    2004-01-01

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

  12. Materials characterization of radioactive waste forms using a multi-element detection method based on the instrumental neutron activation analysis. MEDINA; Stoffliche Charakterisierung radioaktiver Abfallprodukte durch ein Multi-Element-Analyseverfahren basierend auf der instrumentellen Neutronen-Aktivierungs-Analyse. MEDINA

    Energy Technology Data Exchange (ETDEWEB)

    Havenith, Andreas Wilhelm

    2015-07-01

    Radioactive waste has to meet the specifications and acceptance criteria defined by national regulatory and management authorities for its intermediate and final storage. In Germany the Federal Office for Radiation Protection (Bundesamt fuer Strahlenschutz - BfS) has established waste acceptance requirements for the Konrad repository. Konrad is the disposal for radioactive waste with negligible heat generation and is located near the city of Salzgitter and is currently under construction. It will start operation not before the year 2021. The waste-acceptance-requirements are derived from a site-specific safety assessment. They include specific requirements on waste forms, packaging as well as limitations to activities of individual radionuclides and limitations to masses of non-radioactive harmful substances. The amount of chemically toxic elements in the waste is limited in order to avoid pollution of underground water reserves. To comply with these requirements every waste package has to be characterised in its radiological and chemical composition. This characterisation can be performed on the basis of existing documentation or, if the documentation is insufficient, on further analytical analysis. Segmented or integral gamma-scanning as well as active or passive neutron counting are used worldwide as the standard measurement methods for the radiological characterisation and quality checking of radioactive waste. These techniques determine the isotope specific activity of waste packages, but they do not allow the detection of non-radioactive hazardous substances inside the waste packages. Against this background the Institute of Nuclear Engineering and Technology Transfer (NET) at RWTH Aachen University and the Institute of Safety Research and Reactor Technology at Forschungszentrum Juelich jointly develop an innovative non-destructive analytical technique called MEDINA - ''Multi-Element Detection based on Instrumental Neutron Activation'' for

  13. Multi-element analysis of bone from the osteogenesis imperfecta model (OIM) mouse using thermal and fast neutron activation analysis

    International Nuclear Information System (INIS)

    Huntington, C.E.; Morris, J.S.; Carleton, S.M.; McBride, D.J.; Phillips, C.L.

    2008-01-01

    Osteogenesis imperfecta (OI) is a heritable osteoporotic bone disease, due to defects in either type I procollagen genes (COL1A1 or COL1A2), resulting in abnormal and/or reduced levels of type I procollagen and alterations in bone mineralization. Our long term objectives are to evaluate the impact of proα1(I) and proα2(I) collagen mutations and the role of the genetic background on bone mineralization. Tibias from wildtype, heterozygous (oim/+), and homozygous (oim/oim) animals were subjected to instrumental neutron activation analysis (INAA) to measure F, P, Na, Mg, Cl, Ca, K, and Zn using the University of Missouri Research Reactor (MURR) pneumatic-tube irradiation facility. (author)

  14. Geographic authentication of Asian rice (Oryza sativa L.) using multi-elemental and stable isotopic data combined with multivariate analysis.

    Science.gov (United States)

    Chung, Ill-Min; Kim, Jae-Kwang; Lee, Kyoung-Jin; Park, Sung-Kyu; Lee, Ji-Hee; Son, Na-Young; Jin, Yong-Ik; Kim, Seung-Hyun

    2018-02-01

    Rice (Oryza sativa L.) is the world's third largest food crop after wheat and corn. Geographic authentication of rice has recently emerged asan important issue for enhancing human health via food safety and quality assurance. Here, we aimed to discriminate rice of six Asian countries through geographic authentication using combinations of elemental/isotopic composition analysis and chemometric techniques. Principal components analysis could distinguish samples cultivated from most countries, except for those cultivated in the Philippines and Japan. Furthermore, orthogonal projection to latent structure-discriminant analysis provided clear discrimination between rice cultivated in Korea and other countries. The major common variables responsible for differentiation in these models were δ 34 S, Mn, and Mg. Our findings contribute to understanding the variations of elemental and isotopic compositions in rice depending on geographic origins, and offer valuable insight into the control of fraudulent labeling regarding the geographic origins of rice traded among Asian countries. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

    Kemp, K.; Danscher, G.

    1979-01-22

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

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

    International Nuclear Information System (INIS)

    Gaudry, Andre.

    1975-01-01

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

  17. Neutron activation analysis on sediments from Victoria Land, Antarctica. Multi-elemental characterization of potential atmospheric dust sources

    International Nuclear Information System (INIS)

    Baccolo, G.; Maggi, V.; Baroni, C.; Clemenza, M.; Motta, A.; Nastasi, M.; Previtali, E.; University of Milano-Bicocca, Milan; Delmonte, B.; Salvatore, M.C.

    2014-01-01

    The elemental composition of 40 samples of mineral sediments collected in Victoria Land, Antarctica, in correspondence of ice-free sites, is presented. Concentration of 36 elements was determined by instrumental neutron activation analysis, INAA. The selection of 6 standard reference materials and the development of a specific analytical procedure allowed to reduce measurements uncertainties and to verify the reproducibility of the results. The decision to analyze sediment samples from Victoria Land ice-free areas is related to recent investigations regarding mineral dust content in the TALos Dome ICE core (159deg11'E; 72deg49'S, East Antarctica, Victoria Land), in which a coarse local fraction of dust was recognized. The characterization of Antarctic potential source areas of atmospheric mineral dust is the first step to identify the active sources of dust for the Talos Dome area and to reconstruct the atmospheric pathways followed by air masses in this region during different climatic periods. Principal components analysis was used to identify elements and samples correlations; attention was paid specially to rare earth elements (REE) and incompatible/compatible elements (ICE) in respect to iron, which proved to be the most discriminating elemental groups. The analysis of REE and ICE concentration profiles supported evidences of chemical weathering in ice-free areas of Victoria Land, whereas cold and dry climate conditions of the Talos Dome area and in general of East Antarctica. (author)

  18. Determination of multi-element composition of Vietnamese marine sediment and tuna fish by k0-standardized neutron activation analysis

    International Nuclear Information System (INIS)

    Manh-Dung Ho; Quang-Thien Tran; Van-Doanh Ho; Thi-Sy Nguyen

    2016-01-01

    The k 0 -standardized neutron activation analysis (k 0 -NAA) has been applied for determination of multiple elements (25 elements: Al, As, Ba, Br, Ca, Cl, Co, Cr, Cs, Cu, Eu, Fe, Hg, K, La, Mg, Na, Rb, Sc, Se, Sm, Th, Ti, V and Zn) in marine sediment and tuna fish. About 50 marine sediment and 9 tuna fish samples were collected in two coastal areas of Vietnam. The health risk index (HRI) values of As and Br were higher than 1.0 for the tuna fish. Also, HRI value of Hg was 8.92 × 10 -1 indicating a relatively high potential health risk, whiles Co and Mn with HRIs = 1.56 × 10 -4 and 8.56 × 10 -4 , respectively, have the lowest potential health risks. Average enrichment factors using Al as a reference element (EF Al ) were higher than 1.5 for Eu, La, Zn, Th, Cs and As in which the highest EF Al value for As was higher than 10. This study showed that the HRI value of As in the tuna fish correlated positively with the EF Al value for the element in the marine sediment. (author)

  19. 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

  20. 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.

  1. Materials characterization of radioactive waste forms using a multi-element detection method based on the instrumental neutron activation analysis. MEDINA

    International Nuclear Information System (INIS)

    Havenith, Andreas Wilhelm

    2015-01-01

    Radioactive waste has to meet the specifications and acceptance criteria defined by national regulatory and management authorities for its intermediate and final storage. In Germany the Federal Office for Radiation Protection (Bundesamt fuer Strahlenschutz - BfS) has established waste acceptance requirements for the Konrad repository. Konrad is the disposal for radioactive waste with negligible heat generation and is located near the city of Salzgitter and is currently under construction. It will start operation not before the year 2021. The waste-acceptance-requirements are derived from a site-specific safety assessment. They include specific requirements on waste forms, packaging as well as limitations to activities of individual radionuclides and limitations to masses of non-radioactive harmful substances. The amount of chemically toxic elements in the waste is limited in order to avoid pollution of underground water reserves. To comply with these requirements every waste package has to be characterised in its radiological and chemical composition. This characterisation can be performed on the basis of existing documentation or, if the documentation is insufficient, on further analytical analysis. Segmented or integral gamma-scanning as well as active or passive neutron counting are used worldwide as the standard measurement methods for the radiological characterisation and quality checking of radioactive waste. These techniques determine the isotope specific activity of waste packages, but they do not allow the detection of non-radioactive hazardous substances inside the waste packages. Against this background the Institute of Nuclear Engineering and Technology Transfer (NET) at RWTH Aachen University and the Institute of Safety Research and Reactor Technology at Forschungszentrum Juelich jointly develop an innovative non-destructive analytical technique called MEDINA - ''Multi-Element Detection based on Instrumental Neutron Activation'' for

  2. Multi Elemental Study Using Prompt Gamma Technique

    International Nuclear Information System (INIS)

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

    2016-01-01

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

  3. Neutron activation spectrometry and neutron activation analysis in analytical geochemistry

    International Nuclear Information System (INIS)

    Dulski, P.; Moeller, P.

    1975-07-01

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

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

    International Nuclear Information System (INIS)

    Enomoto, Shuichi

    2003-01-01

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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

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

    Science.gov (United States)

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

    2007-10-01

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

  7. Statistical Analysis of the Spatial Distribution of Multi-Elements in an Island Arc Region: Complicating Factors and Transfer by Water Currents

    Directory of Open Access Journals (Sweden)

    Atsuyuki Ohta

    2017-01-01

    Full Text Available The compositions and transfer processes affecting coastal sea sediments from the Seto Inland Sea and the Pacific Ocean are examined through the construction of comprehensive terrestrial and marine geochemical maps for western Japan. Two-way analysis of variance (ANOVA suggests that the elemental concentrations of marine sediments vary with particle size, and that this has a greater effect than the regional provenance of the terrestrial material. Cluster analysis is employed to reveal similarities and differences in the geochemistry of coastal sea and stream sediments. This analysis suggests that the geochemical features of fine sands and silts in the marine environment reflect those of stream sediments in the adjacent terrestrial areas. However, gravels and coarse sands do not show this direct relationship, which is likely a result of mineral segregation by strong tidal currents and the denudation of old basement rocks. Finally, the transport processes for the fine-grained sediments are discussed, using the spatial distribution patterns of outliers for those elements enriched in silt and clay. Silty and clayey sediments are found to be transported and dispersed widely by a periodic current in the inner sea, and are selectively deposited at the boundary of different water masses in the outer sea.

  8. Multi-element analysis of wheat flour and white bread by neutron activation.; Analisis multielemental en harina de trigo y pan blanco por activacion neutronica.

    Energy Technology Data Exchange (ETDEWEB)

    Godinez A, M A

    1994-12-31

    One of the best source of feeding even for the human being as for animals are the Cereals. Although they are mainly energetic aliment, due to its composition in starch, they are a very important source of proteins and amino acids. They contribute mineral elements to the diet. Even those elements constitute a very small part of the total diet, they take a very important place in many human metabolic processes. To make a multielemental analysis of an aliment is very important that we are based on a very sensible analytic technique so we are able to find them, just as the Neutronic Activation. This Nuclear technique allows you to make a qualitative and quantitative analysis of the elements that are in a sample, but it does n`t show the way in which the elements are presented. It is based in turning those elements into radioactive ones through its exposition to an uniform and constant fluid of neutrons, so then its radioactivity can be determined. The present work has as a main purpose to make a multielemental analysis of the wheat flour and white bread through the Neutronic Activation Technique, using the comparator method and establishing previously the most appropriate work conditions as much irradiation as digestion and measuring of the radioactivity of the sample. In this way, it was able to know that the wheat flour has potassium, chlorine, magnesium, sodium, iron, zinc, manganese, rubidium and selenium elements in a concentration of 2000, 700, 500, 25, 18, 13, 5.5, 0.9 and 0.01 - 0.3 mg/g respectively. In an other hand it was found that the white bread has the same elements than the wheat flour but its concentration was: 1700, 9000, 400, 7000, 52, 13, 6, 1 and 0.05 - 0.3 mg/g respectively. (Author).

  9. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-10-15

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

  11. 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

  12. Multi-element probabilistic collocation method in high dimensions

    International Nuclear Information System (INIS)

    Foo, Jasmine; Karniadakis, George Em

    2010-01-01

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

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

    Science.gov (United States)

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

    2013-08-11

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-09-01

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  16. 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....

  17. Multi-Element Lean Direct Injection Combustor Module, Phase I

    Data.gov (United States)

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

  18. Chemical analysis of refractories by plasma spectrometry

    International Nuclear Information System (INIS)

    Coutinho, C.A.

    1990-01-01

    X-ray spectrometry has been, since the last two or three decades, the traditional procedure for the chemical analysis of refractories, due to its high degree of accuracy and speed to produce analytical results. An interesting alternative to X-ray fluorescence is provided by the Inductively Coupled Plasma Spectrometry technique, for those laboratories where wet chemistry facilities are already available or process control is not required at high speed, or investiment costs have to be low. This paper presents results obtained by plasma spectroscopy for the analysis of silico - aluminous refractories, showing calibration curves, precion and detection limits. Considerations and comparisons with X-ray fluorescence are also made. (author) [pt

  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. 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.

  1. MULTI ELEMENT SI SENSOR WITH READOUT ASIC FOR EXAFS SPECTROSCOPY.

    Energy Technology Data Exchange (ETDEWEB)

    DE GERONIMO,G.; O CONNOR,P.; BEUTTENMULLER,R.H.; LI,Z.; KUCZEWSKI,A.J.; SIDDONS,D.P.

    2002-09-09

    Extended X-ray Absorption Fine Structure (EXAFS) experiments impose stringent requirements on a detection system, due to the need for processing ionizing events at a high rate, typically above of 10Mcps/cm{sup 2}, and with a high resolution, typically better than 300eV. The detection system here presented is being developed targeting these stringent requirements. It is the result of a cooperation between the Instrumentation Division and the National Synchrotron Light Source (NSLS) of the Brookhaven National Laboratory (BNL). The system is composed of a multi-element Si sensor with dedicated per pixel electronics. The combination of high rate, high resolution and moderate complexity makes this system attractive when compared to other multi-element solutions. In sections 2, 3 and 4 the sensor, the interconnect and the electronics are briefly described. Section 5 reports on the first experimental results.

  2. Wideband multi-element Er-doped fiber amplifier

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    Science.gov (United States)

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

    2018-01-01

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

  4. 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

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

    International Nuclear Information System (INIS)

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

    2000-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

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

    2006-01-01

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

  7. 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

  8. 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

  9. Multi-element proportional counter for radiation protection measurements

    International Nuclear Information System (INIS)

    Kliauga, P.; Rossi, H.H.; Johnson, G.

    1988-01-01

    This article discusses design modifications of a multi-element proportional counter. The original counter exhibited poor resolution, as measured by the width of the event-size spectrum for low-energy photons. It was also suspected that the field inside each volume was not sufficiently symmetric. Results of the modifications showed that a dramatic improvement in resolution could be obtained in the chamber with tissue-equivalent septa if their potentials were adjusted to obtain optimal resolution. The full width at half maximum then approached, although it did not equal, that of a standard spherical counter

  10. Performance Test of Alpha Spectrometry for Environmental Radioactivity Analysis

    International Nuclear Information System (INIS)

    Choi, Jung Youn; Yoon, Jong-Ho; Han, Ki-Tek; Ahn, Gil Hoon

    2015-01-01

    Environmental samples are analyzed by various methods such as, ICP-MS (inductively coupled plasma mass spectrometry), AMS (accelerator mass spectrometry) TIMS (thermal ionization mass spectrometry), HRGS (high resolution gamma spectrometry) and alpha /beta particle analysis. In this study, we will described the result of performance test using alpha spectrometry for analyzing environmental samples. Measurement data of the U activity using SRM based on extraction chromatography with UTEVA resin. It should be effective way to separate of uranium isotope for the measurement of alpha spectrometry. But, the result of this measurement data is higher than another recovery data. Also concentration of U data is lack of consistency. We leave out of consideration many effect of factors about influence in the experiment process. In the future work, we will try to reduce the step of experiment process and reflect the uncertainty factors

  11. 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...

  12. 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

  13. 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

  14. Elemental characterization of herbal medicines used in Ghana by instrumental neutron activation analysis and atomic absorption spectrometry and multivariate statistical analysis

    International Nuclear Information System (INIS)

    Ayivor, J.E.; Nyarko, B.J.B.; Dampare, S.B.; Okine, L.K.

    2010-01-01

    k 0 instrumental neutron activation analysis and atomic absorption spectrometry were applied to determine multi elements in thirteen Ghanaian herbal medicines used for the management of various diseases. Concentrations of AI, Cu, Mg, Mn and Na were determined. As, Br, K, CI, and Na were determined by short and medium irradiations at a thermal neutron flux of 5x10ncm -2 s -1 . Fe, Cr, Pb, Co, Ni, Sn, Ca, Ba, Li and Sb were determined using atomic absorption spectrometry. Ba, Cu, Li and V were present at trace levels whereas AI, CI, Na, Ca were present at major levels. K, Br, Mg, Mn, Co, Ni, Fe and Sb were also present at minor levels. The precision and accuracy of the method using real samples and standard reference materials were within ±10% of the reported value. Multivariate analytical techniques, such as cluster analysis and principal component analysis (PCA)/factor analysis (FA), have been applied to evaluate the chemical variations in the herbal medicine dataset. All the 13 samples may be grouped into two statistically significant clusters, reflecting the different chemical compositions. The concentrations of elements were within the recommended daily allowances or maximum permissible levels posing no adverse effects on human health.

  15. Regional and global atmospheric aerosol studies using the ''Gent'' stacked filter unit sampler and other aerosol collectors, with multi-elemental analysis of the samples by nuclear-related analytical techniques

    International Nuclear Information System (INIS)

    Maenhaut, W.; Francois, F.; Salma, I.; Cafmeyer, J.; Gilot, C.

    1994-01-01

    The ''Gent'' staked filter unit sampler and other collection devices are used in regional and global scale studies on the tropospheric atmospheric aerosols, its composition, sources and fate. The aerosol samples are analyzed by particle-induced X-ray emission analysis, instrumental neutron activation analysis, ion chromatography, a light reflectance technique (for determining black carbon), and gravimetry (for measuring the particular mass). In evaluating the data, use is made of receptor modelling techniques, transport models and wind sector analysis, and also of air mass trajectories and other meteorological information. Preliminary results from a long-term study in southern Norway are presented. It is suggested that the anthropogenic and soil dust aerosol components are mainly adverted to southern Norway by long-range transport and that the major fraction of the submicrometer particle mass is from anthropogenic origin. Preliminary results are also presented for an intensive study in southern Africa. On the basis of the data for two sites (about 40 km apart) in the Kruger National Park it was concluded that regionally representative aerosol samples were collected and that the biomass burning products account for more than 50% of the fine particle mass. Finally, our plans for future work are given. (author). 70 refs, 4 figs, 1 tab

  16. Multi-element isotope dilution analyses using ICP-MS

    International Nuclear Information System (INIS)

    Volpe, A.M.

    1996-01-01

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

  17. Atmospheric aerosol studies using the 'Gent' stacked filter unit and other aerosol collectors, with multi-elemental analysis of the samples by nuclear-related analytical techniques. Appendix 4

    International Nuclear Information System (INIS)

    Maenhaut, Willy; Francois, Filip; Cafmeyer, Jan; Okunade, Olusola

    1995-01-01

    Our research within the core programme of the Co-ordinated Research Programme (CRP) on Air Pollution is described. This included the analysis of the analytical quality control Nuclepore filter samples, work on the calibration of the PM10 inlet of the 'Gent' stacked filter unit (SFU) sampler, and an aerosol study with this SFU sampler at an urban residential site in Gent. The calibration of the Gent PM10 inlet was done through intercomparisons with commercially available PM10 samplers, and quite reasonable agreement was obtained. For the study at the urban residential site, a total of 118 SFU samples were collected. The samples were analyzed for the particulate mass, black carbon and up to 29 elements. The elements were measured by PIXE and short-irradiation INAA. Median atmospheric concentrations and enrichment factors were calculated for the fine and coarse size fractions, and average FINE/COARSE ratios were derived. The median concentrations were compared with those from a study, done at the same site in the fall of 1986. The levels of the automotive elements Pb and Br had decreased by a factor of about three relative to 1986, but most other elements exhibited very similar concentrations. A brief overview is given of the status in our various regional and global scale aerosol studies. Finally, our plans for future work are given. (author)

  18. Arbeitsgemeinschaft fuer die Reinhaltung der Elbe - multi-element analysis of water samples from the Elbe and selected tributaries; Arbeitsgemeinschaft fuer die Reinhaltung der Elbe - Multielementanalysen von Wasserproben der Elbe und ausgewaehlter Nebenfluesse. Laengsprofilbeprobung vom September 1997

    Energy Technology Data Exchange (ETDEWEB)

    Krueger, F.; Berger, H. [Umweltbehoerde Hamburg (Germany). Amt fuer Umweltschutz, Umweltuntersuchungen; Aulinger, A.; Stachel, B.; Reincke, H. [Wasserguetestelle Elbe, Hamburg (Germany)

    2000-10-01

    This special report focuses on measurements of elements whose scope goes far beyond the routine monitoring for metals. The present studies are intended to extend the existing knowledge on the pollution situation of the Elbe and certain of its tributaries as well as provide a basis for formulating future guidelines for action. The first step towards this goal is sampling by means of an helicopter. The sampling is followed by a very involved and costly analysis programme, accompanied by extensive quality assurance measures. This is the only way of reliably analysing a large number of elements occurring in extremely low concentrations. Once the data have been recorded the question arises how they are to be evaluated. What schemes are suitable for categorising a large number of elements measured in either the suspended matter or the water compartment? What elements are to be regarded as the result of anthropogenic influences and what are their respective background concentrations in the fluvial system under study? These questions are approached by means of statistical methods which permit identifying elemental patterns and pollution sources as well as optimising the selection of measuring points for future studies. [German] In diesem Sonderbericht steht die Bestimmung von Elementen, die in ihrem Umfang ueber die routinemaessig erfassten Metalle deutlich hinausgeht, im Vordergrund. Die vorliegenden Untersuchungen sollen das bereits vorhandene Wissen zur Beschreibung der Immissionssituation der Elbe und von bestimmten Nebenfluessen erweitern, verbunden mit der Moeglichkeit, zukuenftige Handlungsmaximen zu erarbeiten. Zur Erreichung dieses Ziels steht zu Beginn die Probenahme mit einem Helicopter. Im Anschluss an die Probenahme folgt eine sehr aufwendige und teure Analytik, die begleitet wird von umfassenden Massnahmen zur Qualitaetssicherung. Nur so ist es moeglich, eine grosse Vielzahl von Elementen in extrem niedrigen Konzentrationen sicher analysieren zu koennen. Sind

  19. Minicomputer system for radiochemical analysis by coincidence spectrometry

    International Nuclear Information System (INIS)

    Brauer, F.P.; Fager, J.E.

    1979-01-01

    Minicomputer-based coincidence analysis methods have been developed for use in performing radiochemical analysis by high-resolution x- and gamma-ray coincidence spectrometry. This paper describes the data-acquisition and analysis methods develolped for qualitative and quantitative analyses of coincidence spectrometric data. Data-acquisition capabilities include both direct multiparameter pulse-height analysis and buffered list-mode acquisition

  20. Flow injection analysis in inductively coupled plasma spectrometry

    International Nuclear Information System (INIS)

    Rosias, Maria F.G.G.

    1995-10-01

    The main features of flow injection analysis (FIA) as contribution to the inductively coupled plasma (Icp) spectrometry are described. A systematic review of researches using the combined FIA-Icp and the benefits of this association are presented. Flow systems were proposed to perform on-line Icp solution management for multielemental determination by atomic emission spectrometry (Icp-AES) or mass spectrometry. The inclusion of on-line ion exchangers in flow systems for matrix separation and/or analyte preconcentration are presented. Together with those applications the new advent of instruments with facilities for multielement detection on flow injection signals are described. (author). 75 refs., 19 figs

  1. 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....

  2. Studies on absorption coefficient near edge of multi elements

    International Nuclear Information System (INIS)

    Eisa, M.H.; Shen, H.; Yao, H.Y.; Mi, Y.; Zhou, Z.Y.; Hu, T.D.; Xie, Y.N.

    2005-01-01

    X-ray absorption near edge structure (XANES) was used to study the near edge mass-absorption coefficients of seven elements, such as, Ti, V, Fe, Co, Ni, Cu and Zn. It is well known that, on the near edge absorption of element, when incident X-ray a few eV change can make the absorption coefficient an order magnitude alteration. So that, there are only a few points mass-absorption coefficient at the near edge absorption and that always average value in published table. Our results showed a wide range of data, the total measured data of mass-absorption coefficient of the seven elements was about 505. The investigation confirmed that XANES is useful technique for multi-element absorption coefficient measurement. Details of experimental methods and results are given and discussed. The experimental work has been performed at Beijing Synchrotron Radiation Facility. The measured values were compared with the published data. Good agreement between experimental results and published data is obtained

  3. Studies on absorption coefficient near edge of multi elements

    Science.gov (United States)

    Eisa, M. H.; Shen, H.; Yao, H. Y.; Mi, Y.; Zhou, Z. Y.; Hu, T. D.; Xie, Y. N.

    2005-12-01

    X-ray absorption near edge structure (XANES) was used to study the near edge mass-absorption coefficients of seven elements, such as, Ti, V, Fe, Co, Ni, Cu and Zn. It is well known that, on the near edge absorption of element, when incident X-ray a few eV change can make the absorption coefficient an order magnitude alteration. So that, there are only a few points mass-absorption coefficient at the near edge absorption and that always average value in published table. Our results showed a wide range of data, the total measured data of mass-absorption coefficient of the seven elements was about 505. The investigation confirmed that XANES is useful technique for multi-element absorption coefficient measurement. Details of experimental methods and results are given and discussed. The experimental work has been performed at Beijing Synchrotron Radiation Facility. The measured values were compared with the published data. Good agreement between experimental results and published data is obtained.

  4. Spectral response of multi-element silicon detectors

    Energy Technology Data Exchange (ETDEWEB)

    Ludewigt, B.A.; Rossington, C.S.; Chapman, K. [Univ. of California, Berkeley, CA (United States)

    1997-04-01

    Multi-element silicon strip detectors, in conjunction with integrated circuit pulse-processing electronics, offer an attractive alternative to conventional lithium-drifted silicon Si(Li) and high purity germanium detectors (HPGe) for high count rate, low noise synchrotron x-ray fluorescence applications. One of the major differences between the segmented Si detectors and the commercially available single-element Si(Li) or HPGe detectors is that hundreds of elements can be fabricated on a single Si substrate using standard silicon processing technologies. The segmentation of the detector substrate into many small elements results in very low noise performance at or near, room temperature, and the count rate of the detector is increased many-fold due to the multiplication in the total number of detectors. Traditionally, a single channel of detector with electronics can handle {approximately}100 kHz count rates while maintaining good energy resolution; the segmented detectors can operate at greater than MHz count rates merely due to the multiplication in the number of channels. One of the most critical aspects in the development of the segmented detectors is characterizing the charge sharing and charge loss that occur between the individual detector strips, and determining how these affect the spectral response of the detectors.

  5. Parameter Optimization of Multi-Element Synthetic Aperture Imaging Systems

    Directory of Open Access Journals (Sweden)

    Vera Behar

    2007-03-01

    Full Text Available In conventional ultrasound imaging systems with phased arrays, the further improvement of lateral resolution requires enlarging of the number of array elements that in turn increases both, the complexity and the cost, of imaging systems. Multi-element synthetic aperture focusing (MSAF systems are a very good alternative to conventional systems with phased arrays. The benefit of the synthetic aperture is in reduction of the system complexity, cost and acquisition time. In a MSAF system considered in the paper, a group of elements transmit and receive signals simultaneously, and the transmit beam is defocused to emulate a single element response. The echo received at each element of a receive sub-aperture is recorded in the computer memory. The process of transmission/reception is repeated for all positions of a transmit sub-aperture. All the data recordings associated with each corresponding pair "transmit-receive sub-aperture" are then focused synthetically producing a low-resolution image. The final high-resolution image is formed by summing of the all low-resolution images associated with transmit/receive sub-apertures. A problem of parameter optimization of a MSAF system is considered in this paper. The quality of imaging (lateral resolution and contrast is expressed in terms of the beam characteristics - beam width and side lobe level. The comparison between the MSAF system described in the paper and an equivalent conventional phased array system shows that the MSAF system acquires images of equivalent quality much faster using only a small part of the power per image.

  6. AC power flow importance measures considering multi-element failures

    International Nuclear Information System (INIS)

    Li, Jian; Dueñas-Osorio, Leonardo; Chen, Changkun; Shi, Congling

    2017-01-01

    Quantifying the criticality of individual components of power systems is essential for overall reliability and management. This paper proposes an AC-based power flow element importance measure, while considering multi-element failures. The measure relies on a proposed AC-based cascading failure model, which captures branch overflow, bus load shedding, and branch failures, via AC power flow and optimal power flow analyses. Taking the IEEE 30, 57 and 118-bus power systems as case studies, we find that N-3 analyses are sufficient to measure the importance of a bus or branch. It is observed that for a substation bus, its importance is statistically proportional to its power demand, but this trend is not observed for power plant buses. While comparing with other reliability, functionality, and topology-based importance measures popular today, we find that a DC power flow model, although better correlated with the benchmark AC model as a whole, still fails to locate some critical elements. This is due to the focus of DC-based models on real power that ignores reactive power. The proposed importance measure is aimed to inform decision makers about key components in complex systems, while improving cascading failure prevention, system backup setting, and overall resilience. - Highlights: • We propose a novel importance measure based on joint failures and AC power flow. • A cascading failure model considers both AC power flow and optimal power flow. • We find that N-3 analyses are sufficient to measure the importance of an element. • Power demand impacts the importance of substations but less so that of generators. • DC models fail to identify some key elements, despite correlating with AC models.

  7. 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.

  8. Alpha particle analysis using PEARLS spectrometry

    International Nuclear Information System (INIS)

    McKlveen, J.W.; Klingler, G.W.; McDowell, W.J.; Case, G.N.

    1984-01-01

    Alpha particle assay by conventional plate-counting methods is difficult because chemical separation, tracer techniques, and/or self-absorption losses in the final sample may cause either non-reproducible results or create unacceptable errors. PEARLS (Photon-Electron Rejecting Alpha Liquid Scintillation) Spectrometry is an attractive alternative since radionuclides may be extracted into a scintillator in which there would be no self-absorption or geometry problems and in which up to 100% chemical recovery and counting efficiency is possible. Sample preparation may include extraction of the alpha emitter of interest by a specific organic-phase-soluble compound directly into the liquid scintillator. Detection electronics use energy and pulse-shape discrimination to provide discrete alpha spectra and virtual absence of beta and gamma backgrounds. Backgrounds on the order of 0.01 cpm are readily achievable. Accuracy and reproducibility are typically in the 100 +-1% range. Specific procedures have been developed for gross alpha, uranium, plutonium, thorium, and polonium assay. This paper will review liquid scintillation alpha counting methods and reference some of the specific applications. 8 refs., 1 fig

  9. 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)

  10. Computer simulation of multi-elemental fusion reactor materials

    International Nuclear Information System (INIS)

    Voertler, K.

    2011-01-01

    Thermonuclear fusion is a sustainable energy solution, in which energy is produced using similar processes as in the sun. In this technology hydrogen isotopes are fused to gain energy and consequently to produce electricity. In a fusion reactor hydrogen isotopes are confined by magnetic fields as ionized gas, the plasma. Since the core plasma is millions of degrees hot, there are special needs for the plasma-facing materials. Moreover, in the plasma the fusion of hydrogen isotopes leads to the production of high energetic neutrons which sets demanding abilities for the structural materials of the reactor. This thesis investigates the irradiation response of materials to be used in future fusion reactors. Interactions of the plasma with the reactor wall leads to the removal of surface atoms, migration of them, and formation of co-deposited layers such as tungsten carbide. Sputtering of tungsten carbide and deuterium trapping in tungsten carbide was investigated in this thesis. As the second topic the primary interaction of the neutrons in the structural material steel was examined. As model materials for steel iron chromium and iron nickel were used. This study was performed theoretically by the means of computer simulations on the atomic level. In contrast to previous studies in the field, in which simulations were limited to pure elements, in this work more complex materials were used, i.e. they were multi-elemental including two or more atom species. The results of this thesis are in the microscale. One of the results is a catalogue of atom species, which were removed from tungsten carbide by the plasma. Another result is e.g. the atomic distributions of defects in iron chromium caused by the energetic neutrons. These microscopic results are used in data bases for multiscale modelling of fusion reactor materials, which has the aim to explain the macroscopic degradation in the materials. This thesis is therefore a relevant contribution to investigate the

  11. Chemical analysis of steel by optical emission spectrometry

    International Nuclear Information System (INIS)

    Hayakawa, M.O.; Kajita, T.; Jeszensky, G.

    1981-01-01

    The development of the chemical analysis for special steels by optical emission spectrometry direct reading method with computer, at the Siderurgica N.S. Aparecida S.A. is presented. Results are presented for the low alloy steels and high speed steel. Also, the contribution of this method to the special steel preparation is commented. (Author) [pt

  12. 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…

  13. X-ray fluorescence spectrometry applied to soil analysis

    International Nuclear Information System (INIS)

    Salvador, Vera Lucia Ribeiro; Sato, Ivone Mulako; Scapin Junior, Wilson Santo; Scapin, Marcos Antonio; Imakima, Kengo

    1997-01-01

    This paper studies the X-ray fluorescence spectrometry applied to the soil analysis. A comparative study of the WD-XRFS and ED-XRFS techniques was carried out by using the following soil samples: SL-1, SOIL-7 and marine sediment SD-M-2/TM, from IAEA, and clay, JG-1a from Geological Survey of Japan (GSJ)

  14. 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.

  15. 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

  16. Time of flight spectrometry in heavy ions backscattering analysis

    International Nuclear Information System (INIS)

    Chevarier, A.; Chevarier, N.

    1983-05-01

    Time of flight spectrometry for backscattering analysis of MeV heavy ions is proposed. The capabilities and limitations of this method are investigated. Depth and mass resolution obtained in measurements of oxide films thickness as well as in GaAs layers analysis are presented. The importance of minimizing pile-up without significant loss of resolution by use of an adequate absorber set just in front of the rear detector is underlined

  17. US Participation in the Solar Orbiter Multi Element Telescope for Imaging and Spectroscopy (METIS) Project

    Data.gov (United States)

    National Aeronautics and Space Administration — The Multi Element Telescope for Imaging and Spectroscopy, METIS, investigation has been conceived to perform off-limb and near-Sun coronagraphy and is motivated by...

  18. 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)

  19. 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

  20. Mobile gamma spectrometry with remote data analysis

    International Nuclear Information System (INIS)

    Anttalainen, O.; Toivonen, H.

    2009-01-01

    There are several devices on the market designed for the detection and identification of a radiation source. The widely used approach for this is to use sensitive scintillation or semiconductor detectors together with software algorithms to get the alarms on-site in real time. The devices may be used in covert operations during major public events such as in international sports events or at political meetings. The screening and surveys are prone to false alarms due to the variability of the natural radiation or to legal radiation sources such as patients who have received radioisotope treatment recently. The correct interpretation of the spectrometric signal is a task of a nuclear specialist; every instrument user is not expected to have such knowledge, and therefore, there is a substantial risk to misinterpret the result given by the instrument. The consequences of a false alarm can be dramatic, and therefore, from the operational point of view correct alarm handling is a key capability. Environics Oy has commercialized the measurement and an analysis concept developed by STUK (Radiation and Nuclear Safety Authority in Finland). This concept includes high performance spectrometric analysis, local and remote data analysis, including wireless online connection to expert systems and expert support allowing multi-user-single-expert (MUSE) operations.(author)

  1. Hydrogen analysis by elastic recoil spectrometry

    International Nuclear Information System (INIS)

    Tirira, J.; Trocellier, P.

    1989-01-01

    An absolute, quantitative procedure was developed to determine the hydrogen content and to describe its concentration profile in the near-surface region of solids. The experimental technique used was the elastic recoil detection analysis of protons induced by 4 He beam bombardment in the energy range <=1.8 MeV. The hydrogen content was calculated using a new recoil cross section expression. The analyses were performed in silicon crystals implanted with hydrogen at 10 keV. The implantation dose was evaluated with an accuracy of 10% and the hydrogen depth profile with that of +-10 nm around 200 nm. (author) 10 refs.; 3 figs

  2. 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.)

  3. 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.)

  4. Secondary neutral mass spectrometry depth profile analysis of silicides

    International Nuclear Information System (INIS)

    Beckmann, P.; Kopnarski, M.; Oechsner, H.

    1985-01-01

    The Direct Bombardment Mode (DBM) of Secondary Neutral Mass Spectrometry (SNMS) has been applied for depth profile analysis of two different multilayer systems containing metal silicides. Due to the extremely high depth resolution obtained with low energy SNMS structural details down to only a few atomic distances are detected. Stoichiometric information on internal oxides and implanted material is supplied by the high quantificability of SNMS. (Author)

  5. Analysis of sample γ-spectrometry with mathematic simulating

    International Nuclear Information System (INIS)

    Guo Hongsheng; He Xijun; Peng Taiping; Yang Gaozhao; Wang Wenchuan; Feng Chun

    2005-01-01

    When a sample contains various energy γ-rays, its peak area records not only the events of optical-electronic effect but also the Compton scattering events of higher energy γ-rays. So the γ-ray intensity conducted by the peak area can not be gained. Using the anti-matrix method, the better results of analysis on the γ-spectrometry can be obtained. (authors)

  6. 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.

  7. Nuclear spectrometry for environmental analysis and mapping

    International Nuclear Information System (INIS)

    Simon, Aliz

    2013-01-01

    visits, and provision of equipment. This talk gives an overview of the lAEA Physics Section activities with a special emphasis on the following activities: 1)Improving the analytical performance of PIXE and other IBA techniques; 2)Networking for environmental analysis; 3)Radioisotope environmental mapping; 4)Future perspectives for new IBA methods, especially Heavy lon PIXE combined with MeVSIMS. (author)

  8. Nuclear spectrometry for environmental analysis and mapping

    Energy Technology Data Exchange (ETDEWEB)

    Simon, Aliz, E-mail: Aliz.Simon@iaea.org [International Atomic Energy Agency (IAEA), Division of Physical and Chemical Sciences, Vienna (Austria)

    2013-07-01

    visits, and provision of equipment. This talk gives an overview of the lAEA Physics Section activities with a special emphasis on the following activities: 1)Improving the analytical performance of PIXE and other IBA techniques; 2)Networking for environmental analysis; 3)Radioisotope environmental mapping; 4)Future perspectives for new IBA methods, especially Heavy lon PIXE combined with MeVSIMS. (author)

  9. Direct analysis of traditional Chinese medicines by mass spectrometry.

    Science.gov (United States)

    Wong, Melody Yee-Man; So, Pui-Kin; Yao, Zhong-Ping

    2016-07-15

    Analysis of traditional Chinese medicines (TCMs) plays important roles in quality control of TCMs and understanding their pharmacological effects. Mass spectrometry (MS) is a technique of choice for analysis of TCMs due to its superiority in speed, sensitivity and specificity. However, conventional MS analysis of TCMs typically requires extensive sample pretreatment and chromatographic separation, which could be time-consuming and laborious, prior to the analysis. The expanding usage of TCMs worldwide demands development of rapid, cost-effective and reliable methods for analysis of TCMs. In recent years, new sample preparation and ionization techniques have been developed to enable direct analysis of TCMs by MS, significantly reducing the analysis time and cost. In this review, various MS-based techniques, mainly including ambient ionization-MS and MALDI-MS based techniques, applied for direct analysis of TCMs are summarized and their applicability and future prospects are discussed. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. On neutron activation analysis with γγ coincidence spectrometry

    International Nuclear Information System (INIS)

    Zeisler, Rolf; Danyal Turkoglu; Ibere Souza Ribeiro Junior; Shetty, M.G.

    2017-01-01

    A new γγ coincidence system has been set up at NIST. It is operated with a digital data finder supported by new software developed at NIST. The system is used to explore possible enhancements in instrumental neutron activation analysis (INAA) and study applicability to neutron capture prompt gamma activation analysis (PGAA). The performance of the system is tested with certified reference materials for efficiency calibration and quantitative performance. Comparisons of INAA results based on conventional gamma-ray spectrometry data with INAA results based on coincidence data obtained from the same samples show improvements in the counting uncertainties and demonstrates the quantitative accuracy of the new system. (author)

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    Science.gov (United States)

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

    2017-07-01

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

  14. Gas analysis by computer-controlled microwave rotational spectrometry

    International Nuclear Information System (INIS)

    Hrubesh, L.W.

    1978-01-01

    Microwave rotational spectrometry has inherently high resolution and is thus nearly ideal for qualitative gas mixture analysis. Quantitative gas analysis is also possible by a simplified method which utilizes the ease with which molecular rotational transitions can be saturated at low microwave power densities. This article describes a computer-controlled microwave spectrometer which is used to demonstrate for the first time a totally automated analysis of a complex gas mixture. Examples are shown for a complete qualitative and quantitative analysis, in which a search of over 100 different compounds is made in less than 7 min, with sensitivity for most compounds in the 10 to 100 ppm range. This technique is expected to find increased use in view of the reduced complexity and increased reliabiity of microwave spectrometers and because of new energy-related applications for analysis of mixtures of small molecules

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

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

    International Nuclear Information System (INIS)

    Govindaraju, K.; Mevelle, G.

    1987-01-01

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

  17. Native Liquid Extraction Surface Analysis Mass Spectrometry: Analysis of Noncovalent Protein Complexes Directly from Dried Substrates

    Science.gov (United States)

    Martin, Nicholas J.; Griffiths, Rian L.; Edwards, Rebecca L.; Cooper, Helen J.

    2015-08-01

    Liquid extraction surface analysis (LESA) mass spectrometry is a promising tool for the analysis of intact proteins from biological substrates. Here, we demonstrate native LESA mass spectrometry of noncovalent protein complexes of myoglobin and hemoglobin from a range of surfaces. Holomyoglobin, in which apomyoglobin is noncovalently bound to the prosthetic heme group, was observed following LESA mass spectrometry of myoglobin dried onto glass and polyvinylidene fluoride surfaces. Tetrameric hemoglobin [(αβ)2 4H] was observed following LESA mass spectrometry of hemoglobin dried onto glass and polyvinylidene fluoride (PVDF) surfaces, and from dried blood spots (DBS) on filter paper. Heme-bound dimers and monomers were also observed. The `contact' LESA approach was particularly suitable for the analysis of hemoglobin tetramers from DBS.

  18. Transition of Iodine Analysis to Accelerator Mass Spectrometry

    International Nuclear Information System (INIS)

    Watrous, Matthew George; Adamic, Mary Louise; Olson, John Eric; Baeck, D. L.; Fox, R. V.; Hahn, P. A.; Jenson, D. D.; Lister, T. E.

    2015-01-01

    The goal of the project, New Paradigms for Isotope Ratio Mass Spectrometry: Raising the Scientific Profile and Improved Performance for Accelerator Mass Spectrometry (AMS) and Thermal Ionization Mass Spectrometry (TIMS), is to ensure that the ongoing isotope ratio determination capability within the U.S. Department of Energy complex is the world's best for application to nonproliferation. This report spells out the progress of Task 4, Transition of TIMS to AMS for Iodine Analysis, of the larger project. The subtasks under Task 4 and the accomplishments throughout the three year project life cycle are presented in this report. Progress was made in optimization of chemical extraction, determination of a detection limit for 127Iodine, production of standard materials for AMS analysis quality assurance, facilitation of knowledge exchange with respect to analyzing iodine on an AMS, cross comparison with a world-leading AMS laboratory, supercritical fluid extraction of iodine for AMS analysis and electrodeposition of seawater as a direct method of preparation for iodine analysis by AMS--all with the goal of minimizing the time required to stand up an AMS capability for iodine analysis of exposed air filters at INL. An effective extraction method has been developed and demonstrated for iodine analysis of exposed air filters. Innovative techniques to accomplish the cathode preparation for AMS analysis were developed and demonstrated and published. The known gap of a lack of available materials for reference standards in the analysis of iodine by AMS was filled by the preparation of homogenous materials that were calibrated against NIST materials. A minimum limit on the amount of abundant isotope in a sample was determined for AMS analysis. The knowledge exchange occurred with fantastic success. Scientists engaged the international AMS community at conferences, as well as in their laboratories for collaborative work. The supercritical fluid extraction work has positive

  19. Transition of Iodine Analysis to Accelerator Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Watrous, Matthew George [Idaho National Lab. (INL), Idaho Falls, ID (United States); Adamic, Mary Louise [Idaho National Lab. (INL), Idaho Falls, ID (United States); Olson, John Eric [Idaho National Lab. (INL), Idaho Falls, ID (United States); Baeck, D. L. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Fox, R. V. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Hahn, P. A. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Jenson, D. D. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Lister, T. E. [Idaho National Lab. (INL), Idaho Falls, ID (United States)

    2015-09-01

    The goal of the project, New Paradigms for Isotope Ratio Mass Spectrometry: Raising the Scientific Profile and Improved Performance for Accelerator Mass Spectrometry (AMS) and Thermal Ionization Mass Spectrometry (TIMS), is to ensure that the ongoing isotope ratio determination capability within the U.S. Department of Energy complex is the world’s best for application to nonproliferation. This report spells out the progress of Task 4, Transition of TIMS to AMS for Iodine Analysis, of the larger project. The subtasks under Task 4 and the accomplishments throughout the three year project life cycle are presented in this report. Progress was made in optimization of chemical extraction, determination of a detection limit for 127Iodine, production of standard materials for AMS analysis quality assurance, facilitation of knowledge exchange with respect to analyzing iodine on an AMS, cross comparison with a world-leading AMS laboratory, supercritical fluid extraction of iodine for AMS analysis and electrodeposition of seawater as a direct method of preparation for iodine analysis by AMS--all with the goal of minimizing the time required to stand up an AMS capability for iodine analysis of exposed air filters at INL. An effective extraction method has been developed and demonstrated for iodine analysis of exposed air filters. Innovative techniques to accomplish the cathode preparation for AMS analysis were developed and demonstrated and published. The known gap of a lack of available materials for reference standards in the analysis of iodine by AMS was filled by the preparation of homogenous materials that were calibrated against NIST materials. A minimum limit on the amount of abundant isotope in a sample was determined for AMS analysis. The knowledge exchange occurred with fantastic success. Scientists engaged the international AMS community at conferences, as well as in their laboratories for collaborative work. The supercritical fluid extraction work has positive

  20. Improovement of statistical counting conditions for the determination of chloride in Beams leaves (Phaseolus vulgaris L.) by thermal neutron activation analysis

    International Nuclear Information System (INIS)

    Ferraz, E.S.B.; Nascimento Filho, V.F.

    1975-04-01

    The use of two radiation peaks from the same gamma-emitting source in the calculation of the corresponding liquid counting rate in multi-element gamma spectrometry is discussed. It is shown that, in the determination of chlorine in Phaseolus vulgaris L. using neutronic activation analysis will result in an increase in accuracy of measurement of approximately 40%

  1. Mass spectrometry-based analysis of whole-grain phytochemicals.

    Science.gov (United States)

    Koistinen, Ville Mikael; Hanhineva, Kati

    2017-05-24

    Whole grains are a rich source of several classes of phytochemicals, such as alkylresorcinols, benzoxazinoids, flavonoids, lignans, and phytosterols. A high intake of whole grains has been linked to a reduced risk of some major noncommunicable diseases, and it has been postulated that a complex mixture of phytochemicals works in synergy to generate beneficial health effects. Mass spectrometry, especially when coupled with liquid chromatography, is a widely used method for the analysis of phytochemicals owing to its high sensitivity and dynamic range. In this review, the current knowledge of the mass spectral properties of the most important classes of phytochemicals found in cereals of common wheat, barley, oats, and rye is discussed.

  2. 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.)

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

    International Nuclear Information System (INIS)

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

    1986-12-01

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

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

    DEFF Research Database (Denmark)

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

    2016-01-01

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

  5. DETERMINATION OF MULTI ELEMENT LEVELS IN LEAVES AND ...

    African Journals Online (AJOL)

    Preferred Customer

    ICP-OES (Spectro Analytical Instruments, Kleve, Germany) was used for the determination of elements. ... Samples. In this study, 18 different herbal tea samples (leaves and flowers) that are traditionally used for medical ... analysis of CRM were all within the 95% reliability limit. The results ..... reasons for serious health risks.

  6. The role of mass spectrometry in hydrocarbon analysis

    International Nuclear Information System (INIS)

    Kerenyi, E.

    1980-01-01

    Modern mass spectrometry has an outstandin.o role in solving problems concerning the composition and structure of hydrocarbon mixtures and their derivatives, petroleum and petrochemical products. Its efficiency in hydrocarbon analysis has been increased not only by high resolving power and computerized spectrum processing but also by the metastable ion spectrum technique promoting structural examinations, by mild ionization facilitating composition analysis, and by selective ion-detecting technique. The author presents the advantages of the metastable ion spectra, the field ionization, field desorption and other mild ionization methods, and finally, those of fragmentation analysis in connection with the examination of hydrocarbons and hydrocarbon derivatives. Examples taken from the literature and from the research work carried out in the Institute are also given. (author)

  7. Multi-elemental characterization of Cuban natural zeolites

    International Nuclear Information System (INIS)

    Diaz Rizo, O.; Herrera Peraza, E.F.

    1996-01-01

    Concentrations of 38 elements in samples from four important Cuban zeolite bed have beam obtained by Instrumental Neutron Activation (INAA) and X-Ray Fluorescence Analysis (XRFA). In comparison with other analytical techniques good agreement was achieved. The concentration values of minor element Ba, Sr, Zn, and Mn, and 25 trace element (including 9 REE) are at the first time reported in Cuban zeolite. It is important for the zeolite evaluation in different industrial uses

  8. Overview of multi-element monolithic germanium detectors for XAFS experiments at diamond light source

    International Nuclear Information System (INIS)

    Chatterji, S.; Dennis, G. J.; Dent, A.; Diaz-Moreno, S.; Cibin, G.; Tartoni, N.; Helsby, W. I.

    2016-01-01

    An overview of multi-element monolithic germanium detectors being used at the X-ray absorption spectroscopy (XAS) beam lines at Diamond Light Source (DLS) is being reported. The hardware details and a summary of the performance of these detectors have also been provided. Recent updates about various ongoing projects being worked on to improve the performance of these detectors are summarized.

  9. Overview of multi-element monolithic germanium detectors for XAFS experiments at diamond light source

    Energy Technology Data Exchange (ETDEWEB)

    Chatterji, S.; Dennis, G. J.; Dent, A.; Diaz-Moreno, S.; Cibin, G.; Tartoni, N. [Diamond Light Source Ltd, Oxfordshire (United Kingdom); Helsby, W. I. [STFC Daresbury Laboratory, Warrington (United Kingdom)

    2016-07-27

    An overview of multi-element monolithic germanium detectors being used at the X-ray absorption spectroscopy (XAS) beam lines at Diamond Light Source (DLS) is being reported. The hardware details and a summary of the performance of these detectors have also been provided. Recent updates about various ongoing projects being worked on to improve the performance of these detectors are summarized.

  10. Pump radiation distribution in multi-element first cladding laser fibres

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  11. MEGHNAD – A multi element detector array for heavy ion collision ...

    Indian Academy of Sciences (India)

    When heavy ion beam available from such machines fall on a target and undergo collision, very rich and often pristine fields of research open up. In order to carry on such activities, we have taken up a project to build a multi element gamma, heavy ion and neutron array of detectors (MEGHNAD) to detect and study the ...

  12. Design and Wind Tunnel Testing of a Thick, Multi-Element High-Lift Airfoil

    DEFF Research Database (Denmark)

    Zahle, Frederik; Gaunaa, Mac; Sørensen, Niels N.

    2012-01-01

    In this work a 2D CFD solver has been used to optimize the shape of a leading edge slat with a chord length of 30% of the main airfoil which was 40% thick. The airfoil configuration was subsequently tested in a wind tunnel and compared to numerical predictions. The multi-element airfoil was predi...

  13. 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

  14. Multi-element measurements in mexican cigarette tobacco

    International Nuclear Information System (INIS)

    Vega-Carrillo, H.R.; Texas Univ., Austin, TX; Zacatecas Univ.; Iskander, F.Y.; Manzanares-Acuna, E.

    1995-01-01

    The concentration of 21 elements in cigarette tobacco in nine different brands manufactured and commercially available in Mexico has been determined using neutron activation analysis. The concentration range of the measured elements (in μg g -1 ) were: As, (four brands) <0.55-3.24; Ba, 64-251; Br, (four brands) 49-136; Ce, <0.3-1.7; Co, 0.29-0.55, Cr, <0.8-2.4; Cs, 0.091-0.40; Eu, <0.03; Fe, 420-680; Hf, <0.03-0.13; K, (four brands) 18300-40300; La, (four brands) < 0.2-0.66; Na, (four brands) 309-566; Rb, 19-50; Sb, <0.7; Sc, 0.13-0.22; Se, <0.7; Sm, (four brands) 0.07-0.14; Sr, 227-472; Th, < 0.1-0.17 and Zn, 14-56. The results are compared with the literature values for the concentration of the above elements in cigarette tobacco from other countries. (author) 18 refs.; 2 tabs

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

    Science.gov (United States)

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

    2018-04-01

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

  16. Analysis of hazardous biological material by MALDI mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    KL Wahl; KH Jarman; NB Valentine; MT Kingsley; CE Petersen; ST Cebula; AJ Saenz

    2000-03-21

    Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-MS) has become a valuable tool for analyzing microorganisms. The speed with which data can be obtained from MALDI-MS makes this a potentially important tool for biological health hazard monitoring and forensic applications. The excitement in the mass spectrometry community in this potential field of application is evident by the expanding list of research laboratories pursuing development of MALDI-MS for bacterial identification. Numerous research groups have demonstrated the ability to obtain unique MALDI-MS spectra from intact bacterial cells and bacterial cell extracts. The ability to differentiate strains of the same species has been investigated. Reproducibility of MALDI-MS spectra from bacterial species under carefully controlled experimental conditions has also been demonstrated. Wang et al. have reported on interlaboratory reproducibility of the MALDI-MS analysis of several bacterial species. However, there are still issues that need to be addressed, including the careful control of experimental parameters for reproducible spectra and selection of optimal experimental parameters such as solvent and matrix.

  17. 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)

  18. New Isotope Analysis Method: Atom Trap Mass Spectrometry

    International Nuclear Information System (INIS)

    Ko, Kwang Hoon; Park, Hyun Min; Han, Jae Min; Kim, Taek Soo; Cha, Yong Ho; Lim, Gwon; Jeong, Do Young

    2011-01-01

    Trace isotope analysis has been an important role in science, archaeological dating, geology, biology and nuclear industry. Some fission products such as Sr-90, Cs-135 and Kr-85 can be released to the environment when nuclear accident occurs and the reprocessing factory operates. Thus, the analysis of artificially produced radioactive isotopes has been of interest in nuclear industry. But it is difficult to detect them due to low natural abundance less then 10 -10 . In general, radio-chemical method has been applied to detect ultra-trace radio isotopes. But this method has disadvantages of long measurement time for long lived radioisotopes and toxic chemical process for the purification. The Accelerator Mass Spectrometer has high isotope selectivity, but the system is huge and its selectivity is affected by isobars. The laser based method, such as RIMS (Resonance Ionization Mass Spectrometry) has the advantage of isobar-effect free characteristics. But the system size is still huge for high isotope selective system. Recently, ATTA (Atom Trap Trace Analysis) has been successfully applied to detect ultra-trace isotope, Kr-81 and Kr-85. ATTA is the isobar-effect free detection with high isotope selectivity and the system size is small. However, it requires steady atomic beam source during detection, and is not allowed simultaneous detection of several isotopes. In this presentation, we introduce new isotope detection method which is a coupled method of Atom Trap Mass Spectrometry (ATMS). We expect that it can overcome the disadvantage of ATTA while it has both advantages of ATTA and mass spectrometer. The basic concept and the system design will be presented. In addition, the experimental status of ATMS will also be presented

  19. Laser desorption mass spectrometry for fast DNA analysis

    Energy Technology Data Exchange (ETDEWEB)

    Chen, C.H.; Ch`ang, L.Y.; Taranenko, N.I.; Allman, S.L.; Tang, K.; Matteson, K.J.

    1995-09-01

    During the past few years, major effort has been directed toward developing mass spectrometry to measure biopolymers because of the great potential benefit to biomedical research. Hellenkamp and his co-workers were the first to report that large polypeptide molecules can be ionized and detected without significant fragmentation when a greater number of nicotinic acid molecules are used as a matrix. This method is now well known as matrix-assisted laser desorption/ionization (MALDI). Since then, various groups have reported measurements of very large proteins by MALDI. Reliable protein analysis by MALDI is more or less well established. However, the application of MALDI to nucleic acids analysis has been found to be much more difficult. Most research on the measurement of nucleic acid by MALDI were stimulated by the Human Genome Project. Up to now, the only method for reliable routine analysis of nucleic acid is gel electrophoresis. Different sizes of nucleic acids can be separated in gel medium when a high electric field is applied to the gel. However, the time needed to separate different sizes of DNA segments usually takes from several minutes to several hours. If MALDI can be successfully used for nucleic acids analysis, the analysis time can be reduced to less than I millisecond. In addition, no tagging with radioactive materials or chemical dyes is needed. In this work, we will review recent progress related to MALDI for DNA analysis.

  20. Isotopic analysis of boron by thermal ionization mass spectrometry

    International Nuclear Information System (INIS)

    Kakazu, M.H.; Sarkis, J.E.S.; Souza, I.M.S.

    1991-07-01

    This paper presents a methodology for isotopic analysis of boron by thermal ionization mass spectrometry technique through the ion intensity measurement of Na 2 BO + 2 in H 3 BO 3 , B o and B 4 C. The samples were loaded on single tantalum filaments by different methods. In the case of H 3 BO 3 , the method of neutralization with NaOH was used. For B 4 C the alcaline fusion with Na 2 CO 3 and for B o dissolution with 1:1 nitric sulfuric acid mixture followed by neutralization with NaOH was used. The isotopic ratio measurements were obtained by the use of s Faraday cup detector with external precision of ±0,4% and accuracy of ±0,1%, relative to H 3 BO 3 isotopic standard NBS 951. The effects of isotopic fractionation was studied in function of the time during the analyses and the different chemical forms of deposition. (author)

  1. Isotopic analysis of uranium by thermoionic mass spectrometry

    International Nuclear Information System (INIS)

    Moraes, N.M.P. de.

    1979-01-01

    Uranium isotopic ratio measurements by thermoionic spectrometry are presented. Emphasis is given upon the investigation of the parameters that directly affect the precision and accuracy of the results. Optimized procedures, namely, chemical processing, sample loading on the filaments, vaporization, ionization and measurements of ionic currents, are established. Adequate statistical analysis of the data for the calculation of the internal and external variances and mean standard deviation are presented. These procedures are applied to natural and NBS isotopic standard uranium samples. The results obtained agree with the certified values within specified limits. 235 U/ 238 U isotopic ratios values determined for NBS-U500, and a series of standard samples with variable isotopic compositon, are used to calculate mass discrimination factor [pt

  2. Statistical analysis of proteomics, metabolomics, and lipidomics data using mass spectrometry

    CERN Document Server

    Mertens, Bart

    2017-01-01

    This book presents an overview of computational and statistical design and analysis of mass spectrometry-based proteomics, metabolomics, and lipidomics data. This contributed volume provides an introduction to the special aspects of statistical design and analysis with mass spectrometry data for the new omic sciences. The text discusses common aspects of design and analysis between and across all (or most) forms of mass spectrometry, while also providing special examples of application with the most common forms of mass spectrometry. Also covered are applications of computational mass spectrometry not only in clinical study but also in the interpretation of omics data in plant biology studies. Omics research fields are expected to revolutionize biomolecular research by the ability to simultaneously profile many compounds within either patient blood, urine, tissue, or other biological samples. Mass spectrometry is one of the key analytical techniques used in these new omic sciences. Liquid chromatography mass ...

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

    International Nuclear Information System (INIS)

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

    1991-01-01

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

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

    Science.gov (United States)

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

    2013-12-01

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

  5. Analysis of metals in solution using electrospray ionization mass spectrometry

    International Nuclear Information System (INIS)

    Van Berkel, G.J.; McLuckey, S.A.; Glish, G.L.

    1991-01-01

    Electrospray ionization-mass spectrometry (ES-MS) has gained most of its recent attention because of the ability to produce multiply charged ions from very large biomolecules making them amenable to analysis by most modern mass spectrometers. However, ES-MS is equally well suited for compounds of low or moderate molecular weight that are difficult to volatilize intact by others methods. Moreover, the early work of Fenn and co-workers (1,2) and recent reports by Kebarle and co-workers (3,4) attest to the applicability of ES-MS to the study of the gas-phase chemistry of multiply solvated or coordinated metal ions. The utility of ES-MS for the analysis of metals in solution derives in part from the facility with which the metal ions are solvated by or form complexes with the ES solvent or other reagents added to the solvent. Solvation and complexation can be a hindrance, however, in the analytical application of ES-MS to the analysis of metals in solution, especially solutions of metals in water. The data presented here demonstrate that many of the problems in the ES-MS analysis of metals can be overcome by complexing the metals with crown ethers and/or extracting the metals from water into an organic phase using crown ethers. 5 refs., 4 figs

  6. Petroleomics by Direct Analysis in Real Time-Mass Spectrometry.

    Science.gov (United States)

    Romão, Wanderson; Tose, Lilian V; Vaz, Boniek G; Sama, Sara G; Lobinski, Ryszard; Giusti, Pierre; Carrier, Hervé; Bouyssiere, Brice

    2016-01-01

    The analysis of crude oil and its fractions by applying ambient ionization techniques remains underexplored in mass spectrometry (MS). Direct analysis in real time (DART) in the positive-ion mode was coupled to a linear quadrupole ion trap Orbitrap mass spectrometer (LTQ Orbitrap) to analyze crude oil, paraffin samples, and porphyrin standard compounds. The ionization parameters of DART-MS were optimized for crude oil analysis. DART-MS rendered the optimum conditions of the operation using paper as the substrate, T = 400°C, helium as the carrier gas, and a sample concentration ≥6 mg mL(-1). In the crude oils analysis, the DART(+)-Orbitrap mass spectra detected the typical N, NO, and O-containing compounds. In the paraffin samples, oxidized hydrocarbon species (Ox classes, where x = 1-4) with double-bond equivalent of 1-4 were detected, and their structures and connectivity were confirmed by collision-induced dissociation (CID) experiments. DART(+)-MS has identified the porphyrin standard compounds as [M + H](+) ions of m/z 615.2502 and 680.1763, where M = C44H30N4 and C44H28N4OV, respectively, based on the formula assignment and by phenyl losses observed on CID experiments.

  7. Limitation of multi-elemental fingerprinting of wheat grains: Effect of cultivar, sowing date, and nutrient management

    DEFF Research Database (Denmark)

    Suarez-Tapia, Alfonso; Kucheryavskiy, Sergey V.; Christensen, Bent Tolstrup

    2017-01-01

    Multi-element fingerprinting demonstrates some potential for tracing the origin of agricultural products but not for discriminating among crop cultivars and nutrient management (source, rate). With principal component analysis (PCA) and univariate statistics, we examined 19 elements in grains from...... two winter wheat cultivars (Hereford, Mariboss) grown with different rates of animal manure (AM) or mineral fertilisers (NPK) in a long-term field experiment and two sowing dates (early, timely). Nitrogen, Cd and Mn related to NPK, and Mo and Na to AM. Barium, Fe, and P reflected nutrient rate......; these elements increased with nutrient rate regardless of source. Unmanured grains were enriched in Cu. Mariboss was characterized by higher concentrations of Sr, Ba and Sc compared to Hereford with Sr in grain as the main separator. Univariate statistics showed higher concentrations of N, P, Mg, Ba, Cu, Mo...

  8. The 1 MV multi-element AMS system for biomedical applications at the Netherlands Organization for Applied Scientific Research (TNO)

    Energy Technology Data Exchange (ETDEWEB)

    Klein, Matthias, E-mail: mklein@highvolteng.com [High Voltage Engineering Europa B.V., P.O. Box 99, 3800 AB Amersfoort (Netherlands); Vaes, W.H.J.; Fabriek, B.; Sandman, H. [TNO, P.O. Box 360, 3700 AJ Zeist (Netherlands); Mous, D.J.W.; Gottdang, A. [High Voltage Engineering Europa B.V., P.O. Box 99, 3800 AB Amersfoort (Netherlands)

    2013-01-15

    The Netherlands Organization for Applied Scientific Research (TNO) has installed a compact 1 MV multi-element AMS system manufactured by High Voltage Engineering Europa B.V., The Netherlands. TNO performs clinical research programs for pharmaceutical and innovative foods industry to obtain early pharmacokinetic data and to provide anti-osteoporotic efficacy data of new treatments. The AMS system will analyze carbon, iodine and calcium samples for this purpose. The first measurements on blank samples indicate background levels in the low 10{sup -12} for calcium and iodine, making the system well suited for these biomedical applications. Carbon blanks have been measured at low 10{sup -16}. For unattended, around-the-clock analysis, the system features the 200 sample version of the SO110 hybrid ion source and user friendly control software.

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

    International Nuclear Information System (INIS)

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

    1993-01-01

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

  10. Continuous-flow accelerator mass spectrometry for radiocarbon analysis

    International Nuclear Information System (INIS)

    Wills, J.S.C.; Han, B.X.; Von Reden, K.F.; Schneider, R.J.; Roberts, M.L.

    2006-01-01

    Accelerator Mass Spectrometry (AMS) is a widely used technique for radiocarbon dating of archaeological or environmental samples that are very small or very old (up to 50,000 years before present). Because of the method's extreme sensitivity, AMS can also serve as an environmental tracer and supplements conventional nuclear counting techniques for monitoring 14 C emissions from operating nuclear power plants and waste repositories. The utility of present AMS systems is limited by the complex sample preparation process required. Carbon from combusted artefacts must be incorporated into a solid metallic target from which a negative ion beam is produced and accelerated to MeV energies by an accelerator for subsequent analysis. This paper will describe a novel technique being developed by the National Ocean Sciences Accelerator Mass Spectrometry (NOSAMS) Laboratory at the Woods Hole Oceanographic Institution for the production of negative carbon ion beams directly from a continuously flowing sample gas stream, eliminating the requirement for a solid target. A key component of the new technique is a microwave-driven, gaseous-feed ion source originally developed at Chalk River Laboratories for the very different requirements of a high current proton linear accelerator. A version of this ion source is now being adapted to serve as an injector for a dedicated AMS accelerator facility at NOSAMS. The paper begins with a review of the fundamentals of radiocarbon dating. Experiments carried out at NOSAMS with a prototype of the microwave ion source are described, including measurements of sample utilization efficiency and sample 'memory' effect. A new version of the microwave ion source, optimized for AMS, is also described. The report concludes with some predictions of new research opportunities that will become accessible to the technique of continuous-flow AMS. (author)

  11. Continuous-flow accelerator mass spectrometry for radiocarbon analysis

    International Nuclear Information System (INIS)

    Wills, J.S.C.; Han, B.X.; Von Reden, K.F.; Schneider, R.J.; Roberts, M.L.

    2006-05-01

    Accelerator Mass Spectrometry (AMS) is a widely used technique for radiocarbon dating of archaeological or environmental samples that are very small or very old (up to 50,000 years before present). Because of the method's extreme sensitivity, AMS can also serve as an environmental tracer and supplements conventional nuclear counting techniques for monitoring 14 C emissions from operating nuclear power plants and waste repositories. The utility of present AMS systems is limited by the complex sample preparation process required. Carbon from combusted artefacts must be incorporated into a solid metallic target from which a negative ion beam is produced and accelerated to MeV energies by an accelerator for subsequent analysis. This paper will describe a novel technique being developed by the National Ocean Sciences Accelerator Mass Spectrometry (NOSAMS) Laboratory at the Woods Hole Oceanographic Institution for the production of negative carbon ion beams directly from a continuously flowing sample gas stream, eliminating the requirement for a solid target. A key component of the new technique is a microwave-driven, gaseous-feed ion source originally developed at Chalk River Laboratories for the very different requirements of a high current proton linear accelerator. A version of this ion source is now being adapted to serve as an injector for a dedicated AMS accelerator facility at NOSAMS. The paper begins with a review of the fundamentals of radiocarbon dating. Experiments carried out at NOSAMS with a prototype of the microwave ion source are described, including measurements of sample utilization efficiency and sample 'memory' effect. A new version of the microwave ion source, optimized for AMS, is also described. The report concludes with some predictions of new research opportunities that will become accessible to the technique of continuous-flow AMS. (author)

  12. Automated gamma spectrometry and data analysis on radiometric neutron dosimeters

    International Nuclear Information System (INIS)

    Matsumoto, W.Y.

    1983-01-01

    An automated gamma-ray spectrometry system was designed and implemented by the Westinghouse Hanford Company at the Hanford Engineering Development Laboratory (HEDL) to analyze radiometric neutron dosimeters. Unattended, automatic, 24 hour/day, 7 day/week operation with online data analysis and mainframe-computer compatible magnetic tape output are system features. The system was used to analyze most of the 4000-plus radiometric monitors (RM's) from extensive reactor characterization tests during startup and initial operation of th Fast Flux Test Facility (FFTF). The FFTF, operated by HEDL for the Department of Energy, incorporates a 400 MW(th) sodium-cooled fast reactor. Aumomated system hardware consists of a high purity germanium detector, a computerized multichannel analyzer data acquisition system (Nuclear Data, Inc. Model 6620) with two dual 2.5 Mbyte magnetic disk drives plus two 10.5 inch reel magnetic tape units for mass storage of programs/data and an automated Sample Changer-Positioner (ASC-P) run with a programmable controller. The ASC-P has a 200 sample capacity and 12 calibrated counting (analysis) positions ranging from 6 inches (15 cm) to more than 20 feet (6.1 m) from the detector. The system software was programmed in Fortran at HEDL, except for the Nuclear Data, Inc. Peak Search and Analysis Program and Disk Operating System (MIDAS+)

  13. Theory of error for target factor analysis with applications to mass spectrometry and nuclear magnetic resonance spectrometry

    International Nuclear Information System (INIS)

    Malinowski, E.R.

    1978-01-01

    Based on the theory of error for abstract factor analysis described earlier, a theory of error for target factor analysis is developed. The theory shows how the error in the data matrix mixes with the error in the target test vector. The apparent error in a target test is found to be a vector sum of the real error in the target vector and the real error in the predicted vector. The theory predicts the magnitudes of these errors without requiring any a priori knowledge of the error in the data matrix or the target vector. A reliability function and a spoil function are developed for the purpose of assessing the validity and the worthiness of a target vector. Examples from model data, mass spectrometry and nuclear magnetic resonance spectrometry are presented. (Auth.)

  14. [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.

  15. Towards metals analysis using corona discharge ionization ion mobility spectrometry.

    Science.gov (United States)

    Jafari, Mohammad T; Saraji, Mohammad; Sherafatmand, Hossein

    2016-02-25

    For the first time, the capability of corona discharge ionization ion mobility spectrometry (CD-IMS) in the determination of metal complex was evaluated. The extreme simplicity of dispersive liquid-liquid microextraction (DLLME) coupled to the high sensitivity of CD-IMS measurement could make this combination really useful for simple, rapid, and sensitive determination of metals in different samples. In this regard, mercury, as a model metal, was complexed with diethyldithiocarbamate (DEDTC), and then extracted into the carbon tetrachloride using DLLME. Some parameters affecting the extraction efficiency, including the type and volume of the extraction solvent, the type and volume of the disperser solvent, the concentration of the chelating agent, salt addition and, pH were exhaustively investigated. Under the optimized condition, the enrichment factor was obtained to be 142. The linear range of 0.035-10.0 μg mL(-1) with r(2) = 0.997 and the detection limit of 0.010 μg mL(-1) were obtained. The relative standard deviation values were calculated to be lower than 4% and 8% for intra-day and inter-day, respectively. Finally, the developed method was successfully applied for the extraction and determination of mercury in various real samples. The satisfactory results revealed the capability of the proposed method in trace analysis without tedious derivatization or hydride generation. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Neutron activation analysis of lipsticks using gamma-ray spectrometry

    International Nuclear Information System (INIS)

    Mirsa, G.; Mittal, V.K.

    2004-01-01

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

  17. 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.

  18. Derivative flame atomic absorption spectrometry and its application in trace analysis

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  19. An introduction to the technique of combined ion mobility spectrometry-mass spectrometry for the analysis of complex biological samples

    International Nuclear Information System (INIS)

    McDowall, Mark A.; Bateman, Robert H.; Bajic, Steve; Giles, Kevin; Langridge, Jim; McKenna, Therese; Pringle, Steven D.; Wildgoose, Jason L.

    2008-01-01

    Full Text: Ultra Performance Liquid Chromatography (UPLC) offers several advantages compared with conventional High Performance Liquid Chromatography (HPLC) as an 'inlet system' for mass spectrometry. UPLC provides improved chromatographic resolution, increased sensitivity and reduced analysis time. This is achieved through the use of sub 2μm particles (stationary phase) combined with high-pressure solvent delivery (up to 15,000 psi). When coupled with orthogonal acceleration time-of-flight (oa-TOF) mass spectrometry (MS), UPLC presents a means to achieve high sample throughput with reduced spectral overlap, increased sensitivity, and exact mass measurement capabilities with high mass spectral resolution (Ca 20,000 FWHM). Dispersive ion mobility spectrometry (IMS) implemented within a traveling-wave ion guide provides an orthogonal separation strategy for ions in the gas phase that can resolve isobaric ions formed by either Electrospray of MALDI ionization typically in Ca 20 mille seconds. All three techniques have the potential to be combined on-line (e.g. UPLC-IMS-MS/MS) in real time to maximize peak capacity and resolving power for the analysis of complex biological mixtures including; intact proteins, modified peptides and endogenous/exogenous metabolites

  20. Analysis of burnt nuclear fuel elements by gamma-spectrometry

    International Nuclear Information System (INIS)

    Lammer, M.

    1978-01-01

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

  1. Ion beam analysis and spectrometry techniques for Cultural Heritage studies

    International Nuclear Information System (INIS)

    Beck, L.

    2013-01-01

    The implementation of experimental techniques for the characterisation of Cultural heritage materials has to take into account some requirements. The complexity of these past materials requires the development of new techniques of examination and analysis, or the transfer of technologies developed for the study of advanced materials. In addition, due to precious aspect of artwork it is also necessary to use the non-destructive methods, respecting the integrity of objects. It is for this reason that the methods using radiations and/or particles play a important role in the scientific study of art history and archaeology since their discovery. X-ray and γ-ray spectrometry as well as ion beam analysis (IBA) are analytical tools at the service of Cultural heritage. This report mainly presents experimental developments for IBA: PIXE, RBS/EBS and NRA. These developments were applied to the study of archaeological composite materials: layered materials or mixtures composed of organic and non-organic phases. Three examples are shown: evolution of silvering techniques for the production of counterfeit coinage during the Roman Empire and in the 16. century, the characterization of composites or mixed mineral/organic compounds such as bone and paint. In these last two cases, the combination of techniques gave original results on the proportion of both phases: apatite/collagen in bone, pigment/binder in paintings. Another part of this report is then dedicated to the non-invasive/non-destructive characterization of prehistoric pigments, in situ, for rock art studies in caves and in the laboratory. Finally, the perspectives of this work are presented. (author) [fr

  2. 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

  3. Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

    NARCIS (Netherlands)

    Moerdijk-Poortvliet, Tanja C. W.; Schierbeek, Henk; Houtekamer, Marco; van Engeland, Tom; Derrien, Delphine; Stal, Lucas J.; Boschker, Henricus T. S.

    2015-01-01

    We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ(13)C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

  4. Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

    NARCIS (Netherlands)

    Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

    2015-01-01

    We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of d13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

  5. Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

    NARCIS (Netherlands)

    Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

    2015-01-01

    Rationale: We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence,

  6. The multi-element ultrasonic technology: examples of application on military naval structures

    International Nuclear Information System (INIS)

    Recolin, P.; Rivalin, S.

    2009-01-01

    DCNS is the European leader in the military ship construction and maintenance (conventional and nuclear propulsion). The potential of ultrasonic technologies with multi-element probes has been studied in its Materials laboratory since the end of the 80's, and a growing number of applications has appeared these last ten years. A series of examples is given: in-service nuclear reactor pipe welds monitoring, time-of-flight diffraction (TOFD) technique for the inspection of containment welds, coating fabrication control, detection of laminating corrosion on aluminum rings, detection of corrosion on submarine hulls in basin, inspection of hull welded joints

  7. A multi-element cosmological model with a complex space-time topology

    Science.gov (United States)

    Kardashev, N. S.; Lipatova, L. N.; Novikov, I. D.; Shatskiy, A. A.

    2015-02-01

    Wormhole models with a complex topology having one entrance and two exits into the same space-time of another universe are considered, as well as models with two entrances from the same space-time and one exit to another universe. These models are used to build a model of a multi-sheeted universe (a multi-element model of the "Multiverse") with a complex topology. Spherical symmetry is assumed in all the models. A Reissner-Norström black-hole model having no singularity beyond the horizon is constructed. The strength of the central singularity of the black hole is analyzed.

  8. The evaluation of multi-element personal dosemeters using the linear programming method

    International Nuclear Information System (INIS)

    Kragh, P.; Ambrosi, P.; Boehm, J.; Hilgers, G.

    1996-01-01

    Multi-element dosemeters are frequently used in individual monitoring. Each element can be regarded as an individual dosemeter with its own individual dose measurement value. In general, the individual dose values of one dosemeter vary according to the exposure conditions, i. e. the energy and angle of incidence of the radiation. The (final) dose measurement value of the personal dosemeter is calculated from the individual dose values by means of an evaluation algorithm. The best possible dose value, i.e. that of the smallest systematic (type B) uncertainty if the exposure conditions are changed in the dosemeter's rated range of use, is obtained by the method of linear programming. (author)

  9. 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

  10. 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

  11. Assessment of oil weathering by gas chromatography-mass spectrometry, time warping and principal component analysis

    DEFF Research Database (Denmark)

    Malmquist, Linus M.V.; Olsen, Rasmus R.; Hansen, Asger B.

    2007-01-01

    weathering state and to distinguish between various weathering processes is investigated and discussed. The method is based on comprehensive and objective chromatographic data processing followed by principal component analysis (PCA) of concatenated sections of gas chromatography–mass spectrometry...

  12. 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.

  13. 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.)

  14. 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)

  15. Analysis of electrocautery generated smoke by chromatographic-mass spectrometry.

    Science.gov (United States)

    Kalil, Jefferson; Pessine, Francisco B T; Fidelis, Carlos H V; Menezes, Fabio H; Palma, Paulo Cesar Rodrigues

    2016-01-01

    to analyze the chemical components of the smoke from electrocautery from coagulating muscle and liver tissues of pigs. we collected smoke produced by electrocautery applied to porcine tissue in previously evacuated bottles, with qualitative and quantitative analysis of the compounds present through the hyphenated technique gas chromatography / mass spectrometry. there was a majority of decanal aldehyde in the fumes from the subcutaneous, muscle and liver tissues. Fumes of subcutaneous and muscular tissues also showed the presence of hexanal and phenol. In the fumes of subcutaneous and liver tissues we also found toluene and limonene and, finally, nonanal smoke was present in the muscle and liver tissues. there is increasing evidence showing that smoke from electrocautery used in subcutaneous, muscle and liver tissue is harmful to human health. Thus, there is need to reduce exposure to it or wear masks with filters capable of retaining these particles. analisar quimicamente os componentes da fumaça do eletrocautério, provenientes da coagulação de tecidos, muscular e hepático de suino. coleta de fumaça produzida por eletrocauterização de tecido porcino em frascos previamente evacuados com análise qualitativa e quantitativa dos compostos presentes, através de técnica hifenada, cromatografia a gás/espectrometria de massas. houve presença majoritária do aldeído decanal nas fumaças provenientes dos tecidos subcutâneo, muscular e hepático. Fumaças dos tecidos subcutâneo e muscular mostraram também a presença de hexanal e fenol. Nas fumaças dos tecidos subcutâneo e hepático foram encontrados ainda tolueno e limoneno e, por fim, nonanal estava presente nas fumaças dos tecidos muscular e hepático. há número crescente de evidências mostrando que fumaça proveniente de eletrocauterização de tecidos subcutâneo, muscular e hepático é nociva à saúde de seres humanos. Portanto, há necessidade de reduzir a exposição a ela ou usar máscara com

  16. Helium-3 mass spectrometry for low-level tritium analysis of environmental samples

    International Nuclear Information System (INIS)

    Surano, K.A.; Hudson, G.B.; Failor, R.A.; Sims, J.M.; Holland, R.C.; MacLean, S.C.; Garrison, J.C.

    1991-04-01

    Helium-3 ( 3 He) mass spectrometry for the analysis of low-level tritium ( 3 H) concentrations in environmental sample matrices was compared with conventional low-level β-decay counting methods. The mass-spectrometry method compared favorably, equaling or surpassing conventional decay-counting methods with respect to most criteria. Additional research and method refinements may make 3 He mass spectrometry the method of choice for routine, low-level to very-low-level 3 H measurements in a wide variety of environmental samples in the future

  17. Early prediction of wheat quality: analysis during grain development using mass spectrometry and multivariate data analysis

    DEFF Research Database (Denmark)

    Ghirardo, A.; Sørensen, Helle Aagaard; Petersen, M.

    2005-01-01

    Matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry and multivariate data analysis have been used for the determination of wheat quality at different stages of grain development. Wheat varieties with one of two different end-use qualities (i.e. suitable or not suitable...... data analysis, offers a method that can replace the traditional rather time-consuming ones such as gel electrophoresis. This study focused on the determination of wheat quality at 15 dpa, when the grain is due for harvest 1 month later....

  18. 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...

  19. Gamma spectrometry analysis of fertilizers used in Costa Rica

    International Nuclear Information System (INIS)

    Loria, L.G.; Jimenez, R.; Badilla, M.

    2002-01-01

    Using the low level gamma spectrometry technique, the specific activity of natural and artificial isotopes present in national consumption fertilizers, supplied by local dealers, was quantified. The most outstanding isotope found in some of the fertilizers is U 235 , with an specific activity higher than the expected in this kind of product, which might mean that this isotope comes from imported raw material. (Author) [es

  20. Analysis of Ketones by Selected Ion Flow Tube Mass Spectrometry

    Czech Academy of Sciences Publication Activity Database

    Smith, D.; Wang, T.; Španěl, Patrik

    2003-01-01

    Roč. 17, - (2003), s. 2655-2660 ISSN 0951-4198 R&D Projects: GA ČR GA202/03/0827; GA ČR GA203/02/0737 Institutional research plan: CEZ:AV0Z4040901 Keywords : mass spectrometry * selected ion flow tube * ketones Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.789, year: 2003

  1. Multivariate techniques of analysis for ToF-E recoil spectrometry data

    Energy Technology Data Exchange (ETDEWEB)

    Whitlow, H J; Bouanani, M E; Persson, L; Hult, M; Jonsson, P; Johnston, P N [Lund Institute of Technology, Solvegatan, (Sweden), Department of Nuclear Physics; Andersson, M [Uppsala Univ. (Sweden). Dept. of Organic Chemistry; Ostling, M; Zaring, C [Royal institute of Technology, Electrum, Kista, (Sweden), Department of Electronics; Johnston, P N; Bubb, I F; Walker, B R; Stannard, W B [Royal Melbourne Inst. of Tech., VIC (Australia); Cohen, D D; Dytlewski, N [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia)

    1997-12-31

    Multivariate statistical methods are being developed by the Australian -Swedish Recoil Spectrometry Collaboration for quantitative analysis of the wealth of information in Time of Flight (ToF) and energy dispersive Recoil Spectrometry. An overview is presented of progress made in the use of multivariate techniques for energy calibration, separation of mass-overlapped signals and simulation of ToF-E data. 6 refs., 5 figs.

  2. Multivariate techniques of analysis for ToF-E recoil spectrometry data

    Energy Technology Data Exchange (ETDEWEB)

    Whitlow, H.J.; Bouanani, M.E.; Persson, L.; Hult, M.; Jonsson, P.; Johnston, P.N. [Lund Institute of Technology, Solvegatan, (Sweden), Department of Nuclear Physics; Andersson, M. [Uppsala Univ. (Sweden). Dept. of Organic Chemistry; Ostling, M.; Zaring, C. [Royal institute of Technology, Electrum, Kista, (Sweden), Department of Electronics; Johnston, P.N.; Bubb, I.F.; Walker, B.R.; Stannard, W.B. [Royal Melbourne Inst. of Tech., VIC (Australia); Cohen, D.D.; Dytlewski, N. [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia)

    1996-12-31

    Multivariate statistical methods are being developed by the Australian -Swedish Recoil Spectrometry Collaboration for quantitative analysis of the wealth of information in Time of Flight (ToF) and energy dispersive Recoil Spectrometry. An overview is presented of progress made in the use of multivariate techniques for energy calibration, separation of mass-overlapped signals and simulation of ToF-E data. 6 refs., 5 figs.

  3. Application of Pyrolysis - Gas Chromatography/Mass Spectrometry in Failure Analysis in the Automotive Industry

    OpenAIRE

    Kusch, Peter (Dr.)

    2015-01-01

    This book chapter describes application examples of gas chromatography/mass spectrometry and pyrolysis – gas chromatography/mass spectrometry in failure analysis for the identification of chemical materials like mineral oils and nitrile rubber gaskets. Furthermore, failure cases demanding identification of polymers/copolymers in fouling on the compressor wall of a car air conditioner and identification of fouling on the surface of a bearing race from the automotive industry are demonstr...

  4. 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

  5. Direct Analysis of Large Living Organism by Megavolt Electrostatic Ionization Mass Spectrometry

    Science.gov (United States)

    Ng, Kwan-Ming; Tang, Ho-Wai; Man, Sin-Heng; Mak, Pui-Yuk; Choi, Yi-Ching; Wong, Melody Yee-Man

    2014-09-01

    A new ambient ionization method allowing the direct chemical analysis of living human body by mass spectrometry (MS) was developed. This MS method, namely Megavolt Electrostatic Ionization Mass Spectrometry, is based on electrostatic charging of a living individual to megavolt (MV) potential, illicit drugs, and explosives on skin/glove, flammable solvent on cloth/tissue paper, and volatile food substances in breath were readily ionized and detected by a mass spectrometer.

  6. Advancements in mass spectrometry for biological samples: Protein chemical cross-linking and metabolite analysis of plant tissues

    Energy Technology Data Exchange (ETDEWEB)

    Klein, Adam [Iowa State Univ., Ames, IA (United States)

    2015-01-01

    This thesis presents work on advancements and applications of methodology for the analysis of biological samples using mass spectrometry. Included in this work are improvements to chemical cross-linking mass spectrometry (CXMS) for the study of protein structures and mass spectrometry imaging and quantitative analysis to study plant metabolites. Applications include using matrix-assisted laser desorption/ionization-mass spectrometry imaging (MALDI-MSI) to further explore metabolic heterogeneity in plant tissues and chemical interactions at the interface between plants and pests. Additional work was focused on developing liquid chromatography-mass spectrometry (LC-MS) methods to investigate metabolites associated with plant-pest interactions.

  7. An approach to unfold the response of a multi-element system using an artificial neural network

    International Nuclear Information System (INIS)

    Cordes, E.; Fehrenbacher, G.; Schuetz, R.; Sprunck, M.; Hahn, K.; Hofmann, R.; Wahl, W.

    1998-01-01

    An unfolding procedure is proposed which aims at obtaining spectral information of a neutron radiation field by the analysis of the response of a multi-element system consisting of converter type semiconductors. For the unfolding procedure an artificial neural network (feed forward network), trained by the back-propagation method, was used. The response functions of the single elements to neutron radiation were calculated by application of a computational model for an energy range from 10 -2 eV to 10 MeV. The training of the artificial neural network was based on the computation of responses of a six-element system for a set of 300 neutron spectra and the application of the back-propagation method. The validation was performed by the unfolding of 100 computed responses. Two unfolding examples were pointed out for the determination of the neutron spectra. The spectra resulting from the unfolding procedure agree well with the original spectra used for the response computation

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

    Science.gov (United States)

    Ranjan, Pinku; Gangwar, Ravi Kumar

    2017-12-01

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

  9. Diversity and MIMO Performance Evaluation of Common Phase Center Multi Element Antenna Systems

    Directory of Open Access Journals (Sweden)

    V. Papamichael

    2008-06-01

    Full Text Available The diversity and Multiple Input Multiple Output (MIMO performance provided by common phase center multi element antenna (CPCMEA systems is evaluated using two practical methods which make use of the realized active element antenna patterns. These patterns include both the impact of the mutual coupling and the mismatch power loss at antenna ports. As a case study, two and four printed Inverted F Antenna (IFA systems are evaluated by means of Effective Diversity Gain (EDG and Capacity (C. EDG is measured in terms of the signal-to-noise ratio (SNR enhancement at a specific outage probability and in terms of the SNR reduction for achieving a desired average bit error rate (BER. The concept of receive antenna selection in MIMO systems is also investigated and the simulation results show a 43% improvement in the 1% outage C of a reconfigurable 2x2 MIMO system over a fixed 2x2 one.

  10. Process recognition in multi-element soil and stream-sediment geochemical data

    Science.gov (United States)

    Grunsky, E.C.; Drew, L.J.; Sutphin, D.M.

    2009-01-01

    Stream-sediment and soil geochemical data from the Upper and Lower Coastal Plains of South Carolina (USA) were studied to determine relationships between soils and stream sediments. From multi-element associations, characteristic compositions were determined for both media. Primary associations of elements reflect mineralogy, including heavy minerals, carbonates and clays, and the effects of groundwater. The effects of groundwater on element concentrations are more evident in soils than stream sediments. A "winnowing index" was created using ratios of Th to Al that revealed differing erosional and depositional environments. Both soils and stream sediments from the Upper and Lower Coastal Plains show derivation from similar materials and subsequent similar multi-element relationships, but have some distinct differences. In the Lower Coastal Plain, soils have high values of elements concentrated in heavy minerals (Ce, Y, Th) that grade into high values of elements concentrated into finer-grain-size, lower-density materials, primarily comprised of carbonates and feldspar minerals (Mg, Ca, Na, K, Al). These gradational trends in mineralogy and geochemistry are inferred to reflect reworking of materials during marine transgressions and regressions. Upper Coastal Plain stream-sediment geochemistry shows a higher winnowing index relative to soil geochemistry. A comparison of the 4 media (Upper Coastal Plain soils and stream sediments and Lower Coastal Plain soils and stream sediments) shows that Upper Coastal Plain stream sediments have a higher winnowing index and a higher concentration of elements contained within heavy minerals, whereas Lower Coastal Plain stream sediments show a strong correlation between elements typically contained within clays. It is not possible to calculate a functional relationship between stream sediment-soil compositions for all elements due to the complex history of weathering, deposition, reworking and re-deposition. However, depending on

  11. Doping control analysis of anabolic steroids in equine urine by gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Wong, April S Y; Leung, Gary N W; Leung, David K K; Wan, Terence S M

    2017-09-01

    Anabolic steroids are banned substances in equine sports. Gas chromatography-mass spectrometry (GC-MS) has been the traditional technique for doping control analysis of anabolic steroids in biological samples. Although liquid chromatography-mass spectrometry (LC/MS) has become an important technique in doping control, the detection of saturated hydroxysteroids by LC-MS remains a problem due to their low ionization efficiency under electrospray. The recent development in fast-scanning gas-chromatography-triple-quadrupole mass spectrometry (GC-MS/MS) has provided a better alternative with a significant reduction in chemical noise by means of selective reaction monitoring. Herein, we present a sensitive and selective method for the screening of over 50 anabolic steroids in equine urine using gas chromatography-tandem mass spectrometry (GC-MS/MS). Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  12. Rare earth aerosol analysis by x-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Citron, I.M.; Mausner, L.F.

    1982-01-01

    An analytical method for the determination of four lanthanides in air filter samples is described. The method involves simultaneous quantitative determinations of La, Ce, Pr, and Nd at the microgram level by x-ray fluorescence spectrometry without chemical separation of these rare earths and without serious interferences from the dust matrices on the filters. The method has been used successfully to analyze some air filter samples collected at a rare earth processing refinery in Illinois. A description of the development of the method is given as well as the results obtained by using this method on the air filter samples. The reproducibility of the results was generally +-5%

  13. Two possible improvements for mass spectrometry analysis of intact biomolecules.

    Science.gov (United States)

    Raznikov, Valeriy V; Zelenov, Vladislav V; Aparina, Elena V; Pikhtelev, Alexander R; Sulimenkov, Ilia V; Raznikova, Marina O

    2017-08-01

    The goals of our study were to investigate abilities of two approaches to eliminate possible errors in electrospray mass spectrometry measurements of biomolecules. Passing of a relatively dense supersonic gas jet through ionization region followed by its hitting the spray of the analyzed solution in low vacuum may be effective to keep an initial biomolecule structure in solution. Provided that retention of charge carriers for some sites in the biomolecule cannot be changed noticeably in electrospray ion source, decomposition and separation of charge-state distributions of electrosprayed ions may give additional information about native structure of biomolecules in solution.

  14. Validation of Plutonium Radioisotopes Analysis Using Alpha Spectrometry

    International Nuclear Information System (INIS)

    Noor Fadzilah Yusof; Jalal Sharib; Mohd Tarmizi Ishak; Zulkifli Daud; Abdul Kadir Ishak

    2016-01-01

    This paper presents the validation of an established method used to detect plutonium (Pu) radioisotopes in marine environment samples. The separation method consists of sample digestion, anion exchange, purification, electroplating and counting by an alpha spectrometry. Applying the method on standard reference materials from marine environment, the results are validated using seven parameters, namely specificity, linearity, bias or accuracy, detection limit, precision/ repeatability, reproducibility/ ruggedness and robustness in accordance with International Organization for Standardization (ISO) guidelines. The findings were that the results obtained were in a good agreement and satisfactory compared to the provided readings from certificate of reference materials. (author)

  15. [Mass spectrometry technology and its application in analysis of biological samples].

    Science.gov (United States)

    Zhao, Long-Shan; Li, Qing; Guo, Chao-Wei; Chen, Xiao-Hui; Bi, Kai-Shun

    2012-02-01

    With the excellent merits of wide analytical range, high sensitivity, small sample size, fast analysis speed, good repeatability, simple operation, low mobile phase consumption, as well as its capability of simultaneous isolation and identification, etc, mass spectrometry techniques have become widely used in the area of environmental science, energy chemical industry, biological medicine, and so on. This article reviews the application of mass spectrometry technology in biological sample analysis in the latest three years with the focus on the new applications in pharmacokinetics and bioequivalence, toxicokinetics, pharmacokinetic-pharmacodynamic, population pharmacokinetics, identification and fragmentation pathways of drugs and their metabolites and metabonomics to provide references for further study of biological sample analysis.

  16. Use of gamma spectrometry for analysis of three reference materials

    International Nuclear Information System (INIS)

    Kinova, L.

    2004-01-01

    All reference materials (Reference material A: weight = 49.23 g; Reference material B: weight = 36.08 g; Reference material C: weight = 26.18 g) were packed in 50 cm 3 polypropylene vials, sealed and measured consecutively three times at intervals of the average of 25 days. Low background gamma spectrometry system: HPGe detector with high energy resolution (FWHM for 1332 KeV of Co-60 is 1.9 KeV, Relative counting efficiency for the same energy is 21 %) was used. Results: All materials are of low activity and must be measured for a long time.The highest specific activity of a man-made radionuclides Cs-137 and Am-241 is in the material A. An instrumentally measurable activity of Pb-210 also can be observed in this material. Medium values are in the material B. The reference material C according to the specific activity seems to be a low natural radioactivity material with highest activity of natural nuclides Th-232 and Pa-234 (progeny of U-238). Conclusions: Gamma spectrometry is an useful tool for initial measurement of materials with low radioactivity. Such measurements give an orientation for the nuclides content and approximate activity in the material for the following radiochemical determinations

  17. Use of Tritium Accelerator Mass Spectrometry for Tree Ring Analysis

    Science.gov (United States)

    LOVE, ADAM H.; HUNT, JAMES R.; ROBERTS, MARK L.; SOUTHON, JOHN R.; CHIARAPPA - ZUCCA, MARINA L.; DINGLEY, KAREN H.

    2010-01-01

    Public concerns over the health effects associated with low-level and long-term exposure to tritium released from industrial point sources have generated the demand for better methods to evaluate historical tritium exposure levels for these communities. The cellulose of trees accurately reflects the tritium concentration in the source water and may contain the only historical record of tritium exposure. The tritium activity in the annual rings of a tree was measured using accelerator mass spectrometry to reconstruct historical annual averages of tritium exposure. Milligram-sized samples of the annual tree rings from a Tamarix located at the Nevada Test Site are used for validation of this methodology. The salt cedar was chosen since it had a single source of tritiated water that was well-characterized as it varied over time. The decay-corrected tritium activity of the water in which the salt cedar grew closely agrees with the organically bound tritium activity in its annual rings. This demonstrates that the milligram-sized samples used in tritium accelerator mass spectrometry are suited for reconstructing anthropogenic tritium levels in the environment. PMID:12144257

  18. Impact of comprehensive two-dimensional gas chromatography with mass spectrometry on food analysis.

    Science.gov (United States)

    Tranchida, Peter Q; Purcaro, Giorgia; Maimone, Mariarosa; Mondello, Luigi

    2016-01-01

    Comprehensive two-dimensional gas chromatography with mass spectrometry has been on the separation-science scene for about 15 years. This three-dimensional method has made a great positive impact on various fields of research, and among these that related to food analysis is certainly at the forefront. The present critical review is based on the use of comprehensive two-dimensional gas chromatography with mass spectrometry in the untargeted (general qualitative profiling and fingerprinting) and targeted analysis of food volatiles; attention is focused not only on its potential in such applications, but also on how recent advances in comprehensive two-dimensional gas chromatography with mass spectrometry will potentially be important for food analysis. Additionally, emphasis is devoted to the many instances in which straightforward gas chromatography with mass spectrometry is a sufficiently-powerful analytical tool. Finally, possible future scenarios in the comprehensive two-dimensional gas chromatography with mass spectrometry food analysis field are discussed. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Improvement of recovery and repeatability in liquid chromatography-mass spectrometry analysis of peptides

    NARCIS (Netherlands)

    van Midwoud, Paul M.; Rieux, Laurent; Bischoff, Rainer; Verpoorte, Elisabeth; Niederlander, Harm A. G.

    2007-01-01

    Poor repeatability of peak areas is a problem frequently encountered in peptide analysis with nanoLiquid Chromatography coupled on-line with Mass Spectrometry (nanoLC-MS). As a result, quantitative analysis will be seriously hampered unless the observed variability can be corrected in some way.

  20. Laser desorption mass spectrometry for high-throughput DNA analysis and its applications

    Science.gov (United States)

    Chen, C. H. Winston; Golovlev, Valeri V.; Taranenko, N. I.; Allman, S. L.; Isola, Narayana R.; Potter, N. T.; Matteson, K. J.; Chang, Linus Y.

    1999-05-01

    Laser desorption mass spectrometry (LDMS) has been developed for DNA sequencing, disease diagnosis, and DNA fingerprinting for forensic applications. With LDMS, the speed of DNA analysis can be much faster than conventional gel electrophoresis. No dye or radioactive tagging to DNA segments for detection is needed. LDMS is emerging as a new alternative technology for DNA analysis.

  1. Methods for the analysis of the overlapped peaks in analytical gamma-spectrometry

    International Nuclear Information System (INIS)

    Sterlinski, S.; Wasek, M.

    1989-01-01

    A new simple method for the quantitative analysis of the doublet peaks in Ge(Li) or HPGe gamma-spectrometry is presented. No assumptions on the shape of the peaks in gamma-ray spectra being measured are required. Special feature of the method proposed is its usefulness for the analysis of closed doublets. 7 refs., 6 figs. (author)

  2. Desorption electrospray ionization mass spectrometry in the analysis of chemical food contaminants in food

    NARCIS (Netherlands)

    Nielen, M.W.F.; Hooijerink, H.; Zomer, P.; Mol, J.G.J.

    2011-01-01

    Since its introduction, desorption electrospray ionization (DESI) mass spectrometry (MS) has been mainly applied in pharmaceutical and forensic analysis. We expect that DESI will find its way in many different fields, including food analysis. In this review, we summarize DESI developments aimed at

  3. Indexing and Analysis of Fungal Phenotypes Using Morphology and Spectrometry

    DEFF Research Database (Denmark)

    Hansen, Michael Adsetts Edberg

    2005-01-01

    and identification of the fungi is considered difficult and laborious. Though visual expressions have been and still is used as phenotype markers in the classification and identification of fungal species, one of the most successful characters used has been the profile of the secondary metabolites. In order...... to evaluate the visual phenotypic characters, a method for visual clone identification of Penicillium commune { the most widespread and most frequently occurring spoilage fungus on cheese { was developed (Papers A, B and C). The method was based on images of fungal colonies acquired after growth on a standard...... extract highly complex and similar ESI-MS mass spectra for identifying fungal extracts in a reference library are being developed and tested (Paper E). Whereas mass spectrometry is one modality used in systematising the fungi, high pressure liquid chromatography combined with an UV diode array detector...

  4. Analysis of cigarette smoke by Fourier transform infrared spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Maddox, W.L. (Oak Ridge National Lab., TN); Mamantov, G.

    1977-02-01

    The application of Fourier transform infrared spectrometry (FT-IR) to the quantitative determination of several components in the gas phase of whole, dilute tobacco smoke was demonstrated. The 18-cm absorption cell was part of a cigarette smoking system similar to the intermittent inhalation exposure devices used in smoking and health research with rodents. Concentrations were measured for carbon monoxide, carbon dioxide, methane, ethylene, and methanol in 7 to 22% smoke. The precision of a measurement in 22% smoke ranged from 3% for carbon dioxide to 34% for ethylene. Absorbances measured for isoprene and hydrogen cyanide followed expected concentrations in different cigarette smokes. It was shown that the concentrations of these components remain constant during a 30-s hold-up following each puff on the cigarettes.

  5. Quality assurance for mass spectrometry research and development analysis

    International Nuclear Information System (INIS)

    Piciorea, Iuliana; Vremera, Raluca; Calota, Iulian Virgil

    2008-01-01

    Full text: A well functioning quality system need not stifle creativity in R and D, and is vital for ensuring the smooth transfer of technology from research to diagnostic or commercial environments. Research workers must have an evaluation of the quality requirements of clients and quality must be ensured by design in every process. No single method of assessment stands out as being the most suitable for monitoring the quality of non-routine and R and D work. It is recommended that where some kind of external assessment is required a combination of approaches should be conducted and formal assessment should be confined wherever possible to those parts of the quality system that remain stable from project to project, e.g. the management levels and technical infrastructure. Illustrations for the case of organophosphorus materials, mass spectrometry research and developments are presented. (authors)

  6. Analysis of sulfates on low molecular weight heparin using mass spectrometry: structural characterization of enoxaparin.

    Science.gov (United States)

    Gupta, Rohitesh; Ponnusamy, Moorthy P

    2018-05-21

    Structural characterization of Low Molecular Weight Heparin (LMWH) is critical to meet biosimilarity standards. In this context, the review focuses on structural analysis of labile sulfates attached to the side-groups of LMWH using mass spectrometry. A comprehensive review of this topic will help readers to identify key strategies for tackling the problem related to sulfate loss. At the same time, various mass spectrometry techniques are presented to facilitate compositional analysis of LMWH, mainly Enoxaparin. Areas covered: This review summarizes findings on mass spectrometry application for LMWH, including modulation of sulfates, using enzymology and sample preparation approaches. Furthermore, popular open-source software packages for automated spectral data interpretation are also discussed. Successful use of LC/MS can decipher structural composition for LMWH and help evaluate their sameness or biosimilarity with the innovator molecule. Overall, the literature has been searched using PubMed by typing various search queries such as "enoxaparin", "mass spectrometry", "low molecular weight heparin", "structural characterization", etc. Expert commentary: This section highlights clinically relevant areas that need improvement to achieve satisfactory commercialization of LMWHs. It also primarily emphasizes the advancements in instrumentation related to mass spectrometry, and discusses building automated software for data interpretation and analysis.

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

    Science.gov (United States)

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

    2004-01-01

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

  8. Surface analysis of lipids by mass spectrometry: more than just imaging.

    Science.gov (United States)

    Ellis, Shane R; Brown, Simon H; In Het Panhuis, Marc; Blanksby, Stephen J; Mitchell, Todd W

    2013-10-01

    Mass spectrometry is now an indispensable tool for lipid analysis and is arguably the driving force in the renaissance of lipid research. In its various forms, mass spectrometry is uniquely capable of resolving the extensive compositional and structural diversity of lipids in biological systems. Furthermore, it provides the ability to accurately quantify molecular-level changes in lipid populations associated with changes in metabolism and environment; bringing lipid science to the "omics" age. The recent explosion of mass spectrometry-based surface analysis techniques is fuelling further expansion of the lipidomics field. This is evidenced by the numerous papers published on the subject of mass spectrometric imaging of lipids in recent years. While imaging mass spectrometry provides new and exciting possibilities, it is but one of the many opportunities direct surface analysis offers the lipid researcher. In this review we describe the current state-of-the-art in the direct surface analysis of lipids with a focus on tissue sections, intact cells and thin-layer chromatography substrates. The suitability of these different approaches towards analysis of the major lipid classes along with their current and potential applications in the field of lipid analysis are evaluated. Copyright © 2013 Elsevier Ltd. All rights reserved.

  9. 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

  10. Accelerator mass spectrometry: ultrasensitive analysis of global science

    International Nuclear Information System (INIS)

    Tuniz, C.; Bird, J.B.; Fink, D.; Herzog, G.F.

    1998-01-01

    Accelerator mass spectrometry (AMS), an innovative analytical technique, measures rare atoms at unprecedented levels of sensitivity, revolutionizing the science of radiocarbon dating and accessing new environmental tracers and chronometers. AMS can study extraterrestrial materials, the earth sciences, the future of the global environment, and the history of mankind. The Shroud of Turin, meteorites from Mars, the crown of Charlemagne, and ancient air trapped in Antarctic ice indicate some of the samples on which AMS has been applied. This book has compiled the diverse set of scientific literature into a single volume, suitable as a text or resource on the major AMS-related outcomes, issues, and methods. It explains how scientists and researchers succeeded in counting Carbon-14 atoms at an extraordinary level, examines the impact of AMS on the branches of scientific technology and historical research, provides an understanding of the chronology and significance of past and present environmental changes, details the advances in AMS equipment, technology, and methods as well as the expansion of AMS research

  11. Embedded gamma spectrometry: new algorithms for spectral analysis

    International Nuclear Information System (INIS)

    Martin-Burtart, Nicolas

    2012-01-01

    Airborne gamma spectrometry was first used for mining prospecting. Three main families were looked for: K-40, U-238 and Th-232. The Chernobyl accident acted as a trigger and for the last fifteen years, a lot of new systems have been developed for intervention in case of nuclear accident or environmental purposes. Depending on their uses, new algorithms were developed, mainly for medium or high energy signal extraction. These spectral regions are characteristics of natural emissions (K-40, U-238 and Th-232 decay chains) and fissions products (mainly Cs-137 and Co-60). Below 400 keV, where special nuclear materials emit, these methods can still be used but are greatly imprecise. A new algorithm called 2-windows (extended to 3), was developed. It allows an accurate extraction, taking the flight altitude into account to minimize false detection. Watching radioactive materials traffic appeared with homeland security policy a few years ago. This particular use of dedicated sensors require a new type of algorithms. Before, one algorithm was very efficient for a particular nuclide or spectral region. Now, we need algorithm able to detect an anomaly wherever it is and whatever it is: industrial, medical or SNM. This work identified two families of methods working under these circumstances. Finally, anomalies have to be identified. IAEA recommend to watch around 30 radionuclides. A brand new identification algorithm was developed, using several rays per element and avoiding identifications conflicts. (author) [fr

  12. Mass spectrometry analysis of tank wastes at the Hanford Site

    International Nuclear Information System (INIS)

    Campbell, J.A.; Mong, G.M.; Clauss, S.A.

    1995-01-01

    Twenty-five of the 177 high-level waste storage tanks at the Hanford Site in southeastern Washington are being watched closely because of the possibility that flammable gas mixtures may be produced from the mixed wastes contained in the storage tanks. One tank in particular, Tank 241-SY-101 (Tank 101-SY), has exhibited episodic releases of flammable gas mixtures since its final filling in the early 1980s. It has been postulated that the organic compounds present in the waste may be precursors to the production of hydrogen. Mass spectrometry has proven to be an invaluable tool for the identification of organic components in wastes from Tank 101-SY and C-103. A suite of physical and chemical analyses has been performed in support of activities directed toward the resolution of an Unresolved Safety Question concerning the potential for a floating organic layer in Hanford Waste Tank 241-C-103 to sustain a pool fire. The aqueous layer underlying the floating organic material was also analyzed for organic components

  13. Resonant laser mass spectrometry for environmental and industrial chemical trace analysis

    International Nuclear Information System (INIS)

    Boesl, Ulrich; Rink, Joerg; Distelrath, Volker; Pueffel, Peter

    2001-01-01

    A promising new method for pollutant trace analysis is resonant laser mass spectrometry. It combines selectivity, sensitivity, and speed of measurement. In this paper, two examples of application are presented: exhaust analysis of combustion engines and analysis of polycylcic aromatic compounds in soil samples. The sensitivity of small, mobile instruments is discussed as well as alternative laser-based techniques in the case formation of cations by nanosecond lasers is improbable

  14. Progress in multi-element silicon detectors for synchrotron XRF applications

    International Nuclear Information System (INIS)

    Ludewigt, B.; Rossington, C.; Kipnis, I.; Krieger, B.

    1995-10-01

    Multi-element silicon strip detectors, in conjunction with integrated circuit pulse-processing electronics, offer an attractive alternative to conventional lithium-drifted silicon and high purity germanium detectors for high count rate, low noise synchrotron x-ray fluorescence applications. We have been developing these types of detectors specifically for low noise synchrotron applications, such as extended x-ray absorption fine structure spectroscopy, microprobe x-ray fluorescence and total reflection x-ray fluorescence. The current version of the 192-element detector and integrated circuit preamplifier, cooled to -25 degrees C with a single-stage thermoelectric cooler, achieves an energy resolution of <200 eV full width of half maximum (FWHM) per channel (at 5.9 keV, 2 μs peaking time), and each detector element is designed to handle ∼20 kHz count rate. The detector system will soon be completed to 64 channels using new application specific integrated circuit (ASIC) amplifier chips, new CAMAC (Computer Automated Measurement and Control standard) analog-to-digital converters recently developed at Lawrence Berkeley National Laboratory (LBNL), CAMAC histogramming modules, and Macintosh-based data acquisition software. We report on the characteristics of this detector system, and the work in progress towards the next generation system

  15. An adaptive multi-element probabilistic collocation method for statistical EMC/EMI characterization

    KAUST Repository

    Yücel, Abdulkadir C.

    2013-12-01

    An adaptive multi-element probabilistic collocation (ME-PC) method for quantifying uncertainties in electromagnetic compatibility and interference phenomena involving electrically large, multi-scale, and complex platforms is presented. The method permits the efficient and accurate statistical characterization of observables (i.e., quantities of interest such as coupled voltages) that potentially vary rapidly and/or are discontinuous in the random variables (i.e., parameters that characterize uncertainty in a system\\'s geometry, configuration, or excitation). The method achieves its efficiency and accuracy by recursively and adaptively dividing the domain of the random variables into subdomains using as a guide the decay rate of relative error in a polynomial chaos expansion of the observables. While constructing local polynomial expansions on each subdomain, a fast integral-equation-based deterministic field-cable-circuit simulator is used to compute the observable values at the collocation/integration points determined by the adaptive ME-PC scheme. The adaptive ME-PC scheme requires far fewer (computationally costly) deterministic simulations than traditional polynomial chaos collocation and Monte Carlo methods for computing averages, standard deviations, and probability density functions of rapidly varying observables. The efficiency and accuracy of the method are demonstrated via its applications to the statistical characterization of voltages in shielded/unshielded microwave amplifiers and magnetic fields induced on car tire pressure sensors. © 2013 IEEE.

  16. The Multi-Element Electronstatic Lens Systems for Controlling and Focusing Charged Particle

    International Nuclear Information System (INIS)

    Sise, O.

    2004-01-01

    Particle optics are very close anolog of photon optics and most of the principles of an barged particle beam can be understood by thinking of the particles as rays of light. There are similar behaviours between particle and photon optics in controlling beams of light and charged particles, such as lenses and mirrors. Extensive information about the properties of charged particle optics, from which appropriate systems can be designed for any specific problem. In this way electrostatic lens systems are used to control beams of c/iarged particle with various energy and directions in several fields, for example electron microscopy, cathode ray tubes, ion accelerators and electron impact studies. In an electrostatic lens system quantative information is required over a wide energy range and a zoom-type of optics is needed. If the magnification is to remain constant over a wide range of energies, quite complicated electrostatic lens systems are required, .containing three, four, five, or even more lens elements. We firstly calculated the optical properties of three and four element cylinder electrostatic lenses with the help of the SIMION and LENSYS programs and developed the method for the calculation of the focal properties of five and more element lenses with afocal mode. In this method we used the combination of three and four element lenses to derive focal properties of multi-element lenses and presented this data over a wide range of energy

  17. Compact electrostatic beam optics for multi-element focused ion beams: simulation and experiments.

    Science.gov (United States)

    Mathew, Jose V; Bhattacharjee, Sudeep

    2011-01-01

    Electrostatic beam optics for a multi-element focused ion beam (MEFIB) system comprising of a microwave multicusp plasma (ion) source is designed with the help of two widely known and commercially available beam simulation codes: AXCEL-INP and SIMION. The input parameters to the simulations are obtained from experiments carried out in the system. A single and a double Einzel lens system (ELS) with and without beam limiting apertures (S) have been investigated. For a 1 mm beam at the plasma electrode aperture, the rms emittance of the focused ion beam is found to reduce from ∼0.9 mm mrad for single ELS to ∼0.5 mm mrad for a double ELS, when S of 0.5 mm aperture size is employed. The emittance can be further improved to ∼0.1 mm mrad by maintaining S at ground potential, leading to reduction in beam spot size (∼10 μm). The double ELS design is optimized for different electrode geometrical parameters with tolerances of ±1 mm in electrode thickness, electrode aperture, inter electrode distance, and ±1° in electrode angle, providing a robust design. Experimental results obtained with the double ELS for the focused beam current and spot size, agree reasonably well with the simulations.

  18. Experimental Combustion Dynamics Behavior of a Multi-Element Lean Direct Injection (LDI) Gas Turbine Combustor

    Science.gov (United States)

    Acosta, Waldo A.; Chang, Clarence T.

    2016-01-01

    An experimental investigation of the combustion dynamic characteristics of a research multi-element lean direct injection (LDI) combustor under simulated gas turbine conditions was conducted. The objective was to gain a better understanding of the physical phenomena inside a pressurized flametube combustion chamber under acoustically isolated conditions. A nine-point swirl venturi lean direct injection (SV-LDI) geometry was evaluated at inlet pressures up to 2,413 kPa and non-vitiated air temperatures up to 867 K. The equivalence ratio was varied to obtain adiabatic flame temperatures between 1388 K and 1905 K. Dynamic pressure measurements were taken upstream of the SV-LDI, in the combustion zone and downstream of the exit nozzle. The measurements showed that combustion dynamics were fairly small when the fuel was distributed uniformly and mostly due to fluid dynamics effects. Dynamic pressure fluctuations larger than 40 kPa at low frequencies were measured at 653 K inlet temperature and 1117 kPa inlet pressure when fuel was shifted and the pilot fuel injector equivalence ratio was increased to 0.72.

  19. A Study of Two Multi-Element Resonant DC-DC Topologies with Loss Distribution Analyses

    Directory of Open Access Journals (Sweden)

    Yifeng Wang

    2017-09-01

    Full Text Available In this paper, two multi-element resonant DC-DC converters are analyzed in detail. Since their resonant tanks have multiple resonant components, the converters display different resonant characteristics within different operating frequency ranges. Through appropriate design, both of the two proposed converters successfully lower the conversion losses and, meanwhile, broaden the voltage gain ranges as well: one converter is able to take full usage of the third order harmonic to deliver the active power, and thus the effective utilization rate of the resonant current is elevated; while the another minimizes the entire switching losses for power switching devices by restricting the input impedance angle of the resonant tank. Besides, the loss distribution is analyzed for the purpose of guiding the component design. In the end, two 500 W prototypes are fabricated to test the theoretical analyses. The results demonstrate that the two proposed converters can achieve wide voltage gain with the small frequency deviation, which noticeably contributes to highly efficient conversion. Their peak efficiencies are measured as 95.4% and 95.3%, respectively.

  20. Simultaneous quantitative analysis of metabolites using ion-pair liquid chromatography-electrospray ionization mass spectrometry

    NARCIS (Netherlands)

    Coulier, L.; Bas, R.; Jespersen, S.; Verheij, E.; Werf, M.J. van der; Hankemeier, T.

    2006-01-01

    We have developed an analytical method, consisting of ion-pair liquid chromatography coupled to electrospray ionization mass spectrometry (IP-LC-ESI-MS), for the simultaneous quantitative analysis of several key classes of polar metabolites, like nucleotides, coenzyme A esters, sugar nucleotides,

  1. Carbohydrate analysis of hemicelluloses by gas chromatography-mass spectrometry of acteylated methyl glycosides

    DEFF Research Database (Denmark)

    Sárossy, Zsuzsa; Plackett, David; Egsgaard, Helge

    2012-01-01

    A method based on gas chromatography–mass spectrometry analysis of acetylated methyl glycosides was developed in order to analyze monosaccharides obtained from various hemicelluloses. The derivatives of monosaccharide standards, arabinose, glucose, and xylose were studied in detail and 13C...

  2. Qualitative and quantitative analysis of pharmaceutical compounds by MALDI-TOF mass spectrometry.

    NARCIS (Netherlands)

    Kampen, J.J. van; Burgers, P.C.; Groot, R. de; Luider, T.M.

    2006-01-01

    In this report, we discuss key issues for the successful application of MALDI-TOF mass spectrometry to quantify drugs. These include choice and preparation of matrix, nature of cationization agent, automation, and data analysis procedures. The high molecular weight matrix

  3. The first results of measurements in military hospital laboratory for gamma spectrometry analysis

    International Nuclear Information System (INIS)

    Jankovic, Lj.; Pantelic, G.; Misovic, M.

    1997-01-01

    In this paper we present the basic features of the equipment for gamma spectrometry analysis and the first measurements results of the 134 Cs and 137 Cs activities. Gamma spectrum is measured using HP GE Detector. The obtained results show low level activities of the 134 Cs and 137 Cs in the environment. (author)

  4. COMPREHENSIVE ANALYSIS OF BIOLOGICALLY RELEVANT ARSENICALS BY PH-SELECTIVE HYDRIDE GENERATION-ATOMIC ABSORPTION SPECTROMETRY

    Science.gov (United States)

    A method based on pH-selective generation and separation of arsines is commonly used for analysis of inorganic, methylated, and dimethylated trivalent and pentavalent arsenicals by hydride generation-atomic absorption spectrometry (HG-AAS). We have optimized this method to pe...

  5. Study of aging mechanism of ammonium dinitramide using thermal analysis and spectrometry

    OpenAIRE

    Matsunaga, Hiroki; Yoshino, Satoru; Kumasaki, Mieko; Miyake, Atsumi; Habu, Hiroto; 松永, 浩貴; 吉野, 悟; 熊崎, 美枝子; 三宅, 淳巳; 羽生, 宏人

    2011-01-01

    To get better information about aging mechanism of ammonium dinitramide (ADN) during storage, thermal analysis and spectrometry were carried out. The infrared, Raman, ultraviolet spectrometry and the sealed cell differential scanning calorimetry (SC-DSC) of AND (1998) which has been stored for 11 years in a dark place suggested that ADN has degraded to ammonium nitrate (AN) during the storage. The amount of ADN in AND (1998) was determined to be 57 wt.% at the surface region and 89 wt.% at th...

  6. Optical spectroscopy versus mass spectrometry: The race for fieldable isotopic analysis

    International Nuclear Information System (INIS)

    Barshick, C.M.; Young, J.P.; Shaw, R.W.

    1995-01-01

    Several techniques have been developed to provide on-site isotopic analyses, including decay-counting and mass spectrometry, as well as methods that rely on the accessibility of optical transitions for isotopic selectivity (e.g., laser-induced fluorescence and optogalvanic spectroscopy). The authors have been investigating both mass spectrometry and optogalvanic spectroscopy for several years. Although others have considered these techniques for isotopic analysis, the authors have focussed on the use of a dc glow discharge for atomization and ionization, and a demountable discharge cell for rapid sample exchange. The authors' goal is a fieldable instrument that provides useful uranium isotope ratio information

  7. 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....

  8. Simultaneous analysis of amino acid and organic acid by NMR spectrometry, 2

    International Nuclear Information System (INIS)

    Koda, Naoya; Yamaguchi, Shuichi; Mori, Takeshi.

    1987-01-01

    Analysis of urine from patients with inborn error of metabolism were studied by 1 H-nuclear magnetic resonance (NMR) spectrometry. Diseases studied were as follows; phenylketonuria, biotin responsive multiple carboxylase deficiency, non-ketotic hyperglycinemia, 3-ketothiolase deficiency, alkaptonuria, methylmalonic acidemia, isovaleric acidemia, glutaric aciduria, argininosuccinic aciduria and hyperornithinemia. In each disease, specific metabolites in urine were recognized by NMR spectrometry. This method is accomplished within 10 minutes with non-treated small volume of urine and will be successfully available for the screening and/or diagnosis of inherited metabolic diseases of amino acid and organic acid. (author)

  9. An analysis of nuclear fuel burnup in the AGR-1 TRISO fuel experiment using gamma spectrometry, mass spectrometry, and computational simulation techniques

    International Nuclear Information System (INIS)

    Harp, Jason M.; Demkowicz, Paul A.; Winston, Philip L.; Sterbentz, James W.

    2014-01-01

    Highlights: • The burnup of irradiated AGR-1 TRISO fuel was analyzed using gamma spectrometry. • The burnup of irradiated AGR-1 TRISO fuel was also analyzed using mass spectrometry. • Agreement between experimental results and neutron physics simulations was excellent. - Abstract: AGR-1 was the first in a series of experiments designed to test US TRISO fuel under high temperature gas-cooled reactor irradiation conditions. This experiment was irradiated in the Advanced Test Reactor (ATR) at Idaho National Laboratory (INL) and is currently undergoing post-irradiation examination (PIE) at INL and Oak Ridge National Laboratory. One component of the AGR-1 PIE is the experimental evaluation of the burnup of the fuel by two separate techniques. Gamma spectrometry was used to non-destructively evaluate the burnup of all 72 of the TRISO fuel compacts that comprised the AGR-1 experiment. Two methods for evaluating burnup by gamma spectrometry were developed, one based on the Cs-137 activity and the other based on the ratio of Cs-134 and Cs-137 activities. Burnup values determined from both methods compared well with the values predicted from simulations. The highest measured burnup was 20.1% FIMA (fissions per initial heavy metal atom) for the direct method and 20.0% FIMA for the ratio method (compared to 19.56% FIMA from simulations). An advantage of the ratio method is that the burnup of the cylindrical fuel compacts can be determined in small (2.5 mm) axial increments and an axial burnup profile can be produced. Destructive chemical analysis by inductively coupled mass spectrometry (ICP-MS) was then performed on selected compacts that were representative of the expected range of fuel burnups in the experiment to compare with the burnup values determined by gamma spectrometry. The compacts analyzed by mass spectrometry had a burnup range of 19.3% FIMA to 10.7% FIMA. The mass spectrometry evaluation of burnup for the four compacts agreed well with the gamma

  10. Multi-element analyses of Vietnamese environmental samples for radiation protection

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  11. Improved sample preparation method for environmental plutonium analysis by ICP-SFMS and alpha-spectrometry

    International Nuclear Information System (INIS)

    Varga, Z.; Stefanka, Z.; Suranyi, G.; Vajda, N.

    2007-01-01

    A rapid and simple sample preparation method for plutonium determination in environmental samples by inductively coupled plasma sector field mass spectrometry (ICP-SFMS) and alpha-spectrometry is described. The developed procedure involves a selective CaF 2 co-precipitation for preconcentration followed by extraction chromatographic separation. The proposed method effectively eliminates the possible interferences in mass spectrometric analysis and also removes interfering radionuclides that may disturb alpha-spectrometric measurement. For 239 Pu, 240 Pu and 241 Pu limits of detection of 9.0 fg x g -1 (0.021 mBq), 1.7 fg x g -1 (0.014 mBq) and 3.1 fg x g -1 (11.9 mBq) were achieved by ICP-SFMS, respectively, and 0.02 mBq by alpha-spectrometry. Results of certified reference materials agreed well with the recommended values. (author)

  12. The use of secondary ion mass spectrometry for uranium analysis in bioassays

    International Nuclear Information System (INIS)

    Amaral, Ademir de Jesus

    1997-01-01

    Today many researches are performed to use mass spectrometry as complementary methods to the alpha spectrometry. In this study performance of the secondary ion mass spectrometry (SIMS) are evaluated for traces of uranium analysis in biological tissues and more particularly in urine. A special attention is done for the samples preparation, using thin polymers. the SIMS method feasibility is presented. The second part of the thesis deals with the use of a tracer to quantify the urinary uranium, the 233 U. The isotopic ratio are obtained with a detection limit of 10 -6 Bq in 238 U per urine litre. Other biological samples are studied to illustrate the adaptability of the SIMS method to internal dosimetry. (A.L.B.)

  13. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-04-08

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

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

    Science.gov (United States)

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

    2011-04-08

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

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

  17. Direct olive oil analysis by mass spectrometry: A comparison of different ambient ionization methods.

    Science.gov (United States)

    Lara-Ortega, Felipe J; Beneito-Cambra, Miriam; Robles-Molina, José; García-Reyes, Juan F; Gilbert-López, Bienvenida; Molina-Díaz, Antonio

    2018-04-01

    Analytical methods based on ambient ionization mass spectrometry (AIMS) combine the classic outstanding performance of mass spectrometry in terms of sensitivity and selectivity along with convenient features related to the lack of sample workup required. In this work, the performance of different mass spectrometry-based methods has been assessed for the direct analyses of virgin olive oil for quality purposes. Two sets of experiments have been setup: (1) direct analysis of untreated olive oil using AIMS methods such as Low-Temperature Plasma Mass Spectrometry (LTP-MS) or paper spray mass spectrometry (PS-MS); or alternatively (2) the use of atmospheric pressure ionization (API) mass spectrometry by direct infusion of a diluted sample through either atmospheric pressure chemical ionization (APCI) or electrospray (ESI) ionization sources. The second strategy involved a minimum sample work-up consisting of a simple olive oil dilution (from 1:10 to 1:1000) with appropriate solvents, which originated critical carry over effects in ESI, making unreliable its use in routine; thus, ESI required the use of a liquid-liquid extraction to shift the measurement towards a specific part of the composition of the edible oil (i.e. polyphenol rich fraction or lipid/fatty acid profile). On the other hand, LTP-MS enabled direct undiluted mass analysis of olive oil. The use of PS-MS provided additional advantages such as an extended ionization coverage/molecular weight range (compared to LTP-MS) and the possibility to increase the ionization efficiency towards nonpolar compounds such as squalene through the formation of Ag + adducts with carbon-carbon double bounds, an attractive feature to discriminate between oils with different degree of unsaturation. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Determination of wheat quality by mass spectrometry and multivariate data analysis

    DEFF Research Database (Denmark)

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

    2002-01-01

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

  19. Spectrochemical analysis of plutonium using direct current plasma emission spectrometry

    International Nuclear Information System (INIS)

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

    1983-01-01

    One year ago, LLNL was just completing the installation of a Direct Current Plasma (DCP) spectrometer for the analysis of Pu and Pu alloys. The installation was completed in December 1982 and has been utilized regularly for Pu analysis since then. This paper discusses the experience with the instrument and some data demonstrating its performance

  20. Attempt of absolute analysis with spark source mass spectrometry; Essai d'analyse absolue par spectrometrie de masse a etincelles

    Energy Technology Data Exchange (ETDEWEB)

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

    1964-10-01

    By means of a graphical method developed in our laboratory, we have studied the linearity of the response of the MS-7 mass spectrometer for impurity determinations over a concentration range of 1 to 1000 ppm (parts per million of atoms). This method consist in transforming optical density measurements into 'true intensities', which are plotted on a logarithm-scale paper against the exposures. A moving transparent ruler graduated at the inverse scale of the exposures allows us to determine directly on the graph, the concentration of impurities in ppm. We have used this method for the determination of sensitivity coefficients in standard samples such as Al, Fe, Cu, Ni, Zr, and non conducting powders like SiO{sub 2} and Al{sub 2}O{sub 3}. This study shows that, for the samples studied, the sensitivity coefficients are practically independent of the matrix and the concentration. Moreover the results show the possibility of obtaining an absolute analysis by spark source mass spectrometry. (author) [French] Au moyen d'une methode graphique developpee ou laboratoire, nous avons etudie la linearite des determinations d'impuretes au spectrometre de masse, type MS-7, dans un domaine de concentration allont de 1 a 1000 ppm. Cette methode consiste en la transformation des mesures de densite optique en 'intensite vraie'. Ces dernieres mesures sont portees sur un graphique logarithmique et une reglette transparente graduee a l'inverse de l'echelle des expositions nous permet de determiner directement la teneur des impuretes en ppm (partie par million d'atomes). Nous avons utilise cette methode pour la determination des coefficients de sensibilite dans des echantillons etalons tels que Al, Fe, Cu, Ni, Zr, et des poudres non conductrices genre SiO{sub 2}, Al{sub 2}O{sub 3}. Cette etude a montre que, pour les echantillons etudies, les coefficients de sensibilite sont pratiquement independants de la matrice et de la concentration. De plus, les resultats obtenus montrent la

  1. Estimation of 129I by low energy spectrometry and neutron activation analysis

    International Nuclear Information System (INIS)

    Ravi, P.M.; Iyer, M.R.; Sahasrabudhe, S.G.; Somasundaram, S.; Subramanian, M.S.

    1986-01-01

    Methods have been developed for the estimation of 129 I by direct passive counting and by neutron activation analysis. The direct counting method using low energy photon spectrometry has been standardised for liquid samples. Interference from different induced radionuclides in the activation method was studied. Limits of detection of 129 I by direct counting method and neutron activation analysis work out to be 0.4 Bq and 1mBq respectively. (author). 6 refs

  2. High precision analysis of trace lithium isotope by thermal ionization mass spectrometry

    International Nuclear Information System (INIS)

    Tang Lei; Liu Xuemei; Long Kaiming; Liu Zhao; Yang Tianli

    2010-01-01

    High precision analysis method of ng lithium by thermal ionization mass spectrometry is developed. By double-filament measurement,phosphine acid ion enhancer and sample pre-baking technique,the precision of trace lithium analysis is improved. For 100 ng lithium isotope standard sample, relative standard deviation is better than 0.086%; for 10 ng lithium isotope standard sample, relative standard deviation is better than 0.90%. (authors)

  3. 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

  4. An improved method for statistical analysis of raw accelerator mass spectrometry data

    International Nuclear Information System (INIS)

    Gutjahr, A.; Phillips, F.; Kubik, P.W.; Elmore, D.

    1987-01-01

    Hierarchical statistical analysis is an appropriate method for statistical treatment of raw accelerator mass spectrometry (AMS) data. Using Monte Carlo simulations we show that this method yields more accurate estimates of isotope ratios and analytical uncertainty than the generally used propagation of errors approach. The hierarchical analysis is also useful in design of experiments because it can be used to identify sources of variability. 8 refs., 2 figs

  5. Modelling of the acoustic field of a multi-element HIFU array scattered by human ribs

    Science.gov (United States)

    Gélat, Pierre; ter Haar, Gail; Saffari, Nader

    2011-09-01

    The efficacy of high-intensity focused ultrasound (HIFU) for the treatment of a range of different cancers, including those of the liver, prostate and breast, has been demonstrated. As a non-invasive focused therapy, HIFU offers considerable advantages over techniques such as chemotherapy and surgical resection in terms of reduced risk of harmful side effects. Despite this, there are a number of significant challenges which currently hinder its widespread clinical application. One of these challenges is the need to transmit sufficient energy through the rib cage to induce tissue necrosis in the required volume whilst minimizing the formation of side lobes. Multi-element random-phased arrays are currently showing great promise in overcoming the limitations of single-element transducers. Nevertheless, successful treatment of a patient with liver tumours requires a thorough understanding of the way in which the ultrasonic pressure field from a HIFU array is scattered by the rib cage. In order to address this, a boundary element approach based on a generalized minimal residual (GMRES) implementation of the Burton-Miller formulation was used in conjunction with phase conjugation techniques to focus the field of a 256-element random HIFU array behind human ribs at locations requiring intercostal and transcostal treatment. Simulations were carried out on a 3D mesh of quadratic pressure patches generated using CT scan anatomical data for adult ribs 9-12 on the right side. The methodology was validated on spherical and cylindrical scatterers. Field calculations were also carried out for idealized ribs, consisting of arrays of strip-like scatterers, demonstrating effects of splitting at the focus. This method has the advantage of fully accounting for the effect of scattering and diffraction in 3D under continuous wave excitation.

  6. Dose determination algorithms for a nearly tissue equivalent multi-element thermoluminescent dosimeter

    International Nuclear Information System (INIS)

    Moscovitch, M.; Chamberlain, J.; Velbeck, K.J.

    1988-01-01

    In a continuing effort to develop dosimetric systems that will enable reliable interpretation of dosimeter readings in terms of the absorbed dose or dose-equivalent, a new multi-element TL dosimeter assembly for Beta and Gamma dose monitoring has been designed. The radiation-sensitive volumes are four LiF-TLD elements, each covered by its own unique filter. For media-matching, care has been taken to employ nearly tissue equivalent filters of thicknesses of 1000 mg/cm 2 and 300 mg/cm 2 for deep dose and dose to the lens-of-the-eye measurements respectively. Only one metal filter (Cu) is employed to provide low energy photon discrimination. A Thin TL element (0.09 mm thick) is located behind an open window designed to improve the energy under-response to low energy beta rays and to provide closer estimate of the shallow dose equivalent. The deep and shallow dose equivalents are derived from the correlation of the response of the various TL elements to the above quantities through computations based on previously defined relationships obtained from experimental results. The theoretical formalization for the dose calculation algorithms is described in detail, and provides a useful methodology which can be applied to different tissue-equivalent dosimeter assemblies. Experimental data has been obtained by performing irradiation according to the specifications established by DOELAP, using 27 types of pure and mixed radiation fields including Cs-137 gamma rays, low energy photons down to 20 keV, Sr/Y-90, Uranium, and Tl-204 beta particles

  7. Modelling of the acoustic field of a multi-element HIFU array scattered by human ribs

    Energy Technology Data Exchange (ETDEWEB)

    Gelat, Pierre [National Physical Laboratory, Hampton Road, Teddington TW11 0LW (United Kingdom); Ter Haar, Gail [Therapeutic Ultrasound Group, Physics Department, Institute of Cancer Research, Sutton SM2 5NG (United Kingdom); Saffari, Nader, E-mail: Pierre.Gelat@npl.co.uk [Department of Mechanical Engineering, University College London, Torrington Place, London WC1E 7JE (United Kingdom)

    2011-09-07

    The efficacy of high-intensity focused ultrasound (HIFU) for the treatment of a range of different cancers, including those of the liver, prostate and breast, has been demonstrated. As a non-invasive focused therapy, HIFU offers considerable advantages over techniques such as chemotherapy and surgical resection in terms of reduced risk of harmful side effects. Despite this, there are a number of significant challenges which currently hinder its widespread clinical application. One of these challenges is the need to transmit sufficient energy through the rib cage to induce tissue necrosis in the required volume whilst minimizing the formation of side lobes. Multi-element random-phased arrays are currently showing great promise in overcoming the limitations of single-element transducers. Nevertheless, successful treatment of a patient with liver tumours requires a thorough understanding of the way in which the ultrasonic pressure field from a HIFU array is scattered by the rib cage. In order to address this, a boundary element approach based on a generalized minimal residual (GMRES) implementation of the Burton-Miller formulation was used in conjunction with phase conjugation techniques to focus the field of a 256-element random HIFU array behind human ribs at locations requiring intercostal and transcostal treatment. Simulations were carried out on a 3D mesh of quadratic pressure patches generated using CT scan anatomical data for adult ribs 9-12 on the right side. The methodology was validated on spherical and cylindrical scatterers. Field calculations were also carried out for idealized ribs, consisting of arrays of strip-like scatterers, demonstrating effects of splitting at the focus. This method has the advantage of fully accounting for the effect of scattering and diffraction in 3D under continuous wave excitation.

  8. Fundamentals of multi-element analysis with electron and beta radiation. 4

    International Nuclear Information System (INIS)

    Thuemmel, H.W.; Koerner, G.; Apel, K.

    1977-01-01

    Mass attenuation coefficients of liquid hydrocarbons and their oxygen, nitrogen and halogen derivates have been measured and compared with the values obtained according to the various calculation instructions (see pt.3). Using the most complete formula according to Schmidt the values obtained are systematically too low (up to 5 per cent), even with best parameter values. Only about half the values deviate by less than 3 per cent. Though the maximum deviations of 5 per cent are beyond the experimental errors (<= +-1 per cent) and the errors introduced by adaption of the general function to the mass attenuation coefficients of elementary absorbers (<= +-2.5 per cent), certain systematic deviation patterns (< 2.5 per cent) can be observed only for individual homologous series (alkanes, benzene derivatives), which may be caused by bonding effects or by remaining shortcomings of the model. The simple formula μsub(Σ) = Σpsub(i)μsub(i) provides effective mass attenuation coefficients, the error of which is up to 10 per cent. (author)

  9. Fundamentals of multi-element analysis with electron and beta radiation. 3

    International Nuclear Information System (INIS)

    Thuemmel, H.W.

    1977-01-01

    Mass attenuation coefficients obtained from calculations with the empirical formula μsub(Σ) = Σ psub(i).μsub(i) have been compared with the theoretical Schmidt formula (1906), in which the effective mass attenuation coefficient μsub(th) of a mixture of substances is the product of a true effective mass attenuation coefficient μ 0 and an effective by-pass coefficient U. Numerical results obtained from many substances of strongly varying composition show that for mixtures of components with atomic numbers Zsub(i) differing not too much from each other (contents psub(i), mass attenuation coefficients μsub(i) μ(Zsub(i)) μsub(Σ) is an approximation of μsub(th). This limitation is the less important, the less the curvature of the dependence of the mass attenuation coefficients of all elements on the atomic number (author)

  10. Analysis of writing inks on paper using direct analysis in real time mass spectrometry.

    Science.gov (United States)

    Jones, Roger W; McClelland, John F

    2013-09-10

    Ink analysis is central to questioned document examination. We applied direct analysis in real time mass spectrometry (DART MS) to ballpoint, gel, and fluid writing ink analysis. DART MS acquires the mass spectrum of an ink while it is still on a document without altering the appearance of the document. Spectra were acquired from ink on a variety of papers, and the spectrum of the blank paper could be subtracted out to produce a cleanly isolated ink spectrum in most cases. Only certain heavy or heavily processed papers interfered. The time since an ink is written on paper has a large effect on its spectrum. DART spectra change radically during the first few months after an ink is written as the more volatile components evaporate, but the spectra stabilize after that. A library-search study involving 166 well-aged inks assessed the ability to identify inks from their DART spectra. The aggregate success rate was 92%. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

  11. Differential Mobility Spectrometry for Improved Selectivity in Hydrophilic Interaction Liquid Chromatography-Tandem Mass Spectrometry Analysis of Paralytic Shellfish Toxins

    Science.gov (United States)

    Beach, Daniel G.

    2017-08-01

    Paralytic shellfish toxins (PSTs) are neurotoxins produced by dinoflagellates and cyanobacteria that cause paralytic shellfish poisoning in humans. PST quantitation by LC-MS is challenging because of their high polarity, lability as gas-phase ions, and large number of potentially interfering analogues. Differential mobility spectrometry (DMS) has the potential to improve the performance of LC-MS methods for PSTs in terms of selectivity and limits of detection. This work describes a comprehensive investigation of the separation of 16 regulated PSTs by DMS and the development of highly selective LC-DMS-MS methods for PST quantitation. The effects of all DMS parameters on the separation of PSTs from one another were first investigated in detail. The labile nature of 11α-gonyautoxin epimers gave unique insight into fragmentation of labile analytes before, during, and after the DMS analyzer. Two sets of DMS parameters were identified that either optimized the resolution of PSTs from one another or transmitted them at a limited number of compensation voltage (CV) values corresponding to structural subclasses. These were used to develop multidimensional LC-DMS-MS/MS methods using existing HILIC-MS/MS parameters. In both cases, improved selectivity was observed when using DMS, and the quantitative capabilities of a rapid UPLC-DMS-MS/MS method were evaluated. Limits of detection of the developed method were similar to those without DMS, and differences were highly analyte-dependant. Analysis of shellfish matrix reference materials showed good agreement with established methods. The developed methods will be useful in cases where specific matrix interferences are encountered in the LC-MS/MS analysis of PSTs in complex biological samples.

  12. An optimum analysis sequence for environmental gamma-ray spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    De la Torre, F.; Rios M, C.; Ruvalcaba A, M. G.; Mireles G, F.; Saucedo A, S.; Davila R, I.; Pinedo, J. L., E-mail: fta777@hotmail.co [Universidad Autonoma de Zacatecas, Centro Regional de Estudis Nucleares, Calle Cipres No. 10, Fracc. La Penuela, 98068 Zacatecas (Mexico)

    2010-10-15

    This work aims to obtain an optimum analysis sequence for environmental gamma-ray spectroscopy by means of Genie 2000 (Canberra). Twenty different analysis sequences were customized using different peak area percentages and different algorithms for: 1) peak finding, and 2) peak area determination, and with or without the use of a library -based on evaluated nuclear data- of common gamma-ray emitters in environmental samples. The use of an optimum analysis sequence with certified nuclear information avoids the problems originated by the significant variations in out-of-date nuclear parameters of commercial software libraries. Interference-free gamma ray energies with absolute emission probabilities greater than 3.75% were included in the customized library. The gamma-ray spectroscopy system (based on a Ge Re-3522 Canberra detector) was calibrated both in energy and shape by means of the IAEA-2002 reference spectra for software intercomparison. To test the performance of the analysis sequences, the IAEA-2002 reference spectrum was used. The z-score and the reduced {chi}{sup 2} criteria were used to determine the optimum analysis sequence. The results show an appreciable variation in the peak area determinations and their corresponding uncertainties. Particularly, the combination of second derivative peak locate with simple peak area integration algorithms provides the greater accuracy. Lower accuracy comes from the combination of library directed peak locate algorithm and Genie's Gamma-M peak area determination. (Author)

  13. An optimum analysis sequence for environmental gamma-ray spectrometry

    International Nuclear Information System (INIS)

    De la Torre, F.; Rios M, C.; Ruvalcaba A, M. G.; Mireles G, F.; Saucedo A, S.; Davila R, I.; Pinedo, J. L.

    2010-10-01

    This work aims to obtain an optimum analysis sequence for environmental gamma-ray spectroscopy by means of Genie 2000 (Canberra). Twenty different analysis sequences were customized using different peak area percentages and different algorithms for: 1) peak finding, and 2) peak area determination, and with or without the use of a library -based on evaluated nuclear data- of common gamma-ray emitters in environmental samples. The use of an optimum analysis sequence with certified nuclear information avoids the problems originated by the significant variations in out-of-date nuclear parameters of commercial software libraries. Interference-free gamma ray energies with absolute emission probabilities greater than 3.75% were included in the customized library. The gamma-ray spectroscopy system (based on a Ge Re-3522 Canberra detector) was calibrated both in energy and shape by means of the IAEA-2002 reference spectra for software intercomparison. To test the performance of the analysis sequences, the IAEA-2002 reference spectrum was used. The z-score and the reduced χ 2 criteria were used to determine the optimum analysis sequence. The results show an appreciable variation in the peak area determinations and their corresponding uncertainties. Particularly, the combination of second derivative peak locate with simple peak area integration algorithms provides the greater accuracy. Lower accuracy comes from the combination of library directed peak locate algorithm and Genie's Gamma-M peak area determination. (Author)

  14. Energy Dispersive Spectrometry and Quantitative Analysis Short Course. Introduction to X-ray Energy Dispersive Spectrometry and Quantitative Analysis

    Science.gov (United States)

    Carpenter, Paul; Curreri, Peter A. (Technical Monitor)

    2002-01-01

    This course will cover practical applications of the energy-dispersive spectrometer (EDS) to x-ray microanalysis. Topics covered will include detector technology, advances in pulse processing, resolution and performance monitoring, detector modeling, peak deconvolution and fitting, qualitative and quantitative analysis, compositional mapping, and standards. An emphasis will be placed on use of the EDS for quantitative analysis, with discussion of typical problems encountered in the analysis of a wide range of materials and sample geometries.

  15. Isotope analysis of lithium by thermionic mass spectrometry

    International Nuclear Information System (INIS)

    Kakazu, M.H.; Sarkis, J.E.S.

    1991-04-01

    An analytical mass spectrometric method for the isotope analysis of lithium has been studied. The analysis were carried out by using a single focusing thermoionic mass spectrometer Varian Mat TH5 with 90 sup(0) magnetic sector field and 21.4 cm deflection radius, equipped with a dual Re-filament thermal ionization ion source. The effect of different lithium chemical forms, such as, carbonate, chloride, nitrate and sulfate upon the isotopic ratios sup(6)Li/ sup(7)Li has been studied. Isotopic fractionation of lithium was studied in terms of the time of analysis. The results obtained with lithium carbonate yielded a precision of ±0.1% and an accuracy of ± 0.6%, whereas with other chemical forms yielded precisions of ±0.5% and accuracies of ±2%. A fractionation correction factor, K=1.005, was obtained for different samples of lithium carbonate isotopic standard CBNM IRM 016, which has been considered constant. (author)

  16. Metabolome analysis - mass spectrometry and microbial primary metabolites

    DEFF Research Database (Denmark)

    Højer-Pedersen, Jesper Juul

    2008-01-01

    , and therefore sample preparation is critical for metabolome analysis. The three major steps in sample preparation for metabolite analysis are sampling, extraction and concentration. These three steps were evaluated for the yeast Saccharomyces cerevisiae with primary focus on analysis of a large number...... of metabolites by one method. The results highlighted that there were discrepancies between different methods. To increase the throughput of cultivation, S. cerevisiae was grown in microtitier plates (MTPs), and the growth was found to be comparable with cultivations in shake flasks. The carbon source was either...... a theoretical metabolome. This showed that in combination with the specificity of MS up to 84% of the metabolites can be identified in a high-accuracy ESI-spectrum. A total of 66 metabolites were systematically analyzed by positive and negative ESI-MS/MS with the aim of initiating a spectral library for ESI...

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  18. Computer programs for data reduction and interpretation in plutonium and uranium analysis by gamma ray spectrometry

    International Nuclear Information System (INIS)

    Singh, R.K.; Moorthy, A.D.; Babbar, R.K.; Udagatti, S.V.

    1989-01-01

    Non destructive gamma ray have been developed for analysis of isotopic abundances and concentrations of plutonium and uranium in the respective product solutions of a reprocessing plant. The method involves analysis of gamma rays emitted from the sample and uses a multichannel analyser system. Data reduction and interpretation of these techniques are tedious and time consuming. In order to make it possible to use them in routine analysis, computer programs have been developed in HP-BASIC language which can be used in HP-9845B desktop computer. A set of programs, for plutonium estimation by high resolution gamma ray spectrometry and for on-line measurement of uranium by gamma ray spectrometry are described in this report. (author) 4 refs., 3 tabs., 6 figs

  19. Direct Analysis of Samples of Various Origin and Composition Using Specific Types of Mass Spectrometry.

    Science.gov (United States)

    Byliński, Hubert; Gębicki, Jacek; Dymerski, Tomasz; Namieśnik, Jacek

    2017-07-04

    One of the major sources of error that occur during chemical analysis utilizing the more conventional and established analytical techniques is the possibility of losing part of the analytes during the sample preparation stage. Unfortunately, this sample preparation stage is required to improve analytical sensitivity and precision. Direct techniques have helped to shorten or even bypass the sample preparation stage; and in this review, we comment of some of the new direct techniques that are mass-spectrometry based. The study presents information about the measurement techniques using mass spectrometry, which allow direct sample analysis, without sample preparation or limiting some pre-concentration steps. MALDI - MS, PTR - MS, SIFT - MS, DESI - MS techniques are discussed. These solutions have numerous applications in different fields of human activity due to their interesting properties. The advantages and disadvantages of these techniques are presented. The trends in development of direct analysis using the aforementioned techniques are also presented.

  20. A micro-fluidic sub-microliter sample introduction system for direct analysis of Chinese rice wine by inductively coupled plasma mass spectrometry using external aqueous calibration

    Science.gov (United States)

    Cheng, Heyong; Liu, Jinhua; Xu, Zigang; Yin, Xuefeng

    2012-07-01

    A microfluidic sub-microliter sample introducing system was developed for direct analysis of Chinese rice wine by inductively coupled plasma mass spectrometry (ICP-MS). It consisted of a microfluidic chip integrating variable-volume sampling channels (0.1-0.8 μL), an eight-way multi-functional valve used in flow injection analysis (FIA), a syringe pump and a peristaltic pump of the Ar ICP-MS instrument. Three solutions, i.e., 15, 40 and 100 g L- 1 glucose in 20% ethanol were used to simulate Chinese rice wine of the dry type, the semidry type and the semisweet type, each. The effects of their volume introduced into ICP-MS on the plasma stability and ICP-MS intensities were studied. The experimental results showed that neither alteration of plasma stability nor carbon deposition was observed when the sampling volume of 20% ethanol containing 100 g L- 1 glucose was downscaled to 0.8 μL. Further reducing the sampling volume to 0.4 μL, no significant difference between the intensities of multi-element standard prepared in three simulated Chinese rice wine matrices and those in aqueous solution was observed. It indicated no negative effect of Chinese rice wine matrix on the ICP-MS intensities. A sampling volume of 0.4 μL was considered to be a good compromise between sensitivity and matrix effect. The flow rate of the carrier was chosen as 20 μL min- 1 for obtaining peaks with the highest peak height within the shortest time. Based on these observations, a microflow injection (μFI) method for the direct determination of cadmium and lead in Chinese rice wine by ICP-MS using an external aqueous calibration was developed. The sample throughput was 45 h- 1 with the detection limit of 19.8 and 10.4 ng L- 1 for Cd and Pb, respectively. The contents of Cd and Pb in 10 Chinese rice wine samples were measured. The results agreed well with those determined by ICP-MS with the conventional sampling system after microwave assisted digestion. The recoveries of three Chinese

  1. The application of atomic absorption spectrometry to chemical analysis

    International Nuclear Information System (INIS)

    Walsh, A.

    1980-01-01

    YhThe history of the development of atomic absorption methods of elemental analysis is outlined. The theoretical basis of atomic absorption methods is discussed and the principle of modern methods of atomic absorption measurements is described. The advantages, scope and limations of these methods are discussed. Related methods based on the measurement of atomic fluorescence are also described

  2. Fundamentals of Biomolecule Analysis by Electrospray Ionization Mass Spectrometry

    Science.gov (United States)

    Weinecke, Andrea; Ryzhov, Victor

    2005-01-01

    Electrospray ionization (ESI) is a soft ionization technique that allows transfer of fragile biomolecules directly from solution into the gas phase. An instrumental analysis laboratory experiment is designed that would introduce the students to the ESI technique, major parameters of the ion trap mass spectrometers and some caveats in…

  3. Isotopic analysis of plutonium by computer controlled mass spectrometry

    International Nuclear Information System (INIS)

    1974-01-01

    Isotopic analysis of plutonium chemically purified by ion exchange is achieved using a thermal ionization mass spectrometer. Data acquisition from and control of the instrument is done automatically with a dedicated system computer in real time with subsequent automatic data reduction and reporting. Separation of isotopes is achieved by varying the ion accelerating high voltage with accurate computer control

  4. Evaluation of three gas chromatography and two direct mass spectrometry techniques for aroma analysis of dried red bell peppers

    NARCIS (Netherlands)

    Ruth, van S.M.; Boscaini, E.; Mayr, D.; Pugh, J.; Posthumus, M.A.

    2003-01-01

    Three gas chromatography methods and two direct mass spectrometry techniques were compared for the analysis of the aroma of rehydrated diced red bell peppers. Gas chromatography methods included systems with olfactometry detection (GC-O), flame ionisation detection (GC-FID) and mass spectrometry

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

    Science.gov (United States)

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

    2017-01-01

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

  6. Analysis of Protein O-GlcNAcylation by Mass Spectrometry

    OpenAIRE

    Ma, Junfeng; Hart, Gerald W.

    2017-01-01

    O-linked β-D-N-acetylglucosamine (O-GlcNAc) addition (O-GlcNAcylation), a post-translational modification of serine/threonine residues of proteins, is involved in diverse cellular metabolic and signaling pathways. Aberrant O-GlcNAcylation underlies the initiation and progression of multiple chronic diseases including diabetes, cancer, and neurodegenerative diseases. Numerous methods have been developed for the analysis of protein O-GlcNAcylation, but instead of discussing the classical bioche...

  7. Application of neural networks to quantitative spectrometry analysis

    International Nuclear Information System (INIS)

    Pilato, V.; Tola, F.; Martinez, J.M.; Huver, M.

    1999-01-01

    Accurate quantitative analysis of complex spectra (fission and activation products), relies upon experts' knowledge. In some cases several hours, even days of tedious calculations are needed. This is because current software is unable to solve deconvolution problems when several rays overlap. We have shown that such analysis can be correctly handled by a neural network, and the procedure can be automated with minimum laboratory measurements for networks training, as long as all the elements of the analysed solution figure in the training set and provided that adequate scaling of input data is performed. Once the network has been trained, analysis is carried out in a few seconds. On submitting to a test between several well-known laboratories, where unknown quantities of 57 Co, 58 Co, 85 Sr, 88 Y, 131 I, 139 Ce, 141 Ce present in a sample had to be determined, the results yielded by our network classed it amongst the best. The method is described, including experimental device and measures, training set designing, relevant input parameters definition, input data scaling and networks training. Main results are presented together with a statistical model allowing networks error prediction

  8. Studies of the source complex behaviour and of the ultrasound radiation of contact flexible multi-element transducers; Etudes du comportement complexe de source et du rayonnement ultrasonore des traducteurs multi-elements flexibles au contact

    Energy Technology Data Exchange (ETDEWEB)

    Amory, V

    2007-12-15

    This work deals with the ultrasonic nondestructive testing of parts with complex geometries using soft multi-element sensors. The different types of contact control configurations are presented first. Then, the difficulties encountered with conventional contact transducers are explained and the multi-element piezoelectric transducers technology, developed to meet these difficulties, is presented. The second chapter presents the results of finite-element calculations showing the complexity of a transducer in a condition of testing utilization. In a same configuration, the radiated far field calculated by finite-elements is compared to the measurement in order to validate the way the source behaviour is calculated. However, despite the efficiency of the finite-elements simulation, this tool is numerically too costly and cannot be used to optimize a full multi-element transducer. Therefore, a realistic source model is built and implemented in a radiation code based on high-frequency asymptotic approximations where only L and T volume waves are calculated. The incapacity of this model to reproduce the behaviour of T waves in some directions of propagation has led to give a particular attention to the fore-waves, neglected in the radiation calculation. Chapter 3 treats of the building of an exact radiation model taking into consideration the fore-waves contribution emitted by a contact transducer exerting a random space-time distribution constraint at the surface of the considered medium. A radiation model, based on the calculation of exact Green functions of the Lamb problem is proposed. The exact model is particularly interesting in the case of sensor geometries with a long length with respect to other dimensions (2D case). Field calculation results are shown for an element of the matrix network (3D case) and for a linear element (2D case). A study of different existing approached models is carried out as well. The last chapter presents some results of the field

  9. Intercomparison of γ-spectrometry analysis of radionuclides between China and Japan in 2012–2013

    International Nuclear Information System (INIS)

    Zhou, Qiang; Wang, Xiaoqiang; Tuo, Fei; Han, Yanqing; Ikeuchi, Yoshihiro; Yang, Jia; Xu, Cuihua; Zhang, Jing; Li, Wenhong; Zhang, Qing; Su, Xu

    2015-01-01

    An intercomparison of γ-spectrometry measurement and analysis was organized by the Japan Chemical Analysis Center (JCAC), the National Institute for Radiological Protection, Chinese Center for Disease Control and Prevention (NIRP, China CDC), and the Radiation Monitoring Technical Center of Ministry of Environmental Protection, Chinese (RMTC). The main objective of this study was to assess the γ-spectrometry measurement and analysis technology. The JCAC completed the collection and preparation of soil and powdered rice samples. Three laboratories compared the measurement of seven radionuclides that included two samples of 214 Pb, 214 Bi, 208 Tl, 228 Ac, 40 K, 137 Cs, and 134 Cs with γ-spectrometry. During the studies conducted at the laboratory, the calculated value E n was found to be the total uncertainty data of the reported activity. Except 134 Cs in powdered rice sample, the calculated E n between each of the two laboratories was <1. The measurement results are acceptable except 134 Cs; therefore, measurement results in the three laboratories were consistent within a certain range except in the case of 134 Cs. Although there is a need to improve the accuracy of measurements and analysis of 134 Cs, an intercomparison was conducted of the tested levels on radionuclide analyzed in the three laboratories. - Highlights: • An intercomparison of γ-spectrometry measurement and analysis was organized. • Three laboratories compared the measurement of seven radionuclides. • Results for 40 K, 208 Tl, 214 Bi, 214 Pb, 228 Ac, and 137 Cs were well matched between two participants. • The results in the powder of the rice sample belonging to 134 Cs were the only ones assigned “not acceptable”.

  10. freeQuant: A Mass Spectrometry Label-Free Quantification Software Tool for Complex Proteome Analysis.

    Science.gov (United States)

    Deng, Ning; Li, Zhenye; Pan, Chao; Duan, Huilong

    2015-01-01

    Study of complex proteome brings forward higher request for the quantification method using mass spectrometry technology. In this paper, we present a mass spectrometry label-free quantification tool for complex proteomes, called freeQuant, which integrated quantification with functional analysis effectively. freeQuant consists of two well-integrated modules: label-free quantification and functional analysis with biomedical knowledge. freeQuant supports label-free quantitative analysis which makes full use of tandem mass spectrometry (MS/MS) spectral count, protein sequence length, shared peptides, and ion intensity. It adopts spectral count for quantitative analysis and builds a new method for shared peptides to accurately evaluate abundance of isoforms. For proteins with low abundance, MS/MS total ion count coupled with spectral count is included to ensure accurate protein quantification. Furthermore, freeQuant supports the large-scale functional annotations for complex proteomes. Mitochondrial proteomes from the mouse heart, the mouse liver, and the human heart were used to evaluate the usability and performance of freeQuant. The evaluation showed that the quantitative algorithms implemented in freeQuant can improve accuracy of quantification with better dynamic range.

  11. Liquid separation techniques coupled with mass spectrometry for chiral analysis of pharmaceuticals compounds and their metabolites in biological fluids.

    Science.gov (United States)

    Erny, G L; Cifuentes, A

    2006-02-24

    Determination of the chiral composition of drugs is nowadays a key step in order to determine purity, activity, bioavailability, biodegradation, etc., of pharmaceuticals. In this article, works published for the last 5 years on the analysis of chiral drugs by liquid separation techniques coupled with mass spectrometry are reviewed. Namely, chiral analysis of pharmaceuticals including, e.g., antiinflammatories, antihypertensives, relaxants, etc., by liquid chromatography-mass spectrometry and capillary electrophoresis-mass spectrometry are included. The importance and interest of the analysis of the enantiomers of the active compound and its metabolites in different biological fluids (plasma, urine, cerebrospinal fluid, etc.) are also discussed.

  12. Application of resonance ionization mass spectrometry for trace analysis and in fundamental research

    International Nuclear Information System (INIS)

    Passler, G.

    1997-01-01

    Resonance ionization mass spectrometry (RIMS) has been used for ultra-trace analysis on long-lived radioisotopes like Pu, Tc and 89,90 Sr in various environmental samples. The experimental approaches cover pulsed laser spectroscopy on a thermal atomic beam and subsequent time-of-flight mass analysis, a pulsed laser ion source combined with conventional mass spectrometry, and collinear resonance ionization on a mass-separated fast atomic beam. The high sensitivity of RIMS also enables atomic spectroscopy on rare isotopes. For the first time experimental values for the ionization potential of actinides up to Cf have been determined. The paper reviews the dependency of the different experimental approaches on the analytical problem. copyright 1997 American Institute of Physics

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

    International Nuclear Information System (INIS)

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

    1994-01-01

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

  14. Ion mobility spectrometry focusing on speciation analysis of metals/metalloids bound to carbonic anhydrase.

    Science.gov (United States)

    Pessôa, Gustavo de Souza; Pilau, Eduardo Jorge; Gozzo, Fábio Cesar; Arruda, Marco Aurélio Zezzi

    2013-09-01

    In the present work, traveling wave ion mobility spectrometry-mass spectrometry (TWIMS-MS) was applied to speciation analysis of metalloproteins. The influence of pH on complexation conditions between some metals and bovine carbonic anhydrase was evaluated from pH 6 to 9, as well as the time involved in their complexation (0-24 h). Employing TWIMS-MS, two conformational states of bovine carbonic anhydrase were observed with charge states of +12 and +11; these configurations being evaluated in terms of the folded state of the apo form and this protein (at charge state +11) being linked to barium, lead, copper, and zinc in their divalent forms. Metalloprotein speciation analysis was carried out for copper (Cu(+) and Cu(2+)), lead (Pb(2+) and Pb(4+)), and selenium (Se(4+) and Se(6+)) species complexed with bovine carbonic anhydrase. Mobilities of all complexed species were compared, also considering the apo form of this protein.

  15. Liquid chromatography mass spectrometry for analysis of microbial metabolites

    DEFF Research Database (Denmark)

    Klitgaard, Andreas

    to human health. Because of this, methods for detection and analysis of these compounds are vital. Estimates suggest that there are around 1.5 million different fungal species on Earth, dwarfing the number of plants estimated to 300,000, meaning that there potentially are many more interesting compounds...... is of large commercial interest for production of the bioactive compounds of the future. One part of my study focused on identification and elucidation of the biosynthesis of a nonribosomal peptide (NRP) nidulanin A from Aspergillus nidulans. Although the study was successful several analogs were......Filamentous fungi serve a very important role in Nature where they break down organic matter, releasing nutrients that can be used by other organisms. Fungi and other microorganisms also produce a wide array of bioactive compounds, the secondary metabolites( SMs), used for such diverse roles...

  16. A Multi-Element Approach to Location Inference of Twitter: A Case for Emergency Response

    Directory of Open Access Journals (Sweden)

    Farhad Laylavi

    2016-04-01

    Full Text Available Since its inception, Twitter has played a major role in real-world events—especially in the aftermath of disasters and catastrophic incidents, and has been increasingly becoming the first point of contact for users wishing to provide or seek information about such situations. The use of Twitter in emergency response and disaster management opens up avenues of research concerning different aspects of Twitter data quality, usefulness and credibility. A real challenge that has attracted substantial attention in the Twitter research community exists in the location inference of twitter data. Considering that less than 2% of tweets are geotagged, finding location inference methods that can go beyond the geotagging capability is undoubtedly the priority research area. This is especially true in terms of emergency response, where spatial aspects of information play an important role. This paper introduces a multi-elemental location inference method that puts the geotagging aside and tries to predict the location of tweets by exploiting the other inherently attached data elements. In this regard, textual content, users’ profile location and place labelling, as the main location-related elements, are taken into account. Location-name classes in three granularity levels are defined and employed to look up the location references from the location-associated elements. The inferred location of the finest granular level is assigned to a tweet, based on a novel location assignment rule. The location assigned by the location inference process is considered to be the inferred location of a tweet, and is compared with the geotagged coordinates as the ground truth of the study. The results show that this method is able to successfully infer the location of 87% of the tweets at the average distance error of 12.2 km and the median distance error of 4.5 km, which is a significant improvement compared with that of the current methods that can predict the location

  17. Rayleigh-based, multi-element coral thermometry: A biomineralization approach to developing climate proxies

    Science.gov (United States)

    Gaetani, G.A.; Cohen, A.L.; Wang, Z.; Crusius, John

    2011-01-01

    This study presents a new approach to coral thermometry that deconvolves the influence of water temperature on skeleton composition from that of “vital effects”, and has the potential to provide estimates of growth temperatures that are accurate to within a few tenths of a degree Celsius from both tropical and cold-water corals. Our results provide support for a physico-chemical model of coral biomineralization, and imply that Mg2+ substitutes directly for Ca2+ in biogenic aragonite. Recent studies have identified Rayleigh fractionation as an important influence on the elemental composition of coral skeletons. Daily, seasonal and interannual variations in the amount of aragonite precipitated by corals from each “batch” of calcifying fluid can explain why the temperature dependencies of elemental ratios in coral skeleton differ from those of abiogenic aragonites, and are highly variable among individual corals. On the basis of this new insight into the origin of “vital effects” in coral skeleton, we developed a Rayleigh-based, multi-element approach to coral thermometry. Temperature is resolved from the Rayleigh fractionation signal by combining information from multiple element ratios (e.g., Mg/Ca, Sr/Ca, Ba/Ca) to produce a mathematically over-constrained system of Rayleigh equations. Unlike conventional coral thermometers, this approach does not rely on an initial calibration of coral skeletal composition to an instrumental temperature record. Rather, considering coral skeletogenesis as a biologically mediated, physico-chemical process provides a means to extract temperature information from the skeleton composition using the Rayleigh equation and a set of experimentally determined partition coefficients. Because this approach is based on a quantitative understanding of the mechanism that produces the “vital effect” it should be possible to apply it both across scleractinian species and to corals growing in vastly different environments. Where

  18. Analysis of phosphatidylcholine oxidation products in human plasma using quadrupole time-of flight mass spectrometry

    OpenAIRE

    Adachi, Junko; Asano, Migiwa; Yoshioka, Naoki; Nushida, Hideyuki; Ueno, Yasuhiro

    2006-01-01

    We report here an application of the previous method for the analysis ofphosphatidylcholine (PC) and lysophosphatidylcholine (lysoPC) oxidation products inhuman plasma using quadrupole time of flight (Q-TOF) mass spectrometry withelectrospray ionization. We separated these products using an HPLC C8 column witha gradient of methanol and 10 mM aqueous ammonium acetate. Monohydroperoxides,epoxyhydroxy derivatives, oxo derivatives, and trihydroxides of palmitoyl-linoleoyl(C16:0/C18:2) PC and stea...

  19. An isotopic analysis process with optical emission spectrometry on a laser-produced plasma

    International Nuclear Information System (INIS)

    Mauchien, P.; Pietsch, W.; Petit, A.; Briand, A.

    1994-01-01

    The sample that is to be analyzed is irradiated with a laser beam to produce a plasma at the sample surface; the spectrum of the light emitted by the plasma is analyzed and the isotope composition of the sample is derived from the spectrometry. The process is preferentially applied to uranium and plutonium; it is rapid, simpler and cheaper than previous methods, and may be applied to 'in-situ' isotopic analysis in nuclear industry. 2 figs

  20. Ambient mass spectrometry: From the planar to the non-planar surface analysis

    Czech Academy of Sciences Publication Activity Database

    Rejšek, Jan; Vrkoslav, Vladimír; Cvačka, Josef

    2017-01-01

    Roč. 15, č. 1 (2017), s. 31 ISSN 2336-7202. [Mezioborové setkání mladých biologů, biochemiků a chemiků /17./. 30.05.2017-01.06.2017, Milovy] Institutional support: RVO:61388963 Keywords : ambient mass spectrometry * thin layer chromatography * non-planar surface analysis Subject RIV: CB - Analytical Chemistry, Separation

  1. Studies of the source complex behaviour and of the ultrasound radiation of contact flexible multi-element transducers

    International Nuclear Information System (INIS)

    Amory, V.

    2007-12-01

    This work deals with the ultrasonic nondestructive testing of parts with complex geometries using soft multi-element sensors. The different types of contact control configurations are presented first. Then, the difficulties encountered with conventional contact transducers are explained and the multi-element piezoelectric transducers technology, developed to meet these difficulties, is presented. The second chapter presents the results of finite-element calculations showing the complexity of a transducer in a condition of testing utilization. In a same configuration, the radiated far field calculated by finite-elements is compared to the measurement in order to validate the way the source behaviour is calculated. However, despite the efficiency of the finite-elements simulation, this tool is numerically too costly and cannot be used to optimize a full multi-element transducer. Therefore, a realistic source model is built and implemented in a radiation code based on high-frequency asymptotic approximations where only L and T volume waves are calculated. The incapacity of this model to reproduce the behaviour of T waves in some directions of propagation has led to give a particular attention to the fore-waves, neglected in the radiation calculation. Chapter 3 treats of the building of an exact radiation model taking into consideration the fore-waves contribution emitted by a contact transducer exerting a random space-time distribution constraint at the surface of the considered medium. A radiation model, based on the calculation of exact Green functions of the Lamb problem is proposed. The exact model is particularly interesting in the case of sensor geometries with a long length with respect to other dimensions (2D case). Field calculation results are shown for an element of the matrix network (3D case) and for a linear element (2D case). A study of different existing approached models is carried out as well. The last chapter presents some results of the field

  2. Analysis of magnetic compounds of Kosice meteorite using Moessbauer spectrometry

    International Nuclear Information System (INIS)

    Dekan, J.; Sitek, J.; Sedlackova, K.

    2013-01-01

    Meteorite fall was observed by the town Kosice in Slovakia in February 2010. The fall itself was imaged by three security video cameras from Hungary. Detailed bolide light curves were obtained through clouds by radiometers on seven cameras of the European Fireball Network. Records of sonic waves were found on six seismic and four infrasonic stations. chondrites in various works. Due to the high abundance of iron in the solar system and its chemical and physical properties, we can gain insight into the formation and evolution of planets through the study of iron compounds in the planetary bodies. These kinds of analyses can bring important knowledge about phases and compounds formed in extraterrestrial conditions, which have another features than their terrestrial analogues. The "5"7Fe Moessbauer spectroscopy is one of the most sensitive methods for such studies. In this work Moessbauer spectroscopy will be used for phase analysis of iron bearing compounds with the aim to identify magnetic fractions using magnetic separation. (authors)

  3. 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

  4. 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)

  5. Direct analysis in real time mass spectrometry for analysis of sexual assault evidence.

    Science.gov (United States)

    Musah, Rabi A; Cody, Robert B; Dane, A John; Vuong, Angela L; Shepard, Jason R E

    2012-05-15

    Sexual assault crimes are vastly underreported and suffer from alarmingly low prosecution and conviction rates. The key scientific method to aid in prosecution of such cases is forensic DNA analysis, where biological evidence such as semen collected using a rape test kit is used to determine a suspect's DNA profile. However, the growing awareness by criminals of the importance of DNA in the prosecution of sexual assaults has resulted in increased condom use by assailants as a means to avoid leaving behind their DNA. Thus, other types of trace evidence are important to help corroborate victims' accounts, exonerate the innocent, link suspects to the crime, or confirm penetration. Direct Analysis in Real Time Mass Spectrometry (DART-MS) was employed for the comprehensive characterization of non-DNA trace evidence associated with sexual assault. The ambient ionization method associated with DART-MS is extremely rapid and samples are processed instantaneously, without the need for extraction, sample preparation, or other means that might compromise forensic evidence for future analyses. In a single assay, we demonstrated the ability to identify lubricant formulations associated with sexual assault, such as the spermicide nonoxynol-9, compounds used in condom manufacture, and numerous other trace components as probative evidence. In addition, the method can also serve to identify compounds within trace biological residues, such as fatty acids commonly identified in latent fingerprints. Characterization of lubricant residues as probative evidence serves to establish a connection between the victim and the perpetrator, and the availability of these details may lead to higher rates of prosecution and conviction, as well as more severe penalties. The methodology described here opens the way for the adoption of a comprehensive, rapid, and sensitive analysis for use in crime labs, while providing knowledge that can inform and guide criminal justice policy and practice

  6. [Ultra-Fine Pressed Powder Pellet Sample Preparation XRF Determination of Multi-Elements and Carbon Dioxide in Carbonate].

    Science.gov (United States)

    Li, Xiao-li; An, Shu-qing; Xu, Tie-min; Liu, Yi-bo; Zhang, Li-juan; Zeng, Jiang-ping; Wang, Na

    2015-06-01

    The main analysis error of pressed powder pellet of carbonate comes from particle-size effect and mineral effect. So in the article in order to eliminate the particle-size effect, the ultrafine pressed powder pellet sample preparation is used to the determination of multi-elements and carbon-dioxide in carbonate. To prepare the ultrafine powder the FRITSCH planetary Micro Mill machine and tungsten carbide media is utilized. To conquer the conglomeration during the process of grinding, the wet grinding is preferred. The surface morphology of the pellet is more smooth and neat, the Compton scatter effect is reduced with the decrease in particle size. The intensity of the spectral line is varied with the change of the particle size, generally the intensity of the spectral line is increased with the decrease in the particle size. But when the particle size of more than one component of the material is decreased, the intensity of the spectral line may increase for S, Si, Mg, or decrease for Ca, Al, Ti, K, which depend on the respective mass absorption coefficient . The change of the composition of the phase with milling is also researched. The incident depth of respective element is given from theoretical calculation. When the sample is grounded to the particle size of less than the penetration depth of all the analyte, the effect of the particle size on the intensity of the spectral line is much reduced. In the experiment, when grounded the sample to less than 8 μm(d95), the particle-size effect is much eliminated, with the correction method of theoretical α coefficient and the empirical coefficient, 14 major, minor and trace element in the carbonate can be determined accurately. And the precision of the method is much improved with RSD element, the fluorescence yield is low and the interference is serious. With the manual multi-layer crystal PX4, coarse collimator, empirical correction, X-ray spectrometer can be used to determine the carbon dioxide in the carbonate

  7. Fast DNA analysis by laser mass spectrometry for human genome analysis

    International Nuclear Information System (INIS)

    Tang, K.; Taranenko, N. I.; Allman, S. L.; Chang, L. Y.; Chen, C. H.

    1995-01-01

    Fast DNA sequencing by laser mass spectrometry is possible if the following 3 criteria are met: (1) Size of DNA fragment should be greater than 300 nucleotides. (2) Enough sensitivity to detect DNA produce from polymerases chain reactins (PCR). (3) Higher resolution of mass spectr. So far, the firt 2 criteria are met: If the resolution can be significantly improve, fast DNA sequencing by laser mass spectrometry weil be a reality in the near feature

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

    International Nuclear Information System (INIS)

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

    2003-05-01

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

  9. PyQuant: A Versatile Framework for Analysis of Quantitative Mass Spectrometry Data.

    Science.gov (United States)

    Mitchell, Christopher J; Kim, Min-Sik; Na, Chan Hyun; Pandey, Akhilesh

    2016-08-01

    Quantitative mass spectrometry data necessitates an analytical pipeline that captures the accuracy and comprehensiveness of the experiments. Currently, data analysis is often coupled to specific software packages, which restricts the analysis to a given workflow and precludes a more thorough characterization of the data by other complementary tools. To address this, we have developed PyQuant, a cross-platform mass spectrometry data quantification application that is compatible with existing frameworks and can be used as a stand-alone quantification tool. PyQuant supports most types of quantitative mass spectrometry data including SILAC, NeuCode, (15)N, (13)C, or (18)O and chemical methods such as iTRAQ or TMT and provides the option of adding custom labeling strategies. In addition, PyQuant can perform specialized analyses such as quantifying isotopically labeled samples where the label has been metabolized into other amino acids and targeted quantification of selected ions independent of spectral assignment. PyQuant is capable of quantifying search results from popular proteomic frameworks such as MaxQuant, Proteome Discoverer, and the Trans-Proteomic Pipeline in addition to several standalone search engines. We have found that PyQuant routinely quantifies a greater proportion of spectral assignments, with increases ranging from 25-45% in this study. Finally, PyQuant is capable of complementing spectral assignments between replicates to quantify ions missed because of lack of MS/MS fragmentation or that were omitted because of issues such as spectra quality or false discovery rates. This results in an increase of biologically useful data available for interpretation. In summary, PyQuant is a flexible mass spectrometry data quantification platform that is capable of interfacing with a variety of existing formats and is highly customizable, which permits easy configuration for custom analysis. © 2016 by The American Society for Biochemistry and Molecular Biology

  10. Efficient isotope ratio analysis of uranium particles in swipe samples by total-reflection x-ray fluorescence spectrometry and secondary ion mass spectrometry

    International Nuclear Information System (INIS)

    Esaka, Fumitaka; Watanabe, Kazuo; Fukuyama, Hiroyasu; Onodera, Takashi; Esaka, Konomi T.; Magara, Masaaki; Sakurai, Satoshi; Usuda, Shigekazu

    2004-01-01

    A new particle recovery method and a sensitive screening method were developed for subsequent isotope ratio analysis of uranium particles in safeguards swipe samples. The particles in the swipe sample were recovered onto a carrier by means of vacuum suction-impact collection method. When grease coating was applied to the carrier, the recovery efficiency was improved to 48±9%, which is superior to that of conventionally-used ultrasoneration method. Prior to isotope ratio analysis with secondary ion mass spectrometry (SIMS), total reflection X-ray fluorescence spectrometry (TXRF) was applied to screen the sample for the presence of uranium particles. By the use of Si carriers in TXRF analysis, the detection limit of 22 pg was achieved for uranium. By combining these methods with SIMS, the isotope ratios of 235 U/ 238 U for individual uranium particles were efficiently determined. (author)

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

    Science.gov (United States)

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

    1990-01-01

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

  12. Pathology interface for the molecular analysis of tissue by mass spectrometry

    Directory of Open Access Journals (Sweden)

    Jeremy L Norris

    2016-01-01

    Full Text Available Background: Imaging mass spectrometry (IMS generates molecular images directly from tissue sections to provide better diagnostic insights and expand the capabilities of clinical anatomic pathology. Although IMS technology has matured over recent years, the link between microscopy imaging currently used by pathologists and MS-based molecular imaging has not been established. Methods: We adapted the Vanderbilt University Tissue Core workflow for IMS into a web-based system that facilitates remote collaboration. The platform was designed to perform within acceptable web response times for viewing, annotating, and processing high resolution microscopy images. Results: We describe a microscopy-driven approach to tissue analysis by IMS. Conclusion: The Pathology Interface for Mass Spectrometry is designed to provide clinical access to IMS technology and deliver enhanced diagnostic value.

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  14. Development of isotope dilution gamma-ray spectrometry for plutonium analysis

    Energy Technology Data Exchange (ETDEWEB)

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

    1991-01-01

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

  15. Liquid separation techniques coupled with mass spectrometry for chiral analysis of pharmaceuticals compounds and their metabolites in biological fluids.

    OpenAIRE

    Erny, Guillaume L.; Cifuentes, Alejandro

    2006-01-01

    Determination of the chiral composition of drugs is nowadays a key step in order to determine purity, activity, bioavailability, biodegradation, etc, of pharmaceuticals. In this manuscript, works published for the last 5 years on the analysis of chiral drugs by liquid separation techniques coupled with mass spectrometry are reviewed. Namely, chiral analysis of pharmaceuticals including e.g., antiinflammatories, antihypertensives, relaxants, etc, by liquid chromatography-mass spectrometry and ...

  16. Analysis of Nitro-aromatic and Nitramine Explosives by Atmospheric Pressure Chemical Ionization / High Performance Liquid Chromatography / Mass Spectrometry / Mass Spectrometry

    International Nuclear Information System (INIS)

    Hicks, B.J.; Han, W.; Robben, J.R.

    2009-01-01

    This procedure is capable of separating and quantifying twenty-nine high explosives and internal surrogates with a single injection. After the initial preparation step, the sample is introduced to the high performance liquid chromatograph for target separation, ionized by atmospheric pressure chemical ionization and the explosives of interest are isolated / quantified by mass spectrometry / mass spectrometry. Concentrations of the target explosives are measured relative to the response of both internal and external standard concentrations. A C-18 reverse phase high performance liquid chromatograph column is used for separation. Ionization is performed using both positive and negative atmospheric pressure chemical ionization resulting in a molecular ion with little fragmentation. These ions are isolated at the first quadrupole of the mass spectrometer, dissociated by collision with argon in the collision cell and the resulting daughter ions are isolated at the second quadrupole. These daughter ions then reach the detector where they are quantified. To date this procedure represents the most thorough high performance liquid chromatography / mass spectrometry / mass spectrometry explosives analysis available in the environmental chemistry market. (authors)

  17. Compositional analysis of silicon nitride films on Si and GaAs by backscattering spectrometry and nuclear resonance reaction analysis

    International Nuclear Information System (INIS)

    Kumar, Sanjiv; Raju, V.S.

    2004-01-01

    This paper describes the application of proton and α-backscattering spectrometry for the determination of atomic ratio of Si to N in 1100-5000 A silicon nitride films on Si and GaAs. The conventional α-Rutherford backscattering spectrometry is suitable for the analysis of films on Si; it is rather inadequate for films on GaAs due to higher background from the substrate. It is shown that these films can be analysed by 14 N(α,α) 14 N scattering with 3.5 MeV α-particles. Proton elastic scattering with enhanced cross sections for 28 Si(p,p) 28 Si and 14 N(p,p) 14 N scatterings, is also suitable for analysing films on GaAs. However, the analysis of films on Si by this technique is difficult due to interferences between the signals of Si from the film and the substrate. In addition, the hydrogen content in films is determined by 1 H( 19 F,αγ) 16 O nuclear reaction analysis using the resonance at 6.4 MeV. The combination of backscattering spectrometry with nuclear reaction analysis provides compositional analysis of ternary Si 1-(x+y) N x H y films

  18. Analysis of aluminium by atomic absorption spectrometry and analysis of thorium and uranium by alpha spectrometry in the black sand of Egypt

    International Nuclear Information System (INIS)

    Hannachi, Dhouha; Mathlouthi, Nadia

    2008-01-01

    Throughout the period of our project of end of study carried out in the Center ; main road Sciences and Nuclear Engineering's CNSTN in one is tallied took one Egypt black sand simple with an aim has of knowing the activities of the existing radio elements and especially Uranium and Thorium. In the same mining, we try to take another Egypt black sand simple an aim has knowing the mass of aluminum by using a techniques in Atomique Absorption Spectrophotometer. After the radio chemical and Spectrometry analysis of the black sand sample we found the results following: - Egypt black sand is contains isotopes of Uranium such as 234 U and 238 U; - The Egypt black sand is contains isotopes of Thorium such as 230 Th and 232 Th. - L' Aluminum is a major. (Author)

  19. Desorption electrospray ionization mass spectrometry for trace analysis of agrochemicals in food.

    Science.gov (United States)

    García-Reyes, Juan F; Jackson, Ayanna U; Molina-Díaz, Antonio; Cooks, R Graham

    2009-01-15

    Desorption electrospray ionization (DESI) is applied to the rapid, in situ, direct qualitative and quantitative (ultra)trace analysis of agrochemicals in foodstuffs. To evaluate the potential of DESI mass spectrometry (MS) in toxic residue testing in food, 16 representative multiclass agricultural chemicals (pesticides, insecticides, herbicides, and fungicides) were selected (namely, ametryn, amitraz, azoxystrobin, bitertanol, buprofezin, imazalil, imazalil metabolite, isofenphos-methyl, malathion, nitenpyram, prochloraz, spinosad, terbuthylazine, thiabendazole, and thiacloprid). The DESI-MS experiments were performed using 3 microL of solution spotted onto conventional smooth poly(tetrafluoroethylene) (PTFE) surfaces, with examination by MS and tandem mass spectrometry (MS/MS) using an ion trap mass spectrometer. Optimization of the spray solvent led to the use of acetonitrile/water (80:20) (v/v), with 1% formic acid. Most of the compounds tested showed remarkable sensitivity in the positive ion mode, approaching that attainable with conventional direct infusion electrospray mass spectrometry. To evaluate the potential of the proposed approach in real samples, different experiments were performed including the direct DESI-MS/MS analysis of fruit peels and also of fruit/vegetable extracts. The results proved that DESI allows the detection and confirmation of traces of agrochemicals in actual market-purchased samples. In addition, MS/MS confirmation of selected pesticides in spiked vegetable extracts was obtained at absolute levels as low as 1 pg for ametryn. Quantitation of imazalil residues was also undertaken using an isotopically labeled standard. The data obtained were in agreement with those from the liquid chromatography mass spectrometry (LC-MS) reference method, with relative standard deviation (RSD) values consistently below 15%. The results obtained demonstrate the sensitivity of DESI as they meet the stringent European Union pesticide regulation

  20. Comparison of 15N analysis by optical emission spectrometry and mass spectrometry for clinical studies during total parenteral nutrition

    International Nuclear Information System (INIS)

    Ragon, A.; Reynier, J.P.; Guiraud, G.

    1985-01-01

    During total and stable parenteral nutrition, a branched chain amino acid enriched solution containing [ 15 N]leucine was infused into a patient to determine the fate of the nitrogen administered through this formulation. Measurements of 15 N isotopic enrichments were performed on the same biological samples (urinary urea, total plasma proteins and albumin) by optical emission spectrometry (OES) and mass spectrometry (MS) to determine if OES with its specific advantages (cost, handling maintenance) constituted even with low enrichments a useful alternative technique to MS considered as the reference method. The results show that OES constituted a very useful analytical technique to obtain reliable information in clinical metabolic studies when low 15 N enrichments must be determined. (Auth.)

  1. Model Titan atmospheric hydrocarbon analysis by Ion Mobility Spectrometry in dry helium

    International Nuclear Information System (INIS)

    Kojiro, D.R.; Stimac, R.M.; Wernlund, R.F.; Cohen, M.J.

    1990-01-01

    Ion Mobility Spectrometry (IMS) is one analytical technique being investigated for the in situ analysis of the atmosphere of Titan. Any hydrocarbon ions that may form react immediately, in microseconds, with the high concentration of water vapor normally present in conventional IMS. By reducing the water concentration to the parts-per-billion range, the lifetime of the hydrocarbon ions may be increased to the milliseconds required for measurement. At low water level concentrations, other species may become the reactant ion. This study focuses on IMS analysis of expected Titan atmospheric hydrocarbons under very dry, low water concentration conditions

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

    International Nuclear Information System (INIS)

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

    1998-01-01

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

  3. Field ionization mass spectrometry (FIMS) applied to tracer studies and isotope dilution analysis

    International Nuclear Information System (INIS)

    Anbar, M.; Heck, H.d'A.; McReynolds, J.H.; St John, G.A.

    1975-01-01

    The nonfragmenting nature of field ionization mass spectrometry makes it a preferred technique for the isotopic analysis of multilabeled organic compounds. The possibility of field ionization of nonvolatile thermolabile materials significantly extends the potential uses of this technique beyond those of conventional ionization methods. Multilabeled tracers may be studied in biological systems with a sensitivity comparable to that of radioactive tracers. Isotope dilution analysis may be performed reliably by this technique down to picogram levels. These techniques will be illustrated by a number of current studies using multilabeled metabolites and drugs. The scope and limitations of the methodology are discussed

  4. X-ray fluorescence analysis and optical emission spectrometry of an roman mirror from Tomis, Romania

    International Nuclear Information System (INIS)

    Belc, M.; Bogoi, M.; Ionescu, D.; Guita, D.; Caiteanu, S.; Caiteanu, D.

    2000-01-01

    The miscellaneous population of Roman Empire, their diverse cultural tradition, their ability to assimilate the roman civilization spirits, had determined a permanent reassessment superimposed upon the roman contribution. Analysis was undertaken using optical emission spectrometry and non-destructive X-ray fluorescence. X-ray fluorescence analysis is a well-established method and is often used in archaeometry and other work dealing with valuable objects pertaining to the history of art and civilization. Roman mirror analysed has been found not to be made of speculum (a high tin bronze). (authors)

  5. Analysis of trace gases at ppb levels by proton transfer reaction mass spectrometry (PTR-MS)

    International Nuclear Information System (INIS)

    Lindinger, W.; Hansel, A.

    1996-01-01

    A proton transfer reaction mass spectrometry (PTR-MS) system has been developed which allows for on-line measurements of trace gas components with concentrations as low as 1 ppb. The method is based on reactions of H 3 O + ions, which perform non-dissociative proton transfer to most of the common organic trace constituents but do not react with any of the components present in clean air. Examples of medical information obtained by means of breath analysis, of environmental trace analysis, and examples in the field of food chemistry demonstrate the wide applicability of the method. (Authors)

  6. Secondary-ion mass spectrometry: some applications in the analysis of nuclear material

    International Nuclear Information System (INIS)

    Christie, W.H.; Eby, R.E.; Warmack, R.J.; Landau, L.

    1981-01-01

    Secondary ion mass spectrometry (SIMS) has been shown to offer some significant advantages over conventional mass spectrometry for the analysis of radioactive samples. We have used SIMS for the rapid, accurate analysis of B, Li, Cs, U and Pu in various nuclear materials. In many instances, SIMS allows one to perform mass and isotopic analysis on samples that are not amenable to other mass spectrometric techniques (e.g., surface ionization, electron impact, etc.). The significant advantage that accrues from the use of SIMS for isotopic analysis of these materials is the cmplete elimination of any chemical sample preparation steps, and only sample dissolution is necessary for the application of isotope dilution methods for quantitative analysis. The high sensitivity of SIMS for B, Li, U and Pu makes it possible to analyze sufficiently small radioactive samples so that radiation is reduced to acceptable levels for safe handling. The precision of SIMS isotopic analysis for natural B samples is about 0.5% and is about 1% for natural Li samples

  7. An Assessment of the SEA Multi-Element Sensor for Liquid Water Content Calibration of the NASA GRC Icing Research Tunnel

    Science.gov (United States)

    Steen, Laura E.; Ide, Robert F.; Van Zante, Judith F.

    2015-01-01

    The NASA Glenn Icing Research tunnel has been using an Icing Blade technique to measure cloud liquid water content (LWC) since 1980. The IRT conducted tests with SEA Multi-Element sensors from 2009 to 2011 to assess their performance in measuring LWC. These tests revealed that the Multi-Element sensors showed some significant advantages over the Icing Blade, particularly at higher water contents, higher impingement rates, and large drop sizes. Results of these and other tests are presented here.

  8. Comparison of the sensitivity of mass spectrometry atmospheric pressure ionization techniques in the analysis of porphyrinoids.

    Science.gov (United States)

    Swider, Paweł; Lewtak, Jan P; Gryko, Daniel T; Danikiewicz, Witold

    2013-10-01

    The porphyrinoids chemistry is greatly dependent on the data obtained in mass spectrometry. For this reason, it is essential to determine the range of applicability of mass spectrometry ionization methods. In this study, the sensitivity of three different atmospheric pressure ionization techniques, electrospray ionization, atmospheric pressure chemical ionization and atmospheric pressure photoionization, was tested for several porphyrinods and their metallocomplexes. Electrospray ionization method was shown to be the best ionization technique because of its high sensitivity for derivatives of cyanocobalamin, free-base corroles and porphyrins. In the case of metallocorroles and metalloporphyrins, atmospheric pressure photoionization with dopant proved to be the most sensitive ionization method. It was also shown that for relatively acidic compounds, particularly for corroles, the negative ion mode provides better sensitivity than the positive ion mode. The results supply a lot of relevant information on the methodology of porphyrinoids analysis carried out by mass spectrometry. The information can be useful in designing future MS or liquid chromatography-MS experiments. Copyright © 2013 John Wiley & Sons, Ltd.

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

    International Nuclear Information System (INIS)

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

    2000-01-01

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

  10. Comparison of mass-spectrometry and α-counting in analysis of uranium and plutonium isotopes in environmental samples

    International Nuclear Information System (INIS)

    Irleweck, K.; Pichlmayer, F.

    1980-01-01

    The determination of trace amounts of U and Pu isotopes is of interest in environmental and personal monitoring programmes. Commonly after preconcentration and separation of the radionuclides a proper sample is prepared electrolytically and the measurements are performed by alpha spectrometry. Some investigations on uranium isotopic abundances and on plutonium fallout deposition in soil have been carried out in this way. It is impossible to distinguish between the isotopes 239 Pu and 240 Pu by alpha spectrometry, however, because their α-energies are too close together. Such determinations can only be carried out by mass spectrometry. Specific Pu emissions, e.g. from nuclear production plants, can be discriminated from the global fallout level. Mass spectrometry is the more sensitive method for measuring long-lived nuclides compared with α-spectrometry. In the case of soil analysis, however, Pu detection is obstructed by the high natural uranium content, usually in the range 0.2 to 2.0 ppm which exceeds the trace amounts of plutonium by several orders of magnitude. This work describes a chemical procedure which separates U/Pu sufficiently for alpha spectrometry as well as for mass spectrometry, and compares results of environmental analysis applying both methods. (author)

  11. A new XRF probe for in-situ determining concentration of multi-elements in ocean sediments

    CERN Document Server

    Ge Liang Quan; Zhou Si Chun; Lin Ling; Lin Yan Chang; Ren Jia Fu

    2001-01-01

    The author introduces a new X-ray fluorescence probe for in-situ determining the concentration of multi-elements in ocean sediments. The probe consists of Si-Pin X-ray detector with an electro-thermal colder, two isotope sources, essential electrical signal processing units and a notebook computer. More than 10 elements can be simultaneously determined at a detection limit of (10-200) x 10 sup - sup 6 and precision of 5%-30% without liquid Nitrogen supply. tests show that the probe can perform the analytical tasks under the water at the depth of less than 1000 meters

  12. A new XRF probe for in-situ determining concentration of multi-elements in ocean sediments

    International Nuclear Information System (INIS)

    Ge Liangquan; Lai Wanchang; Zhou Sichun; Lin Ling; Lin Yanchang; Ren Jiafu

    2001-01-01

    The author introduces a new X-ray fluorescence probe for in-situ determining the concentration of multi-elements in ocean sediments. The probe consists of Si-Pin X-ray detector with an electro-thermal colder, two isotope sources, essential electrical signal processing units and a notebook computer. More than 10 elements can be simultaneously determined at a detection limit of (10-200) x 10 -6 and precision of 5%-30% without liquid Nitrogen supply. tests show that the probe can perform the analytical tasks under the water at the depth of less than 1000 meters

  13. 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...

  14. Toward single-cell analysis by plume collimation in laser ablation electrospray ionization mass spectrometry.

    Science.gov (United States)

    Stolee, Jessica A; Vertes, Akos

    2013-04-02

    Ambient ionization methods for mass spectrometry have enabled the in situ and in vivo analysis of biological tissues and cells. When an etched optical fiber is used to deliver laser energy to a sample in laser ablation electrospray ionization (LAESI) mass spectrometry, the analysis of large single cells becomes possible. However, because in this arrangement the ablation plume expands in three dimensions, only a small portion of it is ionized by the electrospray. Here we show that sample ablation within a capillary helps to confine the radial expansion of the plume. Plume collimation, due to the altered expansion dynamics, leads to greater interaction with the electrospray plume resulting in increased ionization efficiency, reduced limit of detection (by a factor of ~13, reaching 600 amol for verapamil), and extended dynamic range (6 orders of magnitude) compared to conventional LAESI. This enhanced sensitivity enables the analysis of a range of metabolites from small cell populations and single cells in the ambient environment. This technique has the potential to be integrated with flow cytometry for high-throughput metabolite analysis of sorted cells.

  15. Analysis of Dithiocarbamate Fungicides in Vegetable Matrices Using HPLC-UV Followed by Atomic Absorption Spectrometry.

    Science.gov (United States)

    Al-Alam, Josephine; Bom, Laura; Chbani, Asma; Fajloun, Ziad; Millet, Maurice

    2017-04-01

    A simple method combining ion-pair methylation, high-performance liquid chromatography (HPLC) analysis with detection at 272 nm and atomic absorption spectrometry was developed in order to determine 10 dithiocarbamate fungicides (Dazomet, Metam-sodium, Ferbam, Ziram, Zineb, Maneb, Mancozeb, Metiram, Nabam and Propineb) and distinguish ethylenbisdithiocarbamates (EBDTCs) Zineb, Maneb and Mancozeb in diverse matrices. This method associates reverse phase analysis by HPLC analysis with detection at 272 nm, with atomic absorption spectrometry in order to distinguish, with the same extraction protocol, Maneb, Mancozeb and Zineb. The limits of detection (0.4, 0.8, 0.5, 1.25 and 1.97) and quantification (1.18, 2.5, 1.52, 4.2 and 6.52) calculated in injected nanogram, respectively, for Dazomet, Metam-Na, dimethyldithiocarbamates (DMDTCs), EBDTCs and propylenebisdithiocarbamates (PBDTCs) justify the sensitivity of the method used. The coefficients of determination R2 were 0.9985, 0.9978, 0.9949, 0.988 and 0.9794, respectively, for Dazomet, Metam-Na, DMDTCs, EBDTCs and PBDTCs, and the recovery from fortified apple and leek samples was above 90%. Results obtained with the atomic absorption method in comparison with spectrophotometric analysis focus on the importance of the atomic absorption as a complementary specific method for the distinction between different EBDTCs fungicides. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  16. Analysis of hydroxamate siderophores in soil solution using liquid chromatography with mass spectrometry and tandem mass spectrometry with on-line sample preconcentration.

    Science.gov (United States)

    Olofsson, Madelen A; Bylund, Dan

    2015-10-01

    A liquid chromatography with electrospray ionization mass spectrometry method was developed to quantitatively and qualitatively analyze 13 hydroxamate siderophores (ferrichrome, ferrirubin, ferrirhodin, ferrichrysin, ferricrocin, ferrioxamine B, D1 , E and G, neocoprogen I and II, coprogen and triacetylfusarinine C). Samples were preconcentrated on-line by a switch-valve setup prior to analyte separation on a Kinetex C18 column. Gradient elution was performed using a mixture of an ammonium formate buffer and acetonitrile. Total analysis time including column conditioning was 20.5 min. Analytes were fragmented by applying collision-induced dissociation, enabling structural identification by tandem mass spectrometry. Limit of detection values for the selected ion monitoring method ranged from 71 pM to 1.5 nM with corresponding values of two to nine times higher for the multiple reaction monitoring method. The liquid chromatography with mass spectrometry method resulted in a robust and sensitive quantification of hydroxamate siderophores as indicated by retention time stability, linearity, sensitivity, precision and recovery. The analytical error of the methods, assessed through random-order, duplicate analysis of soil samples extracted with a mixture of 10 mM phosphate buffer and methanol, appears negligible in relation to between-sample variations. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Application of ion mobility-mass spectrometry to microRNA analysis.

    Science.gov (United States)

    Takebayashi, Kosuke; Hirose, Kenji; Izumi, Yoshihiro; Bamba, Takeshi; Fukusaki, Eiichiro

    2013-03-01

    Liquid chromatography/mass spectrometry is widely used for studying sequence determination and modification analysis of small RNAs. However, the efficiency of liquid chromatography-based separation of intact small RNA species is insufficient, since the physiochemical properties among small RNAs are very similar. In this study, we focused on ion mobility-mass spectrometry (IM-MS), which is a gas-phase separation technique coupled with mass spectrometry; we have evaluated the utility of IM-MS for microRNA (miRNA) analysis. A multiply charged deprotonated ion derived from an 18-24-nt-long miRNA was formed by electrospray ionization, and then the time, called the "drift time", taken by each ion to migrate through a buffer gas was measured. Each multivalent ion was temporally separated on the basis of the charge state and structural formation; 3 types of unique mass-mobility correlation patterns (i.e., chainlike-form, hairpin-form, and dimer-form) were present on the two-dimensional mobility-mass spectrum. Moreover, we found that the ion size (sequence length) and the secondary structures of the small RNAs strongly contributed to the IM-MS-based separation, although solvent conditions such as pH had no effect. Therefore, sequence isomers could also be discerned by the selection of each specific charged ion, i.e., the 6(-) charged ion reflected a majority among chainlike-, hairpin-, and other structures. We concluded that the IM-MS provides additional capability for separation; thus, this analytical method will be a powerful tool for comprehensive small RNA analysis. Copyright © 2012. Published by Elsevier B.V.

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

    Science.gov (United States)

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

    2018-06-01

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

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

  20. Single particle transfer for quantitative analysis with total-reflection X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Esaka, Fumitaka; Esaka, Konomi T.; Magara, Masaaki; Sakurai, Satoshi; Usuda, Shigekazu; Watanabe, Kazuo

    2006-01-01

    The technique of single particle transfer was applied to quantitative analysis with total-reflection X-ray fluorescence (TXRF) spectrometry. The technique was evaluated by performing quantitative analysis of individual Cu particles with diameters between 3.9 and 13.2 μm. The direct quantitative analysis of the Cu particle transferred onto a Si carrier gave a discrepancy between measured and calculated Cu amounts due to the absorption effects of incident and fluorescent X-rays within the particle. By the correction for the absorption effects, the Cu amounts in individual particles could be determined with the deviation within 10.5%. When the Cu particles were dissolved with HNO 3 solution prior to the TXRF analysis, the deviation was improved to be within 3.8%. In this case, no correction for the absorption effects was needed for quantification

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

    International Nuclear Information System (INIS)

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

    1984-01-01

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

  2. Analysis of arsenic and calcium in soil samples by laser ablation mass spectrometry

    International Nuclear Information System (INIS)

    Beccaglia, Ana M.; Rinaldi, Carlos A.; Ferrero, Juan C.

    2006-01-01

    We present an analytical procedure based on laser ablation mass spectrometry (LAMS) in order to detect and quantify arsenic and calcium in soil samples and we analyze the diverse factors that influence the precision of LAMS, such as laser fluence and matrix effect. The results indicate that a Zn matrix is a good choice for the analysis of those metals in soil samples. This work also provides a method for the direct determination of As in soil samples whose concentrations are lower than 100 ppm with a 70 ppm minimum detection limits (MDL)

  3. Error analysis of isotope dilution mass spectrometry method with internal standard

    International Nuclear Information System (INIS)

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

    1989-02-01

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

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

    International Nuclear Information System (INIS)

    Wagatsuma, K.; Hirokawa, K.

    1984-01-01

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

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

    International Nuclear Information System (INIS)

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

    1998-01-01

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

  6. On the Importance of Mathematical Methods for Analysis of MALDI-Imaging Mass Spectrometry Data

    Directory of Open Access Journals (Sweden)

    Trede Dennis

    2012-03-01

    Full Text Available In the last decade, matrix-assisted laser desorption/ionization (MALDI imaging mass spectrometry (IMS, also called as MALDI-imaging, has proven its potential in proteomics and was successfully applied to various types of biomedical problems, in particular to histopathological label-free analysis of tissue sections. In histopathology, MALDI-imaging is used as a general analytic tool revealing the functional proteomic structure of tissue sections, and as a discovery tool for detecting new biomarkers discriminating a region annotated by an experienced histologist, in particular, for cancer studies.

  7. The analysis, by a fusion procedure and X-ray-fluorescence spectrometry, of silicates and slags

    International Nuclear Information System (INIS)

    Jacobs, J.J.; Balaes, A.M.E.

    1980-01-01

    A glass-disc fusion method is described for the analysis, by X-ray-fluorescence spectrometry, of slags and silicate materials. The data are corrected for detector dead time and short-term instrumental drift. Corrections are made for matrix variations by use of the Lachange-Traill mathematical model, and the results are processed on a mini-computer, an iterative procedure being used in the solving of the simultaneous equations. As the alpha-correction coefficients of the Lachange-Traill model are not truly constant, a modified version of the model is proposed [af

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-12-01

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

  10. Efficiency Evaluation of Food Waste Materials for the Removal of Metals and Metalloids from Complex Multi-Element Solutions

    Science.gov (United States)

    Giuliano, Antonella; Astolfi, Maria Luisa; Congedo, Rossana; Masotti, Andrea; Canepari, Silvia

    2018-01-01

    Recent studies have shown the potential of food waste materials as low cost adsorbents for the removal of heavy metals and toxic elements from wastewater. However, the adsorption experiments have been performed in heterogeneous conditions, consequently it is difficult to compare the efficiency of the individual adsorbents. In this study, the adsorption capacities of 12 food waste materials were evaluated by comparing the adsorbents’ efficiency for the removal of 23 elements from complex multi-element solutions, maintaining homogeneous experimental conditions. The examined materials resulted to be extremely efficient for the adsorption of many elements from synthetic multi-element solutions as well as from a heavy metal wastewater. The 12 adsorbent surfaces were analyzed by Fourier transform infrared spectroscopy and showed different types and amounts of functional groups, which demonstrated to act as adsorption active sites for various elements. By multivariate statistical computations of the obtained data, the 12 food waste materials were grouped in five clusters characterized by different elements’ removal efficiency which resulted to be in correlation with the specific adsorbents’ chemical structures. Banana peel, watermelon peel and grape waste resulted the least selective and the most efficient food waste materials for the removal of most of the elements. PMID:29495363

  11. Efficiency Evaluation of Food Waste Materials for the Removal of Metals and Metalloids from Complex Multi-Element Solutions.

    Science.gov (United States)

    Massimi, Lorenzo; Giuliano, Antonella; Astolfi, Maria Luisa; Congedo, Rossana; Masotti, Andrea; Canepari, Silvia

    2018-02-26

    Recent studies have shown the potential of food waste materials as low cost adsorbents for the removal of heavy metals and toxic elements from wastewater. However, the adsorption experiments have been performed in heterogeneous conditions, consequently it is difficult to compare the efficiency of the individual adsorbents. In this study, the adsorption capacities of 12 food waste materials were evaluated by comparing the adsorbents' efficiency for the removal of 23 elements from complex multi-element solutions, maintaining homogeneous experimental conditions. The examined materials resulted to be extremely efficient for the adsorption of many elements from synthetic multi-element solutions as well as from a heavy metal wastewater. The 12 adsorbent surfaces were analyzed by Fourier transform infrared spectroscopy and showed different types and amounts of functional groups, which demonstrated to act as adsorption active sites for various elements. By multivariate statistical computations of the obtained data, the 12 food waste materials were grouped in five clusters characterized by different elements' removal efficiency which resulted to be in correlation with the specific adsorbents' chemical structures. Banana peel, watermelon peel and grape waste resulted the least selective and the most efficient food waste materials for the removal of most of the elements.

  12. A new large solid angle multi-element silicon drift detector system for low energy X-ray fluorescence spectroscopy

    Science.gov (United States)

    Bufon, J.; Schillani, S.; Altissimo, M.; Bellutti, P.; Bertuccio, G.; Billè, F.; Borghes, R.; Borghi, G.; Cautero, G.; Cirrincione, D.; Fabiani, S.; Ficorella, F.; Gandola, M.; Gianoncelli, A.; Giuressi, D.; Kourousias, G.; Mele, F.; Menk, R. H.; Picciotto, A.; Rachevski, A.; Rashevskaya, I.; Sammartini, M.; Stolfa, A.; Zampa, G.; Zampa, N.; Zorzi, N.; Vacchi, A.

    2018-03-01

    Low-energy X-ray fluorescence (LEXRF) is an essential tool for bio-related research of organic samples, whose composition is dominated by light elements. Working at energies below 2 keV and being able to detect fluorescence photons of lightweight elements such as carbon (277 eV) is still a challenge, since it requires in-vacuum operations to avoid in-air photon absorption. Moreover, the detectors must have a thin entrance window and collect photons at an angle of incidence near 90 degrees to minimize the absorption by the protective coating. Considering the low fluorescence yield of light elements, it is important to cover a substantial part of the solid angle detecting ideally all emitted X-ray fluorescence (XRF) photons. Furthermore, the energy resolution of the detection system should be close to the Fano limit in order to discriminate elements whose XRF emission lines are often very close within the energy spectra. To ensure all these features, a system consisting of four monolithic multi-element silicon drift detectors was developed. The use of four separate detector units allows optimizing the incidence angle on all the sensor elements. The multi-element approach in turn provides a lower leakage current on each anode, which, in combination with ultra-low noise preamplifiers, is necessary to achieve an energy resolution close to the Fano limit. The potential of the new detection system and its applicability for typical LEXRF applications has been proved on the Elettra TwinMic beamline.

  13. Efficiency Evaluation of Food Waste Materials for the Removal of Metals and Metalloids from Complex Multi-Element Solutions

    Directory of Open Access Journals (Sweden)

    Lorenzo Massimi

    2018-02-01

    Full Text Available Recent studies have shown the potential of food waste materials as low cost adsorbents for the removal of heavy metals and toxic elements from wastewater. However, the adsorption experiments have been performed in heterogeneous conditions, consequently it is difficult to compare the efficiency of the individual adsorbents. In this study, the adsorption capacities of 12 food waste materials were evaluated by comparing the adsorbents’ efficiency for the removal of 23 elements from complex multi-element solutions, maintaining homogeneous experimental conditions. The examined materials resulted to be extremely efficient for the adsorption of many elements from synthetic multi-element solutions as well as from a heavy metal wastewater. The 12 adsorbent surfaces were analyzed by Fourier transform infrared spectroscopy and showed different types and amounts of functional groups, which demonstrated to act as adsorption active sites for various elements. By multivariate statistical computations of the obtained data, the 12 food waste materials were grouped in five clusters characterized by different elements’ removal efficiency which resulted to be in correlation with the specific adsorbents’ chemical structures. Banana peel, watermelon peel and grape waste resulted the least selective and the most efficient food waste materials for the removal of most of the elements.

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

    International Nuclear Information System (INIS)

    Carneiro, Andre Cavalcanti

    2015-01-01

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

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

  16. Analysis of human serum by liquid chromatography-mass spectrometry: improved sample preparation and data analysis.

    Science.gov (United States)

    Govorukhina, N I; Reijmers, T H; Nyangoma, S O; van der Zee, A G J; Jansen, R C; Bischoff, R

    2006-07-07

    Discovery of biomarkers is a fast developing field in proteomics research. Liquid chromatography coupled on line to mass spectrometry (LC-MS) has become a powerful method for the sensitive detection, quantification and identification of proteins and peptides in biological fluids like serum. However, the presence of highly abundant proteins often masks those of lower abundance and thus generally prevents their detection and identification in proteomics studies. To perform future comparative analyses of samples from a serum bank of cervical cancer patients in a longitudinal and cross-sectional manner, methodology based on the depletion of high-abundance proteins followed by tryptic digestion and LC-MS has been developed. Two sample preparation methods were tested in terms of their efficiency to deplete high-abundance serum proteins and how they affect the repeatability of the LC-MS data sets. The first method comprised depletion of human serum albumin (HSA) on a dye ligand chromatographic and immunoglobulin G (IgG) on an immobilized Protein A support followed by tryptic digestion, fractionation by cation-exchange chromatography, trapping on a C18 column and reversed-phase LC-MS. The second method included depletion of the six most abundant serum proteins based on multiple immunoaffinity chromatography followed by tryptic digestion, trapping on a C18 column and reversed-phase LC-MS. Repeatability of the overall procedures was evaluated in terms of retention time and peak area for a selected number of endogenous peptides showing that the second method, besides being less time consuming, gave more repeatable results (retention time: <0.1% RSD; peak area: <30% RSD). Application of an LC-MS component detection algorithm followed by principal component analysis (PCA) enabled discrimination of serum samples that were spiked with horse heart cytochrome C from non-spiked serum and the detection of a concentration trend, which correlated to the amount of spiked horse heart

  17. Biomedical application of MALDI mass spectrometry for small-molecule analysis.

    Science.gov (United States)

    van Kampen, Jeroen J A; Burgers, Peter C; de Groot, Ronald; Gruters, Rob A; Luider, Theo M

    2011-01-01

    Matrix-assisted laser desorption/ionization (MALDI) mass spectrometry (MS) is an emerging analytical tool for the analysis of molecules with molar masses below 1,000 Da; that is, small molecules. This technique offers rapid analysis, high sensitivity, low sample consumption, a relative high tolerance towards salts and buffers, and the possibility to store sample on the target plate. The successful application of the technique is, however, hampered by low molecular weight (LMW) matrix-derived interference signals and by poor reproducibility of signal intensities during quantitative analyses. In this review, we focus on the biomedical application of MALDI-MS for the analysis of small molecules and discuss its favorable properties and its challenges as well as strategies to improve the performance of the technique. Furthermore, practical aspects and applications are presented. © 2010 Wiley Periodicals, Inc.

  18. Direct Surface Analysis of Fungal Species by Matrix-assisted Laser Desorption/Ionization Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Valentine, Nancy B.(BATTELLE (PACIFIC NW LAB)); Wahl, Jon H.(BATTELLE (PACIFIC NW LAB)); Kingsley, Mark T.(BATTELLE (PACIFIC NW LAB)); Wahl, Karen L.(BATTELLE (PACIFIC NW LAB))

    2001-12-01

    Intact spores and/or hyphae of Aspergillus niger, Rhizopus oryzae, Trichoderma reesei and Phanerochaete chrysosporium are analyzed by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS). This study investigates various methods of sample preparation and matrices to determine optimum collection and analysis criteria for fungal analysis by MALDI-MS. Fungi are applied to the MALDI sample target as untreated, sonicated, acid/heat treated, or blotted directly from the fungal culture with double-stick tape. Ferulic acid or sinapinic acid matrix solution is layered over the dried samples and analyzed by MALDI-MS. Statistical analysis of the data show that simply using double stick tape to collect and transfer to a MALDI sample plate typically worked as well as the other preparation methods, but requires the least sample handling.

  19. Carbohydrates on Proteins: Site-Specific Glycosylation Analysis by Mass Spectrometry

    Science.gov (United States)

    Zhu, Zhikai; Desaire, Heather

    2015-07-01

    Glycosylation on proteins adds complexity and versatility to these biologically vital macromolecules. To unveil the structure-function relationship of glycoproteins, glycopeptide-centric analysis using mass spectrometry (MS) has become a method of choice because the glycan is preserved on the glycosylation site and site-specific glycosylation profiles of proteins can be readily determined. However, glycopeptide analysis is still challenging given that glycopeptides are usually low in abundance and relatively difficult to detect and the resulting data require expertise to analyze. Viewing the urgent need to address these challenges, emerging methods and techniques are being developed with the goal of analyzing glycopeptides in a sensitive, comprehensive, and high-throughput manner. In this review, we discuss recent advances in glycoprotein and glycopeptide analysis, with topics covering sample preparation, analytical separation, MS and tandem MS techniques, as well as data interpretation and automation.

  20. Stable Isotope Quantitative N-Glycan Analysis by Liquid Separation Techniques and Mass Spectrometry.

    Science.gov (United States)

    Mittermayr, Stefan; Albrecht, Simone; Váradi, Csaba; Millán-Martín, Silvia; Bones, Jonathan

    2017-01-01

    Liquid phase separation analysis and subsequent quantitation remains a challenging task for protein-derived oligosaccharides due to their inherent structural complexity and diversity. Incomplete resolution or co-detection of multiple glycan species complicates peak area-based quantitation and associated statistical analysis when optical detection methods are used. The approach outlined herein describes the utilization of stable isotope variants of commonly used fluorescent tags that allow for mass-based glycan identification and relative quantitation following separation by liquid chromatography (LC) or capillary electrophoresis (CE). Comparability assessment of glycoprotein-derived oligosaccharides is performed by derivatization with commercially available isotope variants of 2-aminobenzoic acid or aniline and analysis by LC- and CE-mass spectrometry. Quantitative information is attained from the extracted ion chromatogram/electropherogram ratios generated from the light and heavy isotope clusters.

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

    DEFF Research Database (Denmark)

    Andersen, Jens Enevold Thaulov

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

  2. Ion mobility spectrometry-mass spectrometry (IMS-MS) for on- and offline analysis of atmospheric gas and aerosol species

    Science.gov (United States)

    Krechmer, Jordan E.; Groessl, Michael; Zhang, Xuan; Junninen, Heikki; Massoli, Paola; Lambe, Andrew T.; Kimmel, Joel R.; Cubison, Michael J.; Graf, Stephan; Lin, Ying-Hsuan; Budisulistiorini, Sri H.; Zhang, Haofei; Surratt, Jason D.; Knochenmuss, Richard; Jayne, John T.; Worsnop, Douglas R.; Jimenez, Jose-Luis; Canagaratna, Manjula R.

    2016-07-01

    Measurement techniques that provide molecular-level information are needed to elucidate the multiphase processes that produce secondary organic aerosol (SOA) species in the atmosphere. Here we demonstrate the application of ion mobility spectrometry-mass spectrometry (IMS-MS) to the simultaneous characterization of the elemental composition and molecular structures of organic species in the gas and particulate phases. Molecular ions of gas-phase organic species are measured online with IMS-MS after ionization with a custom-built nitrate chemical ionization (CI) source. This CI-IMS-MS technique is used to obtain time-resolved measurements (5 min) of highly oxidized organic molecules during the 2013 Southern Oxidant and Aerosol Study (SOAS) ambient field campaign in the forested SE US. The ambient IMS-MS signals are consistent with laboratory IMS-MS spectra obtained from single-component carboxylic acids and multicomponent mixtures of isoprene and monoterpene oxidation products. Mass-mobility correlations in the 2-D IMS-MS space provide a means of identifying ions with similar molecular structures within complex mass spectra and are used to separate and identify monoterpene oxidation products in the ambient data that are produced from different chemical pathways. Water-soluble organic carbon (WSOC) constituents of fine aerosol particles that are not resolvable with standard analytical separation methods, such as liquid chromatography (LC), are shown to be separable with IMS-MS coupled to an electrospray ionization (ESI) source. The capability to use ion mobility to differentiate between isomers is demonstrated for organosulfates derived from the reactive uptake of isomers of isoprene epoxydiols (IEPOX) onto wet acidic sulfate aerosol. Controlled fragmentation of precursor ions by collisionally induced dissociation (CID) in the transfer region between the IMS and the MS is used to validate MS peak assignments, elucidate structures of oligomers, and confirm the

  3. Recent advancements and future trends in environmental analysis: Sample preparation, liquid chromatography and mass spectrometry.

    Science.gov (United States)

    Pérez-Fernández, Virginia; Mainero Rocca, Lucia; Tomai, Pierpaolo; Fanali, Salvatore; Gentili, Alessandra

    2017-08-29

    Among the thousands of chemicals having potential to enter the environment, the NORMAN network has identified at least 700 substances categorized into 20 classes in the European surface waters. Pesticides, pharmaceuticals, disinfection by-products, wood preservation and industrial chemicals are the prominent classes. Since the impact of these substances on aquatic life and human health might be dramatic, action is urgently required at multiple levels; one of them is just related to the development of more and more sensible and selective analytical methods. This review highlights the latest advancements and trends in liquid chromatography-mass spectrometry based environmental analysis. Specific sections are dedicated to novelties in sample preparation, chromatographic separation and mass spectrometry detection of emerging pollutants. The review also offers insights on last generation chromatographic and extraction materials, technological progresses and innovative methodological approaches for target and non-target analysis. As numerous papers have been published in this field, this overview covers the most representative and original works published in the 2011-2016 period. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Heparin/heparan sulfate analysis by covalently modified reverse polarity capillary zone electrophoresis-mass spectrometry.

    Science.gov (United States)

    Sanderson, Patience; Stickney, Morgan; Leach, Franklin E; Xia, Qiangwei; Yu, Yanlei; Zhang, Fuming; Linhardt, Robert J; Amster, I Jonathan

    2018-04-13

    Reverse polarity capillary zone electrophoresis coupled to negative ion mode mass spectrometry (CZE-MS) is shown to be an effective and sensitive tool for the analysis of glycosaminoglycan mixtures. Covalent modification of the inner wall of the separation capillary with neutral or cationic reagents produces a stable and durable surface that provides reproducible separations. By combining CZE-MS with a cation-coated capillary and a sheath flow interface, a rapid and reliable method has been developed for the analysis of sulfated oligosaccharides from dp4 to dp12. Several different mixtures have been separated and detected by mass spectrometry. The mixtures were selected to test the capability of this approach to resolve subtle differences in structure, such as sulfation position and epimeric variation of the uronic acid. The system was applied to a complex mixture of heparin/heparan sulfate oligosaccharides varying in chain length from dp3 to dp12 and more than 80 molecular compositions were identified by accurate mass measurement. Copyright © 2018 Elsevier B.V. All rights reserved.

  5. Quantitative analysis of phytosterols in edible oils using APCI liquid chromatography-tandem mass spectrometry

    Science.gov (United States)

    Mo, Shunyan; Dong, Linlin; Hurst, W. Jeffrey; van Breemen, Richard B.

    2014-01-01

    Previous methods for the quantitative analysis of phytosterols have usually used GC-MS and require elaborate sample preparation including chemical derivatization. Other common methods such as HPLC with absorbance detection do not provide information regarding the identity of the analytes. To address the need for an assay that utilizes mass selectivity while avoiding derivatization, a quantitative method based on LC-tandem mass spectrometry (LC-MS-MS) was developed and validated for the measurement of six abundant dietary phytosterols and structurally related triterpene alcohols including brassicasterol, campesterol, cycloartenol, β-sitosterol, stigmasterol, and lupeol in edible oils. Samples were saponified, extracted with hexane and then analyzed using reversed phase HPLC with positive ion atmospheric pressure chemical ionization tandem mass spectrometry and selected reaction monitoring. The utility of the LC-MS-MS method was demonstrated by analyzing 14 edible oils. All six compounds were present in at least some of the edible oils. The most abundant phytosterol in all samples was β-sitosterol, which was highest in corn oil at 4.35 ± 0.03 mg/g, followed by campesterol in canola oil at 1.84 ± 0.01 mg/g. The new LC-MS-MS method for the quantitative analysis of phytosterols provides a combination of speed, selectivity and sensitivity that exceed those of previous assays. PMID:23884629

  6. Detection of Low Molecular Weight Adulterants in Beverages by Direct Analysis in Real Time Mass Spectrometry.

    Science.gov (United States)

    Sisco, Edward; Dake, Jeffrey

    2016-04-14

    Direct Analysis in Real Time Mass Spectrometry (DART-MS) has been used to detect the presence of non-narcotic adulterants in beverages. The non-narcotic adulterants that were examined in this work incorporated a number low molecular weight alcohols, acetone, ammonium hydroxide, and sodium hypochlorite. Analysis of the adulterants was completed by pipetting 1 µL deposits onto glass microcapillaries along with an appropriate dopant species followed by introduction into the DART gas stream. It was found that detection of these compounds in the complex matrices of common beverages (soda, energy drinks, etc.) was simplified through the use of a dopant species to allow for adduct formation with the desired compound(s) of interest. Other parameters that were investigated included DART gas stream temperature, in source collision induced dissociation, ion polarity, and DART needle voltage. Sensitivities of the technique were found to range from 0.001 % volume fraction to 0.1 % volume fraction, comparable to traditional analyses completed using headspace gas chromatography mass spectrometry (HS-GC/MS). Once a method was established using aqueous solutions, , fifteen beverages were spiked with each of the nine adulterants, to simulate real world detection, and in nearly all cases the adulterant could be detected either in pure form, or complexed with the added dopant species. This technique provides a rapid way to directly analyze beverages believed to be contaminated with non-narcotic adulterants at sensitivities similar to or exceeding those of traditional confirmatory analyses.

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

    Science.gov (United States)

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

    2013-08-07

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

  8. Nonreductive chemical release of intact N-glycans for subsequent labeling and analysis by mass spectrometry.

    Science.gov (United States)

    Yuan, Jiangbei; Wang, Chengjian; Sun, Yujiao; Huang, Linjuan; Wang, Zhongfu

    2014-10-01

    A novel strategy is proposed, using cost-saving chemical reactions to generate intact free reducing N-glycans and their fluorescent derivatives from glycoproteins for subsequent analysis. N-Glycans without core α-1,3-linked fucose are released in reducing form by selective hydrolysis of the N-type carbohydrate-peptide bond of glycoproteins under a set of optimized mild alkaline conditions and are comparable to those released by commonly used peptide-N-glycosidase (PNGase) F in terms of yield without any detectable side reaction (peeling or deacetylation). The obtained reducing glycans can be routinely derivatized with 2-aminobenzoic acid (2-AA), 1-phenyl-3-methyl-5-pyrazolone (PMP), and potentially some other fluorescent reagents for comprehensive analysis. Alternatively, the core α-1,3-fucosylated N-glycans are released in mild alkaline medium and derivatized with PMP in situ, and their yields are comparable to those obtained using commonly used PNGase A without conspicuous peeling reaction or any detectable deacetylation. Using this new technique, the N-glycans of a series of purified glycoproteins and complex biological samples were successfully released and analyzed by electrospray ionization mass spectrometry (ESI-MS) and tandem mass spectrometry (MS/MS), demonstrating its general applicability to glycomic studies. Copyright © 2014 Elsevier Inc. All rights reserved.

  9. Chemical analysis of zinc electroplating solutions by x-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Jung, Sung-Mo; Cho, Young-Mo; Na, Han-Gil

    2007-01-01

    A quantitative analysis method used to analyze chlorine, iron and zinc in electroplating solutions, using X-ray spectrometry in atmospheric He mode, is proposed. The present research concerns the replacement of the conventional analyses of electroplating solutions with rapid and reproducible quantification using X-ray fluorescence spectrometer. An in-depth investigation conducted in the present study identifies the species present in the real electroplating solutions. XRD patterns and semi-quantitative results for the electroplating solutions show synthetic standards based on the compositional range of solutions by analyzing the electroplating solutions obtained in real processes. 28 calibration standard solutions are prepared by diluting liquid standard solutions certified by titration and ICP-OES analyses used to construct the XRF calibration curves for Cl, Fe and Zn. The suggested method showed satisfactory precision and accuracy in the analysis of electroplating solutions. The present study provides evidences that the proposed XRF spectrometry could be an alternative analytical method to replace the conventional techniques by comparing the uncertainties estimated for each method. (author)

  10. Carboxylic acid functional group analysis using constant neutral loss scanning-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Dron, Julien [Laboratoire de Chimie et Environnement, Marseille Universites (case 29), 3 place Victor Hugo, 13331 Marseille Cedex 3 (France)], E-mail: julien.dron@up.univ-mrs.fr; Eyglunent, Gregory; Temime-Roussel, Brice; Marchand, Nicolas; Wortham, Henri [Laboratoire de Chimie et Environnement, Marseille Universites (case 29), 3 place Victor Hugo, 13331 Marseille Cedex 3 (France)

    2007-12-12

    The present study describes the development of a new analytical technique for the functional group determination of the carboxylic moiety using atmospheric pressure chemical ionization-mass spectrometry (APCI-MS/MS) operated in the constant neutral loss scanning (CNLS) mode. Carboxylic groups were first derivatized into their corresponding methyl esters by reacting with BF{sub 3}/methanol mix and the reaction mixture was then directly injected into the APCI chamber. The loss of methanol (m/z = 32 amu) resulting from the fragmentation of the protonated methyl esters was then monitored. Applying this method together with a statistical approach to reference mixtures containing 31 different carboxylic acids at randomly calculated concentrations demonstrated its suitability for quantitative functional group measurements with relative standard deviations below 15% and a detection limit of 0.005 mmol L{sup -1}. Its applicability to environmental matrices was also shown through the determination of carboxylic acid concentrations inside atmospheric aerosol samples. To the best of our knowledge, it is the first time that the tandem mass spectrometry was successfully applied to functional group analysis, offering great perspectives in the characterization of complex mixtures which are prevailing in the field of environmental analysis as well as in the understanding of the chemical processes occurring in these matrices.

  11. Carboxylic acid functional group analysis using constant neutral loss scanning-mass spectrometry

    International Nuclear Information System (INIS)

    Dron, Julien; Eyglunent, Gregory; Temime-Roussel, Brice; Marchand, Nicolas; Wortham, Henri

    2007-01-01

    The present study describes the development of a new analytical technique for the functional group determination of the carboxylic moiety using atmospheric pressure chemical ionization-mass spectrometry (APCI-MS/MS) operated in the constant neutral loss scanning (CNLS) mode. Carboxylic groups were first derivatized into their corresponding methyl esters by reacting with BF 3 /methanol mix and the reaction mixture was then directly injected into the APCI chamber. The loss of methanol (m/z = 32 amu) resulting from the fragmentation of the protonated methyl esters was then monitored. Applying this method together with a statistical approach to reference mixtures containing 31 different carboxylic acids at randomly calculated concentrations demonstrated its suitability for quantitative functional group measurements with relative standard deviations below 15% and a detection limit of 0.005 mmol L -1 . Its applicability to environmental matrices was also shown through the determination of carboxylic acid concentrations inside atmospheric aerosol samples. To the best of our knowledge, it is the first time that the tandem mass spectrometry was successfully applied to functional group analysis, offering great perspectives in the characterization of complex mixtures which are prevailing in the field of environmental analysis as well as in the understanding of the chemical processes occurring in these matrices

  12. Multi-element, multi-compound isotope profiling as a means to distinguish the geographical and varietal origin of fermented cocoa (Theobroma cacao L.) beans.

    Science.gov (United States)

    Diomande, Didier; Antheaume, Ingrid; Leroux, Maël; Lalande, Julie; Balayssac, Stéphane; Remaud, Gérald S; Tea, Illa

    2015-12-01

    Multi-element stable isotope ratios have been assessed as a means to distinguish between fermented cocoa beans from different geographical and varietal origins. Isotope ratios and percentage composition for C and N were measured in different tissues (cotyledons, shells) and extracts (pure theobromine, defatted cocoa solids, protein, lipids) obtained from fermented cocoa bean samples. Sixty-one samples from 24 different geographical origins covering all four continental areas producing cocoa were analyzed. Treatment of the data with unsupervised (Principal Component Analysis) and supervised (Partial Least Squares Discriminant Analysis) multiparametric statistical methods allowed the cocoa beans from different origins to be distinguished. The most discriminant variables identified as responsible for geographical and varietal differences were the δ(15)N and δ(13)C values of cocoa beans and some extracts and tissues. It can be shown that the isotope ratios are correlated with the altitude and precipitation conditions found in the different cocoa-growing regions. Copyright © 2015 Elsevier Ltd. All rights reserved.

  13. Mass spectrometry-based serum proteome pattern analysis in molecular diagnostics of early stage breast cancer

    Directory of Open Access Journals (Sweden)

    Stobiecki Maciej

    2009-07-01

    Full Text Available Abstract Background Mass spectrometric analysis of the blood proteome is an emerging method of clinical proteomics. The approach exploiting multi-protein/peptide sets (fingerprints detected by mass spectrometry that reflect overall features of a specimen's proteome, termed proteome pattern analysis, have been already shown in several studies to have applicability in cancer diagnostics. We aimed to identify serum proteome patterns specific for early stage breast cancer patients using MALDI-ToF mass spectrometry. Methods Blood samples were collected before the start of therapy in a group of 92 patients diagnosed at stages I and II of the disease, and in a group of age-matched healthy controls (104 women. Serum specimens were purified and the low-molecular-weight proteome fraction was examined using MALDI-ToF mass spectrometry after removal of albumin and other high-molecular-weight serum proteins. Protein ions registered in a mass range between 2,000 and 10,000 Da were analyzed using a new bioinformatic tool created in our group, which included modeling spectra as a sum of Gaussian bell-shaped curves. Results We have identified features of serum proteome patterns that were significantly different between blood samples of healthy individuals and early stage breast cancer patients. The classifier built of three spectral components that differentiated controls and cancer patients had 83% sensitivity and 85% specificity. Spectral components (i.e., protein ions that were the most frequent in such classifiers had approximate m/z values of 2303, 2866 and 3579 Da (a biomarker built from these three components showed 88% sensitivity and 78% specificity. Of note, we did not find a significant correlation between features of serum proteome patterns and established prognostic or predictive factors like tumor size, nodal involvement, histopathological grade, estrogen and progesterone receptor expression. In addition, we observed a significantly (p = 0

  14. ENVIRONMENTAL ANALYSIS BY AB INITIO QUANTUM MECHANICAL COMPUTATION AND GAS CHROMATOGRAPHY/FOURIER TRANSFORM INFRARED SPECTROMETRY.

    Science.gov (United States)

    Computational chemistry, in conjunction with gas chromatography/mass spectrometry/Fourier transform infrared spectrometry (GC/MS/FT-IR), was used to tentatively identify seven tetrachlorobutadiene (TCBD) isomers detected in an environmental sample. Computation of the TCBD infrare...

  15. Multi-element bioimaging of Arabidopsis thaliana roots

    DEFF Research Database (Denmark)

    Persson, Daniel Olof; Chen, Anle; Aarts, Mark G.M.

    2016-01-01

    Better understanding of root function is central for the development of plants with more efficient nutrient uptake and translocation. We here present a method for multielement bioimaging at the cellular level in roots of the genetic model system Arabidopsis (Arabidopsis thaliana). Using conventio......Better understanding of root function is central for the development of plants with more efficient nutrient uptake and translocation. We here present a method for multielement bioimaging at the cellular level in roots of the genetic model system Arabidopsis (Arabidopsis thaliana). Using...... omics techniques. To demonstrate the potential of the method, we analyzed a mutant of Arabidopsis unable to synthesize the metal chelator nicotianamine. The mutant accumulated substantially more zinc and manganese than the wild type in the tissues surrounding the vascular cylinder. For iron, the images...... looked completely different, with iron bound mainly in the epidermis of the wild-type plants but confined to the cortical cell walls of the mutant. The method offers the power of inductively coupled plasma-mass spectrometry to be fully employed, thereby providing a basis for detailed studies of ion...

  16. Multi-Elemental Profiling of Tibial and Maxillary Trabecular Bone in Ovariectomised Rats

    Directory of Open Access Journals (Sweden)

    Pingping Han

    2016-06-01

    Full Text Available Atomic minerals are the smallest components of bone and the content of Ca, being the most abundant mineral in bone, correlates strongly with the risk of osteoporosis. Postmenopausal women have a far greater risk of suffering from OP due to low Ca concentrations in their bones and this is associated with low bone mass and higher bone fracture rates. However, bone strength is determined not only by Ca level, but also a number of metallic and non-metallic elements in bone. Thus, in this study, the difference of metallic and non-metallic elements in ovariectomy-induced osteoporosis tibial and maxillary trabecular bone was investigated in comparison with sham operated normal bone by laser ablation inductively-coupled plasma mass spectrometry using a rat model. The results demonstrated that the average concentrations of 25Mg, 28Si, 39K, 47Ti, 56Fe, 59Co, 77Se, 88Sr, 137Ba, and 208Pb were generally higher in tibia than those in maxilla. Compared with the sham group, Ovariectomy induced more significant changes of these elements in tibia than maxilla, indicating tibial trabecular bones are more sensitive to changes of circulating estrogen. In addition, the concentrations of 28Si, 77Se, 208Pb, and Ca/P ratios were higher in tibia and maxilla in ovariectomised rats than those in normal bone at all time-points. The present study indicates that ovariectomy could significantly impact the element distribution and concentrations between tibia and maxilla.

  17. Dynamic analysis of CO₂ labeling and cell respiration using membrane-inlet mass spectrometry.

    Science.gov (United States)

    Yang, Tae Hoon

    2014-01-01

    Here, we introduce a mass spectrometry-based analytical method and relevant technical details for dynamic cell respiration and CO2 labeling analysis. Such measurements can be utilized as additional information and constraints for model-based (13)C metabolic flux analysis. Dissolved dynamics of oxygen consumption and CO2 mass isotopomer evolution from (13)C-labeled tracer substrates through different cellular processes can be precisely measured on-line using a miniaturized reactor system equipped with a membrane-inlet mass spectrometer. The corresponding specific rates of physiologically relevant gases and CO2 mass isotopomers can be quantified within a short-term range based on the liquid-phase dynamics of dissolved fermentation gases.

  18. Laser microprobe mass spectrometry: Potential and limitations for inorganic and organic micro-analysis. Pt. 1

    International Nuclear Information System (INIS)

    Vaeck, I. van; Gijbels, R.

    1990-01-01

    Laser microprobe mass spectrometry (LMMS) employs a highly focused UV laser beam to ionise a microvolume in the order of 1 μm 3 . The ions produced are then mass-separated in a time-of-flight (TOF) or a Fourier Transform (FT) mass spectrometer. TOF LMMS allows element localisation, detailed speciation of inorganic substances and structural information of organic molecules. Quantitation is difficult. This paper focuses on instrumental aspects and inorganic analysis. Organic applications are treated in part II of this series. Selected examples illustrate that TOF LMMS is a valuable tool for the qualitative characterisation of micro-samples. Also, the applicability to the analysis with high spatial resolution is shown. The current technology and the prospects from the recent FTMS development are discussed. (orig.)

  19. Phytochemical analysis of Hibiscus caesius using high performance liquid chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Ain, Quratul; Naveed, Muhammad Na; Mumtaz, Abdul Samad; Farman, Muhammad; Ahmed, Iftikhar; Khalid, Nauman

    2015-09-01

    Various species in genus Hibiscus are traditionally known for their therapeutic attributes. The present study focused on the phytochemical analysis of a rather unexplored species Hibiscus caesius (H. caesius), using high-pressure liquid chromatography coupled with mass spectrometry (HPLC-MS). The analysis revealed five major compounds in the aqueous extract, viz. vanillic acid, protocatechoic acid, quercetin, quercetin glucoside and apigenin, being reported for the first time in H. caesius. Literature suggests that these compounds have important pharmacological traits such as anti-cancer, anti-inflammatory, anti-bacterial and hepatoprotective etc. however, this requires further pharmacological investigations at in vitro and in vivo scale. The above study concluded the medicinal potential of H. caesius.

  20. Quantitative analysis of abused drugs in physiological fluids by gas chromatography/chemical ionization mass spectrometry

    International Nuclear Information System (INIS)

    Foltz, R.L.

    1978-01-01

    Methods have been developed for quantitative analysis of commonly abused drugs in physiological fluids using gas chromatography/chemical ionization mass spectrometry. The methods are being evaluated in volunteer analytical and toxicological laboratories, and analytical manuals describing the methods are being prepared. The specific drug and metabolites included in this program are: Δ 9 -tetrahydrocannabinol, methadone, phencyclidine, methaqualone, morphine, amphetamine, methamphetamine, mescaline, 2,5-dimethoxy-4-methyl amphetamine, cocaine, benzoylecgonine, diazepam, and N-desmethyldiazepam. The current analytical methods utilize relatively conventional instrumentation and procedures, and are capable of measuring drug concentrations as low as 1 ng/ml. Various newer techniques such as sample clean-up by high performance liquid chromatography, separation by glass capillary chromatography, and ionization by negative ion chemical ionization are being investigated with respect to their potential for achieving higher sensitivity and specificity, as well as their ability to facilitate simultaneous analysis of more than one drug and metabolite. (Auth.)

  1. Sulphate analysis in uranium leach iron(III) chloride solutions by inductively coupled argon plasma spectrometry

    International Nuclear Information System (INIS)

    Nirdosh, I.; Lakhani, S.; Yunus, M.Z.M.

    1993-01-01

    Inductively coupled Argon Plasma Spectrometry is used for the indirect determination of sulphate in iron(III) chloride leach solution of Elliot Lake uranium ores via addition of a known amount of barium ions and analyzing for excess of barium. The ore contains ∼ 7 wt% pyrite, FeS 2 , as the major mineral which oxidizes to generate sulphate during leaching with Fe(III). The effects of pH, the concentrations of Fe(III) and chloride ions and for presence of ethanol in the test samples on the accuracy of analysis are studied. It is found that unlike the Rhodizonate method, removal of iron(III) from or addition of ethanol to the test sample prior to analysis are not required. Linear calibration curves are obtained. (author)

  2. The application of computer technique in routine neutron activation analysis using high resolution gamma ray spectrometry

    International Nuclear Information System (INIS)

    Szopa, Z.; Plejewska, M.; Staszelis, J.

    1982-01-01

    A full system of four computer programs for routine - qualitative and quantitative - neutron activation analysis (NAA) using high resolution gamma ray-spectrometry had been elaborated. The structure and possibilities of the ''data flow'' programs i.e. programs DIDPDP and DIDCDC, dedicated for fast and reliable ''off line'' data transfer between the buffer memory of the spectrometric line (9-track magnetic tape) and the fast access memory (disc) of the used computers PDP-11/45 and CYBER-73 had been presented. The structure and organization of the ''data processing'' programs i.e. programs SAWAPS and MAZYG had been presented as well. The utility and reliability of these programs in the case of the large-scale, routine NAA, exampled by analysis of filters with air polutants, had been tested and discussed. Programs are written mainly in FORTRAN. (author)

  3. Analytical developments in thermal ionization mass spectrometry for the isotopic analysis of very small amounts

    International Nuclear Information System (INIS)

    Mialle, S.

    2011-01-01

    In the framework of the French transmutation project of nuclear wastes, experiments consisted in the irradiation in a fast neutron reactor of few milligrams of isotopically enriched powders. Hence, the isotopic analysis of very small amount of irradiation products is one of the main issues. The aim of this study was to achieve analytical developments in thermal ionization mass spectrometry in order to accurately analyze these samples. Several axes were studied including the new total evaporation method, deposition techniques, electron multiplier potentialities and comparison between different isotope measurement techniques. Results showed that it was possible to drastically decrease the amounts needed for analysis, especially with Eu and Nd, while maintaining an uncertainty level in agreement with the project requirements. (author) [fr

  4. Comparison of public peak detection algorithms for MALDI mass spectrometry data analysis.

    Science.gov (United States)

    Yang, Chao; He, Zengyou; Yu, Weichuan

    2009-01-06

    In mass spectrometry (MS) based proteomic data analysis, peak detection is an essential step for subsequent analysis. Recently, there has been significant progress in the development of various peak detection algorithms. However, neither a comprehensive survey nor an experimental comparison of these algorithms is yet available. The main objective of this paper is to provide such a survey and to compare the performance of single spectrum based peak detection methods. In general, we can decompose a peak detection procedure into three consequent parts: smoothing, baseline correction and peak finding. We first categorize existing peak detection algorithms according to the techniques used in different phases. Such a categorization reveals the differences and similarities among existing peak detection algorithms. Then, we choose five typical peak detection algorithms to conduct a comprehensive experimental study using both simulation data and real MALDI MS data. The results of comparison show that the continuous wavelet-based algorithm provides the best average performance.

  5. Analysis of solvent dyes in refined petroleum products by electrospray ionization mass spectrometry

    Science.gov (United States)

    Rostad, C.E.

    2010-01-01

    Solvent dyes are used to color refined petroleum products to enable differentiation between gasoline, diesel, and jet fuels. Analysis for these dyes in the hydrocarbon product is difficult due to their very low concentrations in such a complex matrix. Flow injection analysis/electrospray ionization/mass spectrometry in both negative and positive mode was used to optimize ionization of ten typical solvent dyes. Samples of hydrocarbon product were analyzed under similar conditions. Positive electrospray ionization produced very complex spectra, which were not suitably specific for targeting only the dyes. Negative electrospray ionization produced simple spectra because aliphatic and aromatic moieties were not ionized. This enabled screening for a target dye in samples of hydrocarbon product from a spill.

  6. Mass Spectrometry and Fourier Transform Infrared Spectroscopy for Analysis of Biological Materials

    Energy Technology Data Exchange (ETDEWEB)

    Anderson, Timothy J. [Iowa State Univ., Ames, IA (United States)

    2014-12-01

    Time-of-flight mass spectrometry along with statistical analysis was utilized to study metabolic profiles among rats fed resistant starch (RS) diets. Fischer 344 rats were fed four starch diets consisting of 55% (w/w, dbs) starch. A control starch diet consisting of corn starch was compared against three RS diets. The RS diets were high-amylose corn starch (HA7), HA7 chemically modified with octenyl succinic anhydride, and stearic-acid-complexed HA7 starch. A subgroup received antibiotic treatment to determine if perturbations in the gut microbiome were long lasting. A second subgroup was treated with azoxymethane (AOM), a carcinogen. At the end of the eight week study, cecal and distal-colon contents samples were collected from the sacrificed rats. Metabolites were extracted from cecal and distal colon samples into acetonitrile. The extracts were then analyzed on an accurate-mass time-of-flight mass spectrometer to obtain their metabolic profile. The data were analyzed using partial least-squares discriminant analysis (PLS-DA). The PLS-DA analysis utilized a training set and verification set to classify samples within diet and treatment groups. PLS-DA could reliably differentiate the diet treatments for both cecal and distal colon samples. The PLS-DA analyses of the antibiotic and no antibiotic treated subgroups were well classified for cecal samples and modestly separated for distal-colon samples. PLS-DA analysis had limited success separating distal colon samples for rats given AOM from those not treated; the cecal samples from AOM had very poor classification. Mass spectrometry profiling coupled with PLS-DA can readily classify metabolite differences among rats given RS diets.

  7. 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

  8. Applications of inorganic mass spectrometry in metal analysis of high-tech industry

    International Nuclear Information System (INIS)

    Ling Yongjian; Wang Shimin; Li Peiling; Chen Lizhen

    2007-01-01

    The metals in the nature are closely related to the progress of human culture and economic activities. Various kinds of metals are continuously being applied to new processes and products. During the effect by biogeochemical cycle, metals were released to environmental compartments, such as air, water, soil, and living organisms. The deficiency in knowledge, poor management, greedy, and bad intention usually leads to serious environmental pollution, eco-environment damage, and human poisoning. Effective analysis of metal concentrations and species during economic activities and eco-environment is an important research and survey subject. Internationally, the establishment of high-tech industrial park has become the major means to simultaneously improve living quality and broaden economic activity. High-tech industry uses metals. It is mandatory to control the distribution of metals in feed, process, product, waste, environment, and the life-cycle. This report is based on our experience with inorganic mass spectrometry focusing on the use of secondary ion mass spectrometry (SIMS) and inductively-coupled mass spectrometry (ICP-MS) in metal analysis of high-tech industrial parts. The report includes (1) The use of SIMS for analyzing impurity in depth and on surface demonstrates the importance of integrating trace metal, depth profile, micro-area, and surface analyses. (2) Survey ambient heavy metals (As, Be, Cd, Dr, Hg, Mn, Ni and Pb) around industrial parks and compare the findings to stack heavy metals. The results demonstrate that ICP-MS is indispensable to help reveal heavy metal distribution in industrial park ambient air and clarify suspected polluting sources. (3) Research and develop analytical method to determine metal impurities (Na, K, Mg, Ca, Cu, Fe, Mn, Li and Al) in photoresist. The method uses a novel nitric acid digestion technique to convert photoresist into carbon dioxide and water, followed by ICP-MS analysis of high-purity nitric acid recovery

  9. Mass spectrometry analysis of etch products from CR-39 plastic irradiated by heavy ions

    Science.gov (United States)

    Kodaira, S.; Nanjo, D.; Kawashima, H.; Yasuda, N.; Konishi, T.; Kurano, M.; Kitamura, H.; Uchihori, Y.; Naka, S.; Ota, S.; Ideguchi, Y.; Hasebe, N.; Mori, Y.; Yamauchi, T.

    2012-09-01

    As a feasibility study, gas chromatography-mass spectrometry (GC-MS) and matrix-assisted laser desorption ionization-mass spectrometry (MALDI-MS) have been applied to analyze etch products of CR-39 plastic (one of the most frequently used solid states nuclear track detector) for the understanding of track formation and etching mechanisms by heavy ion irradiation. The etch products of irradiated CR-39 dissolved in sodium hydroxide solution (NaOH) contain radiation-induced fragments. For the GC-MS analysis, we found peaks of diethylene glycol (DEG) and a small but a definitive peak of ethylene glycol (EG) in the etch products from CR-39 irradiated by 60 MeV N ion beams. The etch products of unirradiated CR-39 showed a clear peak of DEG, but no other significant peaks were found. DEG is known to be released from the CR-39 molecule as a fragment by alkaline hydrolysis reaction of the polymer. We postulate that EG was formed as a result of the breaking of the ether bond (C-O-C) of the DEG part of the CR-39 polymer by the irradiation. The mass distribution of polyallylalcohol was obtained from the etch products from irradiated and unirradiated CR-39 samples by MALDI-MS analysis. Polyallylalcohol, with the repeating mass interval of m/z = 58 Da (dalton) between m/z = 800 and 3500, was expected to be produced from CR-39 by alkaline hydrolysis. We used IAA as a matrix to assist the ionization of organic analyte in MALDI-MS analysis and found that peaks from IAA covered mass spectrum in the lower m/z region making difficult to identify CR-39 fragment peaks which were also be seen in the same region. The mass spectrometry analysis using GC-MS and MALDI-MS will be powerful tools to investigate the radiation-induced polymeric fragments and helping to understand the track formation mechanism in CR-39 by heavy ions.

  10. In Cell Footprinting Coupled with Mass Spectrometry for the Structural Analysis of Proteins in Live Cells.

    Science.gov (United States)

    Espino, Jessica A; Mali, Vishaal S; Jones, Lisa M

    2015-08-04

    Protein footprinting coupled with mass spectrometry has become a widely used tool for the study of protein-protein and protein-ligand interactions and protein conformational change. These methods provide residue-level analysis on protein interaction sites and have been successful in studying proteins in vitro. The extension of these methods for in cell footprinting would open an avenue to study proteins that are not amenable for in vitro studies and would probe proteins in their native environment. Here we describe the application of an oxidative-based footprinting approach inside cells in which hydroxyl radicals are used to oxidatively modify proteins. Mass spectrometry is used to detect modification sites and to calculate modification levels. The method is probing biologically relevant proteins in live cells, and proteins in various cellular compartments can be oxdiatively modified. Several different amino acid residues are modified making the method a general labeling strategy for the study of a variety of proteins. Further, comparison of the extent of oxidative modification with solvent accessible surface area reveals the method successfully probes solvent accessibility. This marks the first time protein footprinting has been performed in live cells.

  11. Automated Morphological and Morphometric Analysis of Mass Spectrometry Imaging Data: Application to Biomarker Discovery

    Science.gov (United States)

    Picard de Muller, Gaël; Ait-Belkacem, Rima; Bonnel, David; Longuespée, Rémi; Stauber, Jonathan

    2017-12-01

    Mass spectrometry imaging datasets are mostly analyzed in terms of average intensity in regions of interest. However, biological tissues have different morphologies with several sizes, shapes, and structures. The important biological information, contained in this highly heterogeneous cellular organization, could be hidden by analyzing the average intensities. Finding an analytical process of morphology would help to find such information, describe tissue model, and support identification of biomarkers. This study describes an informatics approach for the extraction and identification of mass spectrometry image features and its application to sample analysis and modeling. For the proof of concept, two different tissue types (healthy kidney and CT-26 xenograft tumor tissues) were imaged and analyzed. A mouse kidney model and tumor model were generated using morphometric - number of objects and total surface - information. The morphometric information was used to identify m/z that have a heterogeneous distribution. It seems to be a worthwhile pursuit as clonal heterogeneity in a tumor is of clinical relevance. This study provides a new approach to find biomarker or support tissue classification with more information. [Figure not available: see fulltext.

  12. Diagnostic prediction of renal failure from blood serum analysis by FTIR spectrometry and chemometrics

    Science.gov (United States)

    Khanmohammadi, Mohammdreza; Ghasemi, Keyvan; Garmarudi, Amir Bagheri; Ramin, Mehdi

    2015-02-01

    A new diagnostic approach based on Attenuated Total Reflectance-Fourier Transform Infrared (ATR-FTIR) spectrometry and classification algorithm has been introduced which provides a rapid, reliable, and easy way to perform blood test for the diagnosis of renal failure. Blood serum samples from 35 renal failure patients and 40 healthy persons were analyzed by ATR-FTIR spectrometry. The resulting data was processed by Quadratic Discriminant Analysis (QDA) and QDA combined with simple filtered method. Spectroscopic studies were performed in 900-2000 cm-1 spectral region with 3.85 cm-1 data space. Results showed 93.33% and 100% of accuracy for QDA and filter-QDA models, respectively. In the first step, 30 samples were applied to construct the model. In order to modify the capability of QDA in prediction of test samples, filter-based feature selection methods were applied. It was found that the filtered spectra coupled with QDA could correctly predict the test samples in most of the cases.

  13. Mass Spectrometry-Based Proteomics for the Analysis of Chromatin Structure and Dynamics

    Directory of Open Access Journals (Sweden)

    Monica Soldi

    2013-03-01

    Full Text Available Chromatin is a highly structured nucleoprotein complex made of histone proteins and DNA that controls nearly all DNA-dependent processes. Chromatin plasticity is regulated by different associated proteins, post-translational modifications on histones (hPTMs and DNA methylation, which act in a concerted manner to enforce a specific “chromatin landscape”, with a regulatory effect on gene expression. Mass Spectrometry (MS has emerged as a powerful analytical strategy to detect histone PTMs, revealing interplays between neighbouring PTMs and enabling screens for their readers in a comprehensive and quantitative fashion. Here we provide an overview of the recent achievements of state-of-the-art mass spectrometry-based proteomics for the detailed qualitative and quantitative characterization of histone post-translational modifications, histone variants, and global interactomes at specific chromatin regions. This synopsis emphasizes how the advances in high resolution MS, from “Bottom Up” to “Top Down” analysis, together with the uptake of quantitative proteomics methods by chromatin biologists, have made MS a well-established method in the epigenetics field, enabling the acquisition of original information, highly complementary to that offered by more conventional, antibody-based, assays.

  14. Portable Dew Point Mass Spectrometry System for Real-Time Gas and Moisture Analysis

    Science.gov (United States)

    Arkin, C.; Gillespie, Stacey; Ratzel, Christopher

    2010-01-01

    A portable instrument incorporates both mass spectrometry and dew point measurement to provide real-time, quantitative gas measurements of helium, nitrogen, oxygen, argon, and carbon dioxide, along with real-time, quantitative moisture analysis. The Portable Dew Point Mass Spectrometry (PDP-MS) system comprises a single quadrupole mass spectrometer and a high vacuum system consisting of a turbopump and a diaphragm-backing pump. A capacitive membrane dew point sensor was placed upstream of the MS, but still within the pressure-flow control pneumatic region. Pressure-flow control was achieved with an upstream precision metering valve, a capacitance diaphragm gauge, and a downstream mass flow controller. User configurable LabVIEW software was developed to provide real-time concentration data for the MS, dew point monitor, and sample delivery system pressure control, pressure and flow monitoring, and recording. The system has been designed to include in situ, NIST-traceable calibration. Certain sample tubing retains sufficient water that even if the sample is dry, the sample tube will desorb water to an amount resulting in moisture concentration errors up to 500 ppm for as long as 10 minutes. It was determined that Bev-A-Line IV was the best sample line to use. As a result of this issue, it is prudent to add a high-level humidity sensor to PDP-MS so such events can be prevented in the future.

  15. Ultratrace analysis of plutonium in environmental samples by resonance ionization mass spectrometry (RIMS)

    International Nuclear Information System (INIS)

    Trautmann, N.; Erdmann, N.; Gruening, C.; Kratz, J. V.; Waldek, A.; Huber, G.; Nunnemann, M.; Passler, G.

    2000-01-01

    Plutonium is present in the environment mainly as a result of global fallout from nuclear weapons tests, satellite and reactor accidents as well as releases from nuclear facilities. Sensitive and fast detection methods are required for risk assessment, low-level surveillance of the environment, personnel dose monitoring, studies of biological effects and investigations of the migration behavior of plutonium. Furthermore, the isotopic composition is of interest to get information from what source the plutonium contamination originated. Alpha-spectroscopy is most frequently used for the determination of trace amounts of plutonium in the environment with the disadvantage that the detection sensitivity depends on the half-life of the isotope to be measured and that there are limitations in the isotopic resolution. Conventional mass spectrometry may suffer from isobaric interferences. Therefore, in the last years resonant laser ionization mass spectrometry (RIMS) has been explored as an alternative for ultratrace analysis of plutonium. This method provides a high element and isotope selectivity and a good overall efficiency, resulting in a detection limit of ∼10 6 atoms (∼0.4 fg). RIMS meets also the requirements of a low background and a short measuring time (1-2 h)

  16. Mass Spectrometry Based Proteomic Analysis of Salivary Glands of Urban Malaria Vector Anopheles stephensi

    Directory of Open Access Journals (Sweden)

    Sonam Vijay

    2014-01-01

    Full Text Available Salivary gland proteins of Anopheles mosquitoes offer attractive targets to understand interactions with sporozoites, blood feeding behavior, homeostasis, and immunological evaluation of malaria vectors and parasite interactions. To date limited studies have been carried out to elucidate salivary proteins of An. stephensi salivary glands. The aim of the present study was to provide detailed analytical attributives of functional salivary gland proteins of urban malaria vector An. stephensi. A proteomic approach combining one-dimensional electrophoresis (1DE, ion trap liquid chromatography mass spectrometry (LC/MS/MS, and computational bioinformatic analysis was adopted to provide the first direct insight into identification and functional characterization of known salivary proteins and novel salivary proteins of An. stephensi. Computational studies by online servers, namely, MASCOT and OMSSA algorithms, identified a total of 36 known salivary proteins and 123 novel proteins analysed by LC/MS/MS. This first report describes a baseline proteomic catalogue of 159 salivary proteins belonging to various categories of signal transduction, regulation of blood coagulation cascade, and various immune and energy pathways of An. stephensi sialotranscriptome by mass spectrometry. Our results may serve as basis to provide a putative functional role of proteins in concept of blood feeding, biting behavior, and other aspects of vector-parasite host interactions for parasite development in anopheline mosquitoes.

  17. A micro-fluidic sub-microliter sample introduction system for direct analysis of Chinese rice wine by inductively coupled plasma mass spectrometry using external aqueous calibration

    Energy Technology Data Exchange (ETDEWEB)

    Cheng, Heyong [Institute of Microanalytical Systems, Department of Chemistry, Zhejiang University, Hangzhou, 310027 (China); College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou, 310036 (China); Liu, Jinhua [College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou, 310036 (China); Xu, Zigang [Institute of Analytical and Applied Chemistry, Department of Chemistry, Zhejiang University, Hangzhou, 310027 (China); Yin, Xuefeng, E-mail: yinxf@zju.edu.cn [Institute of Microanalytical Systems, Department of Chemistry, Zhejiang University, Hangzhou, 310027 (China); College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou, 310036 (China)

    2012-07-15

    A microfluidic sub-microliter sample introducing system was developed for direct analysis of Chinese rice wine by inductively coupled plasma mass spectrometry (ICP-MS). It consisted of a microfluidic chip integrating variable-volume sampling channels (0.1-0.8 {mu}L), an eight-way multi-functional valve used in flow injection analysis (FIA), a syringe pump and a peristaltic pump of the Ar ICP-MS instrument. Three solutions, i.e., 15, 40 and 100 g L{sup -1} glucose in 20% ethanol were used to simulate Chinese rice wine of the dry type, the semidry type and the semisweet type, each. The effects of their volume introduced into ICP-MS on the plasma stability and ICP-MS intensities were studied. The experimental results showed that neither alteration of plasma stability nor carbon deposition was observed when the sampling volume of 20% ethanol containing 100 g L{sup -1} glucose was downscaled to 0.8 {mu}L. Further reducing the sampling volume to 0.4 {mu}L, no significant difference between the intensities of multi-element standard prepared in three simulated Chinese rice wine matrices and those in aqueous solution was observed. It indicated no negative effect of Chinese rice wine matrix on the ICP-MS intensities. A sampling volume of 0.4 {mu}L was considered to be a good compromise between sensitivity and matrix effect. The flow rate of the carrier was chosen as 20 {mu}L min{sup -1} for obtaining peaks with the highest peak height within the shortest time. Based on these observations, a microflow injection ({mu}FI) method for the direct determination of cadmium and lead in Chinese rice wine by ICP-MS using an external aqueous calibration was developed. The sample throughput was 45 h{sup -1} with the detection limit of 19.8 and 10.4 ng L{sup -1} for Cd and Pb, respectively. The contents of Cd and Pb in 10 Chinese rice wine samples were measured. The results agreed well with those determined by ICP-MS with the conventional sampling system after microwave assisted digestion

  18. A micro-fluidic sub-microliter sample introduction system for direct analysis of Chinese rice wine by inductively coupled plasma mass spectrometry using external aqueous calibration

    International Nuclear Information System (INIS)

    Cheng, Heyong; Liu, Jinhua; Xu, Zigang; Yin, Xuefeng

    2012-01-01

    A microfluidic sub-microliter sample introducing system was developed for direct analysis of Chinese rice wine by inductively coupled plasma mass spectrometry (ICP-MS). It consisted of a microfluidic chip integrating variable-volume sampling channels (0.1–0.8 μL), an eight-way multi-functional valve used in flow injection analysis (FIA), a syringe pump and a peristaltic pump of the Ar ICP-MS instrument. Three solutions, i.e., 15, 40 and 100 g L −1 glucose in 20% ethanol were used to simulate Chinese rice wine of the dry type, the semidry type and the semisweet type, each. The effects of their volume introduced into ICP-MS on the plasma stability and ICP-MS intensities were studied. The experimental results showed that neither alteration of plasma stability nor carbon deposition was observed when the sampling volume of 20% ethanol containing 100 g L −1 glucose was downscaled to 0.8 μL. Further reducing the sampling volume to 0.4 μL, no significant difference between the intensities of multi-element standard prepared in three simulated Chinese rice wine matrices and those in aqueous solution was observed. It indicated no negative effect of Chinese rice wine matrix on the ICP-MS intensities. A sampling volume of 0.4 μL was considered to be a good compromise between sensitivity and matrix effect. The flow rate of the carrier was chosen as 20 μL min −1 for obtaining peaks with the highest peak height within the shortest time. Based on these observations, a microflow injection (μFI) method for the direct determination of cadmium and lead in Chinese rice wine by ICP-MS using an external aqueous calibration was developed. The sample throughput was 45 h −1 with the detection limit of 19.8 and 10.4 ng L −1 for Cd and Pb, respectively. The contents of Cd and Pb in 10 Chinese rice wine samples were measured. The results agreed well with those determined by ICP-MS with the conventional sampling system after microwave assisted digestion. The recoveries of three

  19. MEDEA: A multi element detector array for gamma ray and light charged particle detection at the LNS-Catania

    International Nuclear Information System (INIS)

    Migneco, E.; Agodi, C.; Alba, R.; Coniglione, R.; Del Zoppo, A.; Finocchiaro, P.; Maiolino, C.; Piattelli, P.; Raia, G.; Sapienza, P.; Bellia, G.

    1992-01-01

    A 4π highly granular Multi Element Detector Array (MEDEA) for γ-rays and light charged particles is described. Its basic configuration consists of 180 barium fluoride scintillator crystals, arranged in the shape of a ball, plus a forward angle wall of 120 phoswich detectors. The inner radius of the ball (22 cm) and the distance of the wall from the target (55 cm) allow the placement of other detectors in the inner volume. The whole detection system operates under vacuum inside a large scattering chamber. Dedicated electronics has been designed and realized. It includes a powerful hardware second level trigger and preanalysis system, which allows on-line event selection, and a modular VME-bus based data acquisition system. In-beam performances of the system are also described. (orig.)

  20. Development and characterization of multi-element doped hydroxyapatite bioceramic coatings on metallic implants for orthopedic applications

    International Nuclear Information System (INIS)

    Furko, M.; Havasi, V.; Kónya, Z.; Grünewald, D.; Detsch, R.; Boccaccini, A.R.; Balázsi, C.

    2018-01-01

    Multi-element modified bioactive hydroxyapatite bioceramic (mHAp) coatings were successfully developed onto surgical grade titanium alloy material (Ti6Al4V). The coatings were prepared by pulse current deposition from electrolyte containing adequate amounts of calcium nitrate and ammonium dihydrogen phosphate at 70C. The pure HAp layer was doped and co-deposited with Ag, Zn, Mg, Sr ions. The biocompatible properties of layers were investigated by seeding osteoblast-like MG-63 cells onto the samples’ surface. The biocompatible measurements revealed enhanced bioactivity of modified HAp compared to uncoated implant materials and pure bioceramic coating. The morphology and structure of coatings and cells were characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) as well as FT-IR and XRD measurements. The biodegradable properties of samples were investigated by electrochemical potentiodynamic measurements. [es

  1. A positive and multi-element conserving time stepping scheme for biogeochemical processes in marine ecosystem models

    Science.gov (United States)

    Radtke, H.; Burchard, H.

    2015-01-01

    In this paper, an unconditionally positive and multi-element conserving time stepping scheme for systems of non-linearly coupled ODE's is presented. These systems of ODE's are used to describe biogeochemical transformation processes in marine ecosystem models. The numerical scheme is a positive-definite modification of the Runge-Kutta method, it can have arbitrarily high order of accuracy and does not require time step adaption. If the scheme is combined with a modified Patankar-Runge-Kutta method from Burchard et al. (2003), it also gets the ability to solve a certain class of stiff numerical problems, but the accuracy is restricted to second-order then. The performance of the new scheme on two test case problems is shown.

  2. Contribution of bulk mass spectrometry isotopic analysis to characterization of materials in the framework of CMX-4

    International Nuclear Information System (INIS)

    Kuchkin, A.; Stebelkov, V.; Zhizhin, K.; Lierse von Gostomski, Ch.; Kardinal, Ch.; Loi, E.; Keegan, E.; Kristo, M.J.

    2018-01-01

    Seven laboratories used the results of bulk uranium isotopic analysis by either inductively coupled plasma mass spectrometry (ICP-MS) or thermal ionization mass spectrometry (TIMS) for characterization of the samples in the Nuclear Forensic International Technical Working Group fourth international collaborative material exercise, CMX-4. Comparison of the measured isotopic compositions of uranium in three exercise samples is implemented for identifying any differences or similarities between the samples. The role of isotopic analyses in the context of a real nuclear forensic investigation is discussed. Several limitations in carrying out ICP-MS or TIMS analysis in CMX-4 are noted. (author)

  3. CLMSVault: A Software Suite for Protein Cross-Linking Mass-Spectrometry Data Analysis and Visualization.

    Science.gov (United States)

    Courcelles, Mathieu; Coulombe-Huntington, Jasmin; Cossette, Émilie; Gingras, Anne-Claude; Thibault, Pierre; Tyers, Mike

    2017-07-07

    Protein cross-linking mass spectrometry (CL-MS) enables the sensitive detection of protein interactions and the inference of protein complex topology. The detection of chemical cross-links between protein residues can identify intra- and interprotein contact sites or provide physical constraints for molecular modeling of protein structure. Recent innovations in cross-linker design, sample preparation, mass spectrometry, and software tools have significantly improved CL-MS approaches. Although a number of algorithms now exist for the identification of cross-linked peptides from mass spectral data, a dearth of user-friendly analysis tools represent a practical bottleneck to the broad adoption of the approach. To facilitate the analysis of CL-MS data, we developed CLMSVault, a software suite designed to leverage existing CL-MS algorithms and provide intuitive and flexible tools for cross-platform data interpretation. CLMSVault stores and combines complementary information obtained from different cross-linkers and search algorithms. CLMSVault provides filtering, comparison, and visualization tools to support CL-MS analyses and includes a workflow for label-free quantification of cross-linked peptides. An embedded 3D viewer enables the visualization of quantitative data and the mapping of cross-linked sites onto PDB structural models. We demonstrate the application of CLMSVault for the analysis of a noncovalent Cdc34-ubiquitin protein complex cross-linked under different conditions. CLMSVault is open-source software (available at https://gitlab.com/courcelm/clmsvault.git ), and a live demo is available at http://democlmsvault.tyerslab.com/ .

  4. Rapid discrimination of bergamot essential oil by paper spray mass spectrometry and chemometric analysis.

    Science.gov (United States)

    Taverna, Domenico; Di Donna, Leonardo; Mazzotti, Fabio; Tagarelli, Antonio; Napoli, Anna; Furia, Emilia; Sindona, Giovanni

    2016-09-01

    A novel approach for the rapid discrimination of bergamot essential oil from other citrus fruits oils is presented. The method was developed using paper spray mass spectrometry (PS-MS) allowing for a rapid molecular profiling coupled with a statistic tool for a precise and reliable discrimination between the bergamot complex matrix and other similar matrices, commonly used for its reconstitution. Ambient mass spectrometry possesses the ability to record mass spectra of ordinary samples, in their native environment, without sample preparation or pre-separation by creating ions outside the instrument. The present study reports a PS-MS method for the determination of oxygen heterocyclic compounds such as furocoumarins, psoralens and flavonoids present in the non-volatile fraction of citrus fruits essential oils followed by chemometric analysis. The volatile fraction of Bergamot is one of the most known and fashionable natural products, which found applications in flavoring industry as ingredient in beverages and flavored foodstuff. The development of the presented method employed bergamot, sweet orange, orange, cedar, grapefruit and mandarin essential oils. PS-MS measurements were carried out in full scan mode for a total run time of 2 min. The capability of PS-MS profiling to act as marker for the classification of bergamot essential oils was evaluated by using multivariate statistical analysis. Two pattern recognition techniques, linear discriminant analysis and soft independent modeling of class analogy, were applied to MS data. The cross-validation procedure has shown excellent results in terms of the prediction ability because both models have correctly classified all samples for each category. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  5. X-ray fluorescence spectrometry and related techniques an introduction

    CERN Document Server

    Margui, Eva

    2013-01-01

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

  6. Quantitative Analysis of Tetramethylenedisulfotetramine ("Tetramine") Spiked into Beverages by Liquid Chromatography Tandem Mass Spectrometry with Validation by Gas Chromatography Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Owens, J; Hok, S; Alcaraz, A; Koester, C

    2008-11-13

    Tetramethylenedisulfotetramine, commonly known as tetramine, is a highly neurotoxic rodenticide (human oral LD{sub 50} = 0.1 mg/kg) used in hundreds of deliberate food poisoning events in China. Here we describe a method for quantitation of tetramine spiked into beverages, including milk, juice, tea, cola, and water and cleaned up by C8 solid phase extraction and liquid-liquid extraction. Quantitation by high performance liquid chromatography tandem mass spectrometry (LC/MS/MS) was based upon fragmentation of m/z 347 to m/z 268. The method was validated by gas chromatography mass spectrometry (GC/MS) operated in SIM mode for ions m/z 212, 240, and 360. The limit of quantitation was 0.10 {micro}g/mL by LC/MS/MS versus 0.15 {micro}g/mL for GC/MS. Fortifications of the beverages at 2.5 {micro}g/mL and 0.25 {micro}g/mL were recovered ranging from 73-128% by liquid-liquid extraction for GC/MS analysis, 13-96% by SPE and 10-101% by liquid-liquid extraction for LC/MS/MS analysis.

  7. Quantitative Analysis of Tetramethylenedisulfotetramine ('Tetramine') Spiked into Beverages by Liquid Chromatography Tandem Mass Spectrometry with Validation by Gas Chromatography Mass Spectrometry

    International Nuclear Information System (INIS)

    Owens, J.; Hok, S.; Alcaraz, A.; Koester, C.

    2008-01-01

    Tetramethylenedisulfotetramine, commonly known as tetramine, is a highly neurotoxic rodenticide (human oral LD 50 = 0.1 mg/kg) used in hundreds of deliberate food poisoning events in China. Here we describe a method for quantitation of tetramine spiked into beverages, including milk, juice, tea, cola, and water and cleaned up by C8 solid phase extraction and liquid-liquid extraction. Quantitation by high performance liquid chromatography tandem mass spectrometry (LC/MS/MS) was based upon fragmentation of m/z 347 to m/z 268. The method was validated by gas chromatography mass spectrometry (GC/MS) operated in SIM mode for ions m/z 212, 240, and 360. The limit of quantitation was 0.10 (micro)g/mL by LC/MS/MS versus 0.15 (micro)g/mL for GC/MS. Fortifications of the beverages at 2.5 (micro)g/mL and 0.25 (micro)g/mL were recovered ranging from 73-128% by liquid-liquid extraction for GC/MS analysis, 13-96% by SPE and 10-101% by liquid-liquid extraction for LC/MS/MS analysis.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-07-15

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

  9. Analysis of O-Glycopeptides by Acetone Enrichment and Capillary Electrophoresis-Mass Spectrometry.

    Science.gov (United States)

    Mancera-Arteu, Montserrat; Giménez, Estela; Benavente, Fernando; Barbosa, José; Sanz-Nebot, Victòria

    2017-11-03

    Acetone precipitation was evaluated as a rapid, simple, low-cost, and efficient method for the selective purification of O-glycopeptides from enzymatic digests of glycoproteins. Ovalbumin (OVA), human and bovine α 1 -acid glycoprotein (hAGP and bAGP), human apolipoprotein C-III (APO-C3), and recombinant human erythropoietin (rhEPO) were used to obtain enzymatic digests with a broad and varied set of peptides, N-glycopeptides, and O-glycopeptides. After digestion and before capillary electrophoresis mass spectrometry (CE-MS) analysis, the amount of ice-cold acetone added to the digests was optimized to maximize recoveries of O-glycopeptides. Furthermore, the different behavior of peptides, N- and O-glycopeptides was explained by studying with multivariate data analysis methods the influence of several physicochemical parameters and properties related to their composition and structure. Principal component analysis (PCA) and, afterward, partial least-squares discriminant analysis (PLS-DA) were used to identify the most significant variables and their importance to differentiate between peptides, N-glycopeptides and O-glycopeptides, or within these classes. This information was useful to understand precipitation of these compounds after addition of acetone and for the selection of the optimal conditions for purification of specific O-glycopeptide biomarkers. Special attention was paid to O 126 -glycopeptide glycoforms of rhEPO because of their applicability in biopharmaceutical quality control and doping analysis.

  10. Rapid Analysis of Corni fructus Using Paper Spray-Mass Spectrometry.

    Science.gov (United States)

    Guo, Yuan; Gu, Zhixin; Liu, Xuemei; Liu, Jingjing; Ma, Ming; Chen, Bo; Wang, Liping

    2017-07-01

    Paper spray-mass spectrometry (PS-MS) is a kind of ambient MS technique for the rapid analysis of samples. Corni fructus has been widely used in traditional Chinese compound preparations and healthy food. However, a number of counterfeits of Corni fructus, such as Crataegi fructus, Lycii fructus, and grape skin are illegally sold in crude herb markets. Therefore, the development of a rapid and high-throughput quality evaluation method is important for ensuring the effectiveness and safety of the crude materials of Corni fructus. To develop PS-MS chemical profiles and a semi-quantitative method of Corni fructus for quality assessment and control, and species distinction of Corni fructus. Both positive and negative ion PS-MS chemical profiles were constructed for species distinction. The statistical analysis of the chemical profiles was accomplished by principal component analysis (PCA). Rapid semi-quantitative analysis of loganin and morroniside in the extracts of Corni fructus were accomplished by PS-MS. The profiles of the Corni fructus and Crataegi fructus samples were clearly clustered into two categories. The limit of quantification (LOQ) in the semi-quantitative analysis was 6 μg/mL and 5.6 μg/mL for loganin and morroniside, respectively. PS-MS is a simple, rapid, and high-throughput method for the quality control and species distinction of Corni fructus. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  11. Rapid quality assessment of Radix Aconiti Preparata using direct analysis in real time mass spectrometry.

    Science.gov (United States)

    Zhu, Hongbin; Wang, Chunyan; Qi, Yao; Song, Fengrui; Liu, Zhiqiang; Liu, Shuying

    2012-11-08

    This study presents a novel and rapid method to identify chemical markers for the quality control of Radix Aconiti Preparata, a world widely used traditional herbal medicine. In the method, the samples with a fast extraction procedure were analyzed using direct analysis in real time mass spectrometry (DART MS) combined with multivariate data analysis. At present, the quality assessment approach of Radix Aconiti Preparata was based on the two processing methods recorded in Chinese Pharmacopoeia for the purpose of reducing the toxicity of Radix Aconiti and ensuring its clinical therapeutic efficacy. In order to ensure the safety and effectivity in clinical use, the processing degree of Radix Aconiti should be well controlled and assessed. In the paper, hierarchical cluster analysis and principal component analysis were performed to evaluate the DART MS data of Radix Aconiti Preparata samples in different processing times. The results showed that the well processed Radix Aconiti Preparata, unqualified processed and the raw Radix Aconiti could be clustered reasonably corresponding to their constituents. The loading plot shows that the main chemical markers having the most influence on the discrimination amongst the qualified and unqualified samples were mainly some monoester diterpenoid aconitines and diester diterpenoid aconitines, i.e. benzoylmesaconine, hypaconitine, mesaconitine, neoline, benzoylhypaconine, benzoylaconine, fuziline, aconitine and 10-OH-mesaconitine. The established DART MS approach in combination with multivariate data analysis provides a very flexible and reliable method for quality assessment of toxic herbal medicine. Copyright © 2012 Elsevier B.V. All rights reserved.

  12. Sulfur analysis by inductively coupled plasma-mass spectrometry: A review

    Energy Technology Data Exchange (ETDEWEB)

    Giner Martínez-Sierra, J.; Galilea San Blas, O.; Marchante Gayón, J.M.; García Alonso, J.I., E-mail: jiga@uniovi.es

    2015-06-01

    In recent years the number of applications of sulfur (S) analysis using inductively coupled plasma mass spectrometry (ICP-MS) as detector has increased significantly. In this article we describe in some depth the application of ICP-MS for S analysis with emphasis placed on the sulfur-specific detection by hyphenated techniques such as LC, GC, CE and LA coupled on-line to ICP-MS. The different approaches available for sulfur isotope ratio measurements by ICP-MS are also detailed. Particular attention has been paid to the quantification of peptides/proteins and the analysis of metallopeptides/metalloproteins via sulfur by LC–ICP-MS. Likewise, the speciation analysis of metal-based pharmaceuticals and metallodrugs and non-metal selective detection of pharmaceuticals via S are highlighted. Labeling procedures for metabolic applications are also included. Finally, the measurement of natural variations in S isotope composition with multicollector ICP-MS instruments is also covered in this review. - Highlights: • Emphasis placed on the sulfur-specific detection by chromatographic techniques coupled on-line to ICP-MS. • Different instrumental approaches available for sulfur measurements by ICP-MS. • Quantification of proteins and the analysis of metalloproteins via sulfur by LC-ICP-MS. • Labelling procedures for metabolic applications are also included. • The measurement of natural variations in S isotope composition with multicollector ICP-MS.

  13. Trace Analysis of Irradiated Granite Samples from Hiroshima by Laser Ablation Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    Amr, M.A.; Helal, N.F.; Zahran, N.F.; Becker, J.S.; Pickhardt, C.; Dietze, H.J.

    1999-01-01

    Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is widely accepted as a rapid and sensitive technique for trace elemental analysis of solid materials and for local analysis of inhomogeneous materials (such as geological samples). Due to its direct solid sample analysis capability, LA-ICP-MS (using a quadrupole based ICP-MS and at the Research Center Juelich developed laser ablation system: Nd-YAG-laser, 226 nm, 10 Hz and 5 ns) is applied for the analysis of geological (granite) samples from Hiroshima. In order to prepare homogeneous targets, these samples were melted together with a lithium-borate mixture in a muffle furnace at 1050 degree c. Furthermore, for investigating of matrix effects the powder of these samples is mixed with graphite and pressed as targets for laser ablation. The quantification of the analysis results was carried out using granite (GM) as standard reference material. The relative sensitivity coefficients (RSCs) for most elements, which were determined for correction of the measured values, varied between 0.3 and 3

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

    International Nuclear Information System (INIS)

    Camayd Viera, Ivette; Robaina Jimenez, Zoe; Contreras Roura, Jiovanna

    2011-01-01

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

  15. Specter: linear deconvolution for targeted analysis of data-independent acquisition mass spectrometry proteomics.

    Science.gov (United States)

    Peckner, Ryan; Myers, Samuel A; Jacome, Alvaro Sebastian Vaca; Egertson, Jarrett D; Abelin, Jennifer G; MacCoss, Michael J; Carr, Steven A; Jaffe, Jacob D

    2018-05-01

    Mass spectrometry with data-independent acquisition (DIA) is a promising method to improve the comprehensiveness and reproducibility of targeted and discovery proteomics, in theory by systematically measuring all peptide precursors in a biological sample. However, the analytical challenges involved in discriminating between peptides with similar sequences in convoluted spectra have limited its applicability in important cases, such as the detection of single-nucleotide polymorphisms (SNPs) and alternative site localizations in phosphoproteomics data. We report Specter (https://github.com/rpeckner-broad/Specter), an open-source software tool that uses linear algebra to deconvolute DIA mixture spectra directly through comparison to a spectral library, thus circumventing the problems associated with typical fragment-correlation-based approaches. We validate the sensitivity of Specter and its performance relative to that of other methods, and show that Specter is able to successfully analyze cases involving highly similar peptides that are typically challenging for DIA analysis methods.

  16. Several experimental applications of gamma ray spectrometry on the analysis of uranium compounds

    International Nuclear Information System (INIS)

    Korob, Ricardo O.; Blasiyh Nuno, Guillermo A.

    2002-01-01

    Several experimental applications of gamma ray spectrometry on the analysis of uranium compounds and materials containing it are studied. Special attention is devoted to the correlation between experimental spectra and the decay chains of 235 U and 238 U contained in the analyzed samples. The following applications are discussed: enrichment determination without using calibration standards, determination of uranium concentration, intensities of the gamma rays emitted by the nuclides present in the decay chains of study and the activity of such nuclides. Because of its importance, detailed discussion about the former one is shown. In addition, preliminary results regarding the emission probabilities of the most important gamma rays of 234m Pa are also informed. (author)

  17. Laser microprobe mass spectrometry: Potential and limitations for inorganic and organic micro-analysis. Pt. 2

    International Nuclear Information System (INIS)

    Vaeck, I. van; Gijbels, R.

    1990-01-01

    Laser microprobe mass spectrometry (LMMS) employs a highly focused UV laser beam to ionise a microvolume in the order of 1 μm 3 . The produced ions are then mass-separated in a time-of-flight (TOF) or a Fourier Transform (FT) mass spectrometer. The technique allows element localisation, detailed speciation of inorganic substances and structural information of organic molecules. Inorganic applications are treated in the preceding part. This paper will focus on the organic aspects. Selected examples illustrate that TOF LMMS can achieve structural characterisation of molecules, untractable by conventional mass spectrometric techniques. Applicability to the analysis with high spatial resolution is shown and the need for surface availability of organic target molecules is discussed. The recently developed FT LMMS may fulfil the need for better mass resolution. However, the comparability of FT LMMS results with TOF LMMS data is not yet obvious. (orig.)

  18. Isotope analysis of hydrogen and oxygen by infrared spectrometry and activation. Applications to biological media

    International Nuclear Information System (INIS)

    Botter, F.; Darras, R.; Engelmann, C.; Scaringella, M.; Basset, G.; Moreau, F.; Marsac, J.

    1977-01-01

    Two methods for the analysis of biological fluids are presented: the γ activation of blood samples in order to determine their 18 O content, and the infrared spectrometry, applied to the circulating blood, in order to evaluate the heavy water concentration. Measurements of pulmonary extravascular, water performed in rat and man, are presented. Favorable conditions for clinical research in pulmonary diseases are obtained by combining the use of a dye (as intravascular indicator) and heavy water (as a diffusible indicator) with their continuous measurement). The method has several major advantages: it is simple, inexpensive safe for the patient, accurate and allows data acquisition and data processing to be immediately performed. Other medical applications are considered [fr

  19. Analysis of hydrogen isotopes in materials by secondary ion mass spectrometry and nuclear microanalysis

    International Nuclear Information System (INIS)

    Ross, G.G.

    1994-01-01

    Only two techniques are really appropriate for the depth profiling of hydrogen isotopes: nuclear microanalysis (NMA) and secondary ion mass spectrometry (SIMS). The intent of this paper is to give an up to date review of both techniques and to show how they can be used in conjunction. Both techniques (SIMS and NMA) will be described briefly. NMA will divided into two different categories: nuclear reaction analysis (NRA) and elastic recoil detection (ERD). Both techniques (SIMS and NMA) will be discussed in terms of sensitivity, resolution, probing depth, quantitative measurement, generality and selectivity, beam induced effects and surface roughness effects. The principal advantages and disadvantages of each of these techniques will be specified, supporting the contention that SIMS and NMA are complementary and should be used in conjunction. Finally, some examples of, and perspectives for, the complementary use of both techniques will be presented. (Author)

  20. Secondary ion mass spectrometry: The application in the analysis of atmospheric particulate matter

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Di; Hua, Xin; Xiu, Guang-Li; Zheng, Yong-Jie; Yu, Xiao-Ying; Long, Yi-Tao

    2017-10-01

    Currently, considerable attention has been paid to atmospheric particulate matter (PM) investigation due to its importance in human health and global climate change. Surface characterization of PM is important since the chemical heterogeneity between the surface and bulk may vary its impact on the environment and human being. Secondary ion mass spectrometry (SIMS) is a surface technique with high surface sensitivity, capable of high spatial chemical imaging and depth profiling. Recent research shows that SIMS holds great potential in analyzing both surface and bulk chemical information of PM. In this review, we presented the working principal of SIMS in PM characterization, summarized recent applications in PM analysis from different sources, discussed its advantages and limitations, and proposed the future development of this technique with a perspective in environmental sciences.

  1. Diode laser based resonance ionization mass spectrometry for spectroscopy and trace analysis of uranium isotopes

    International Nuclear Information System (INIS)

    Hakimi, Amin

    2013-01-01

    In this doctoral thesis, the upgrade and optimization of a diode laser system for high-resolution resonance ionization mass spectrometry is described. A frequency-control system, based on a double-interferometric approach, allowing for absolute stabilization down to 1 MHz as well as frequency detunings of several GHz within a second for up to three lasers in parallel was optimized. This laser system was used for spectroscopic studies on uranium isotopes, yielding precise and unambiguous level energies, total angular momenta, hyperfine constants and isotope shifts. Furthermore, an efficient excitation scheme which can be operated with commercial diode lasers was developed. The performance of the complete laser mass spectrometer was optimized and characterized for the ultra-trace analysis of the uranium isotope 236 U, which serves as a neutron flux dosimeter and tracer for radioactive anthropogenic contaminations in the environment. Using synthetic samples, an isotope selectivity of ( 236 U)/( 238 U) = 4.5(1.5) . 10 -9 was demonstrated.

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-03-03

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

  4. Rapid analysis of Δ-9-tetrahydrocannabinol in hair using direct analysis in real time ambient ionization orbitrap mass spectrometry.

    Science.gov (United States)

    Duvivier, Wilco F; van Beek, Teris A; Pennings, Ed J M; Nielen, Michel W F

    2014-04-15

    Forensic hair analysis methods are laborious, time-consuming and provide only a rough retrospective estimate of the time of drug intake. Recently, hair imaging methods using matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) were reported, but these methods require the application of MALDI matrix and are performed under vacuum. Direct analysis of entire locks of hair without any sample pretreatment and with improved spatial resolution would thus address a need. Hair samples were attached to stainless steel mesh screens and scanned in the X-direction using direct analysis in real time (DART) ambient ionization orbitrap MS. The DART gas temperature and the accuracy of the probed hair zone were optimized using Δ-9-tetrahydrocannabinol (THC) as a model compound. Since external contamination is a major issue in forensic hair analysis, sub-samples were measured before and after dichloromethane decontamination. The relative intensity of the THC signal in spiked blank hair versus that of quinine as the internal standard showed good reproducibility (26% RSD) and linearity of the method (R(2)  = 0.991). With the DART hair scan THC could be detected in hair samples from different chronic cannabis users. The presence of THC was confirmed by quantitative liquid chromatography/tandem mass spectrometry. Zones with different THC content could be clearly distinguished, indicating that the method might be used for retrospective timeline assessments. Detection of THC in decontaminated drug user hair showed that the DART hair scan not only probes THC on the surface of hair, but penetrates deeply enough to measure incorporated THC. A new approach in forensic hair analysis has been developed by probing complete locks of hair using DART-MS. Longitudinal scanning enables detection of incorporated compounds and can be used as pre-screening for THC without sample preparation. The method could also be adjusted for the analysis of other drugs of abuse. Copyright

  5. Performance of alpha spectrometry in the analysis of uranium isotopes in environmental and nuclear materials

    International Nuclear Information System (INIS)

    Carvalho, F.P.; Oliveira, J.M.

    2009-01-01

    The accuracy of alpha spectrometry in the determination of uranium isotopes at various concentrations levels and with various isotope ratios was tested in a round robin international intercomparison exercise. Results of isotope activity/mass and isotope mass ratios obtained by alpha spectrometry were accurate in a wide range of uranium masses and in isotopic ratios typical of depleted, natural, and low enriched uranium samples. Determinations by alpha spectrometry compared very satisfactorily in accuracy with those by mass spectrometry. For example, determination of U isotopes in natural uranium by alpha spectrometry agreed with mass spectrometry determinations at within ±1%. However, the 236 U isotope, particularly if present in activities much lower than 235 U, might not be determined accurately due to overlap in the alpha particle energies of these two uranium isotopes. (author)

  6. Quantitative, multiplexed workflow for deep analysis of human blood plasma and biomarker discovery by mass spectrometry.

    Science.gov (United States)

    Keshishian, Hasmik; Burgess, Michael W; Specht, Harrison; Wallace, Luke; Clauser, Karl R; Gillette, Michael A; Carr, Steven A

    2017-08-01

    Proteomic characterization of blood plasma is of central importance to clinical proteomics and particularly to biomarker discovery studies. The vast dynamic range and high complexity of the plasma proteome have, however, proven to be serious challenges and have often led to unacceptable tradeoffs between depth of coverage and sample throughput. We present an optimized sample-processing pipeline for analysis of the human plasma proteome that provides greatly increased depth of detection, improved quantitative precision and much higher sample analysis throughput as compared with prior methods. The process includes abundant protein depletion, isobaric labeling at the peptide level for multiplexed relative quantification and ultra-high-performance liquid chromatography coupled to accurate-mass, high-resolution tandem mass spectrometry analysis of peptides fractionated off-line by basic pH reversed-phase (bRP) chromatography. The overall reproducibility of the process, including immunoaffinity depletion, is high, with a process replicate coefficient of variation (CV) of 4,500 proteins are detected and quantified per patient sample on average, with two or more peptides per protein and starting from as little as 200 μl of plasma. The approach can be multiplexed up to 10-plex using tandem mass tags (TMT) reagents, further increasing throughput, albeit with some decrease in the number of proteins quantified. In addition, we provide a rapid protocol for analysis of nonfractionated depleted plasma samples analyzed in 10-plex. This provides ∼600 quantified proteins for each of the ten samples in ∼5 h of instrument time.

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

    International Nuclear Information System (INIS)

    Vrebos, B.

    1996-01-01

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

  8. Capillary electrophoresis - Mass spectrometry metabolomics analysis revealed enrichment of hypotaurine in rat glioma tissues.

    Science.gov (United States)

    Gao, Peng; Ji, Min; Fang, Xueyan; Liu, Yingyang; Yu, Zhigang; Cao, Yunfeng; Sun, Aijun; Zhao, Liang; Zhang, Yong

    2017-11-15

    Glioma is one of the most lethal brain malignancies with unknown etiologies. Many metabolomics analysis aiming at diverse kinds of samples had been performed. Due to the varied adopted analytical platforms, the reported disease-related metabolites were not consistent across different studies. Comparable metabolomics results are more likely to be acquired by analyzing the same sample types with identical analytical platform. For tumor researches, tissue samples metabolomics analysis own the unique advantage that it can gain more direct insight into disease-specific pathological molecules. In this light, a previous reported capillary electrophoresis - mass spectrometry human tissues metabolomics analysis method was employed to profile the metabolome of rat C6 cell implantation gliomas and the corresponding precancerous tissues. It was found that 9 metabolites increased in the glioma tissues. Of them, hypotaurine was the only metabolite that enriched in the malignant tissues as what had been reported in the relevant human tissues metabolomics analysis. Furthermore, hypotaurine was also proved to inhibit α-ketoglutarate-dependent dioxygenases (2-KDDs) through immunocytochemistry staining and in vitro enzymatic activity assays by using C6 cell cultures. This study reinforced the previous conclusion that hypotaurine acted as a competitive inhibitor of 2-KDDs and proved the value of metabolomics in oncology studies. Copyright © 2017. Published by Elsevier Inc.

  9. Paper Spray Mass Spectrometry for the Forensic Analysis of Black Ballpoint Pen Inks

    Science.gov (United States)

    Amador, Victoria Silva; Pereira, Hebert Vinicius; Sena, Marcelo Martins; Augusti, Rodinei; Piccin, Evandro

    2017-09-01

    This article describes the use of paper spray mass spectrometry (PS-MS) for the direct analysis of black ink writings made with ballpoint pens. The novel approach was developed in a forensic context by first performing the classification of commercially available ballpoint pens according to their brands. Six of the most commonly worldwide utilized brands (Bic, Paper Mate, Faber Castell, Pentel, Compactor, and Pilot) were differentiated according to their characteristic chemical patterns obtained by PS-MS. MS on the negative ion mode at a mass range of m/ z 100-1000 allowed prompt discrimination just by visual inspection. On the other hand, the concept of relative ion intensity (RII) and the analysis at other mass ranges were necessary for the differentiation using the positive ion mode. PS-MS combined with partial least squares (PLS) was utilized to monitor changes on the ink chemical composition after light exposure (artificial aging studies). The PLS model was optimized by variable selection, which allowed the identification of the most influencing ions on the degradation process. The feasibility of the method on forensic investigations was also demonstrated in three different applications: (1) analysis of overlapped fresh ink lines, (2) analysis of old inks from archived documents, and (3) detection of alterations (simulated forgeries) performed on archived documents. [Figure not available: see fulltext.

  10. Systematic Integrated Process Design and Control of Reactive Distillation Processes Involving Multi-elements

    DEFF Research Database (Denmark)

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

    2016-01-01

    driving force approach. Next, through analytical, steady-state and closed-loop dynamic analysis it is verified that the control structure, disturbance rejection and energy requirement of the reactive distillation column is better than any other operation point that is not at the maximum driving force...

  11. MEGHNAD – A multi element detector array for heavy ion collision ...

    Indian Academy of Sciences (India)

    of the prototype detector and brief outline of the research programme to be ... Such a nucleus often becomes unstable, and sheds away the extra energy and ... reaction products, and event by event analysis of the nuclear reactions for a .... High voltage is applied at the cathode grid, and the anode is kept at the ground.

  12. Oesophageal cancer in the Transkei: multi-elemental investigation of plant material and water

    International Nuclear Information System (INIS)

    Renan, M.J.; Drennan, B.D.; Keddy, R.J.; Sellschop, J.P.F.

    1978-01-01

    A programme which investigates possible environmental factors which may have an effect on the demographic distribution of oesophageal cancer in the Transkei has been initiated. This report deals with the collection, handling and trace elemental analysis of maize leaves, rice, tomato leaves, spinach, pine needles and orchard leaves

  13. Neutron Activation Analysis with k0 standardisation

    International Nuclear Information System (INIS)

    Pomme, S.

    1998-01-01

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

  14. On the analysis of glycomics mass spectrometry data via the regularized area under the ROC curve

    Directory of Open Access Journals (Sweden)

    Lebrilla Carlito B

    2007-12-01

    Full Text Available Abstract Background Novel molecular and statistical methods are in rising demand for disease diagnosis and prognosis with the help of recent advanced biotechnology. High-resolution mass spectrometry (MS is one of those biotechnologies that are highly promising to improve health outcome. Previous literatures have identified some proteomics biomarkers that can distinguish healthy patients from cancer patients using MS data. In this paper, an MS study is demonstrated which uses glycomics to identify ovarian cancer. Glycomics is the study of glycans and glycoproteins. The glycans on the proteins may deviate between a cancer cell and a normal cell and may be visible in the blood. High-resolution MS has been applied to measure relative abundances of potential glycan biomarkers in human serum. Multiple potential glycan biomarkers are measured in MS spectra. With the objection of maximizing the empirical area under the ROC curve (AUC, an analysis method was considered which combines potential glycan biomarkers for the diagnosis of cancer. Results Maximizing the empirical AUC of glycomics MS data is a large-dimensional optimization problem. The technical difficulty is that the empirical AUC function is not continuous. Instead, it is in fact an empirical 0–1 loss function with a large number of linear predictors. An approach was investigated that regularizes the area under the ROC curve while replacing the 0–1 loss function with a smooth surrogate function. The constrained threshold gradient descent regularization algorithm was applied, where the regularization parameters were chosen by the cross-validation method, and the confidence intervals of the regression parameters were estimated by the bootstrap method. The method is called TGDR-AUC algorithm. The properties of the approach were studied through a numerical simulation study, which incorporates the positive values of mass spectrometry data with the correlations between measurements within person

  15. 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

  16. Optimization of a Differential Ion Mobility Spectrometry-Tandem Mass Spectrometry Method for High-Throughput Analysis of Nicotine and Related Compounds: Application to Electronic Cigarette Refill Liquids.

    Science.gov (United States)

    Regueiro, Jorge; Giri, Anupam; Wenzl, Thomas

    2016-06-21

    Fast market penetration of electronic cigarettes is leading to an exponentially growing number of electronic refill liquids with different nicotine contents and an endless list of flavors. Therefore, rapid and simple methods allowing a fast screening of these products are necessary to detect harmful substances which can negatively impact the health of consumers. In this regard, the present work explores the capabilities of differential ion mobility spectrometry coupled to tandem mass spectrometry for high-throughput analysis of nicotine and 11 related compounds in commercial refill liquids for electronic cigarettes. The influence of main factors affecting the ion mobility separation, such as modifier types and concentration, separation voltage, and temperature, was systematically investigated. Despite small molecular weight differences among the studied compounds, a good separation was achieved in the ion mobility cell under the optimized conditions, which involved the use of ethanol as a polar gas-phase chemical modifier. Indeed, differential ion mobility was able to resolve (resolution >4) nicotine from its structural isomer anabasine without the use of any chromatographic separation. The quantitative performance of the proposed method was then evaluated, showing satisfactory precision (RSD ≤ 16%) and recoveries ranging from 85 to 100% for nicotine, and from 84 to 126% for the rest of the target analytes. Several commercial electronic cigarette refill liquids were analyzed to demonstrate the applicability of the method. In some cases, significant differences were found between labeled and measured levels of nicotine. Anatabine, cotinine, myosmine, and nornicotine were also found in some of the analyzed samples.

  17. Intercomparison study of inductively coupled plasma mass spectrometry, thermal ionization mass spectrometry and fission track analysis of μBq quantities of 239Pu in synthetic urine

    International Nuclear Information System (INIS)

    Inn, K.G.W.; McCurdy, D.; Kuruvilla, L.; Barss, N.M.; Bell III, R.T.; Pietrzak, R.; Kaplan, E.; Inkret, W.; Efurd, W.; Rokop, D.; Lewis, D.; Gautier, P.

    2001-01-01

    Even today, some Marshall Islanders are looking forward to permanently resettling their islands after five decades. The U.S. Department of Energy and the resettled residents require reasonable but cost-prudent assurance that the doses to resident from residual 239 Pu will not exceed recognized international standards or recommendations, as estimated from the excretion of 239 Pu in urine. The goal of this study was to evaluate the bias, uncertainty and sensitivity of analytical techniques that measure 3-56 μBq 239 Pu in synthetic urine. The analytical techniques studied in this work included inductively coupled plasma mass spectrometry, thermal ionization mass spectrometry and fission track analysis. The results of the intercomparison demonstrated that all three techniques were capable of marking the measurements, although not with equal degree of bias and uncertainty. The estimated minimum detectable activity was 1 μBq of 239 Pu per synthetic urine sample. This exercise is also the first effort to certify test materials of plutonium in the nBqxg -1 range. (author)

  18. Simultaneous analysis of fourteen tertiary amine stimulants in human urine for doping control purposes by liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry

    International Nuclear Information System (INIS)

    Lu Jianghai; Wang San; Dong Ying; Wang Xiaobing; Yang Shuming; Zhang Jianli; Deng Jing; Qin Yang; Xu Youxuan; Wu Moutian; Ouyang Gangfeng

    2010-01-01

    A method for the simultaneous screening and confirmation of the presence of fourteen tertiary amine stimulants in human urine by gas chromatography-mass spectrometry (GC-MS) in combination with liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed and validated. Solid phase extraction (SPE) and liquid-liquid extraction (LLE) approaches were utilized for the pre-treatment of the urine samples. The study indicated that the capillary temperature played a significant role in the signal abundances of the protonated molecules of cropropamide and crotethamide under positive ion electrospray ionization (ESI) conditions. In addition, comparison studies of two different pre-treatment approaches as well as the two ionization modes were conducted. The LODs of the developed method for all the analytes were lower than the minimum required performance limit (MRPL) as set forth in the World Anti-Doping Agency (WADA) technical document for laboratories. The human urine sample obtained after oral administration of prolintane.HCl was successfully analyzed by the developed method, which demonstrated the applicability and reliability of the method for routine doping control analysis.

  19. Applicability of hybrid linear ion trap-high resolution mass spectrometry and quadrupole-linear ion trap-mass spectrometry for mycotoxin analysis in baby food.

    Science.gov (United States)

    Rubert, Josep; James, Kevin J; Mañes, Jordi; Soler, Carla

    2012-02-03

    Recent developments in mass spectrometers have created a paradoxical situation; different mass spectrometers are available, each of them with their specific strengths and drawbacks. Hybrid instruments try to unify several advantages in one instrument. In this study two of wide-used hybrid instruments were compared: hybrid quadrupole-linear ion trap-mass spectrometry (QTRAP®) and the hybrid linear ion trap-high resolution mass spectrometry (LTQ-Orbitrap®). Both instruments were applied to detect the presence of 18 selected mycotoxins in baby food. Analytical parameters were validated according to 2002/657/CE. Limits of quantification (LOQs) obtained by QTRAP® instrument ranged from 0.45 to 45 μg kg⁻¹ while lower limits of quantification (LLOQs) values were obtained by LTQ-Orbitrap®: 7-70 μg kg⁻¹. The correlation coefficients (r) in both cases were upper than 0.989. These values highlighted that both instruments were complementary for the analysis of mycotoxin in baby food; while QTRAP® reached best sensitivity and selectivity, LTQ-Orbitrap® allowed the identification of non-target and unknowns compounds. Copyright © 2011 Elsevier B.V. All rights reserved.

  20. Screening in veterinary drug analysis and sports doping control based on full-scan, accurate-mass spectrometry

    NARCIS (Netherlands)

    Peters, R.J.B.; Stolker, A.A.M.; Mol, J.G.J.; Lommen, A.; Lyris, E.; Angelis, Y.S.; Vonaparti, A.; Stamou, M.; Georgakopoulos, C.G.; Nielen, M.W.F.

    2010-01-01

    A common trend in food contaminants and sports doping control is towards a limited number of targeted, full-scan, accurate-mass spectrometry (MS) methods based on time-of-flight (TOF) or Fourier-transform orbital trap (Orbitrap) mass analyzers. Retrospective analysis of the full-scan datasets of

  1. Comparative urine analysis by liquid chromatography-mass spectrometry and multivariate statistics : Method development, evaluation, and application to proteinuria

    NARCIS (Netherlands)

    Kemperman, Ramses F. J.; Horvatovich, Peter L.; Hoekman, Berend; Reijmers, Theo H.; Muskiet, Frits A. J.; Bischoff, Rainer

    2007-01-01

    We describe a platform for the comparative profiling of urine using reversed-phase liquid chromatography-mass spectrometry (LC-MS) and multivariate statistical data analysis. Urinary compounds were separated by gradient elution and subsequently detected by electrospray Ion-Trap MS. The lower limit

  2. Atmospheric Pressure-Thermal Desorption (AP-TD)/Electrospray Ionization-Mass Spectrometry for the Rapid Analysis of Bacillus Spores

    Science.gov (United States)

    A technique is described where an atmospheric pressure-thermal desorption (AP-TD) device and electrospray ionization (ESI)-mass spectrometry are coupled and used for the rapid analysis of Bacillus spores in complex matrices. The resulting AP-TD/ESI-MS technique combines the generation of volatile co...

  3. Development of matrix-assisted laser desorption ionization-mass spectrometry imaging (MALDI-MSI) for plant metabolite analysis

    Energy Technology Data Exchange (ETDEWEB)

    Korte, Andrew R [Iowa State Univ., Ames, IA (United States)

    2014-12-01

    This thesis presents efforts to improve the methodology of matrix-assisted laser desorption ionization-mass spectrometry imaging (MALDI-MSI) as a method for analysis of metabolites from plant tissue samples. The first chapter consists of a general introduction to the technique of MALDI-MSI, and the sixth and final chapter provides a brief summary and an outlook on future work.

  4. Solid phase extraction for removal of matrix effects in lipophilic marine toxin analysis by liquid chromatography-tandem mass spectrometry

    NARCIS (Netherlands)

    Gerssen, A.; McElhinney, M.; Mulder, P.P.J.; Bire, R.; Hess, P.; Boer, de J.

    2009-01-01

    The potential of solid phase extraction (SPE) clean-up has been assessed to reduce matrix effects (signal suppression or enhancement) in the liquid chromatography-tandem mass spectrometry (LC¿MS/MS) analysis of lipophilic marine toxins. A large array of ion-exchange, silica-based, and mixed-function

  5. Solid phase extraction for removal of matrix effects in lipophilic marine toxin analysis by liquid chromatography-tandem mass spectrometry

    NARCIS (Netherlands)

    Gerssen, A.; McElhinney, A. M.; Mulder, P.P.J.; Bire, L.; Hess, P.; de Boer, J.

    2009-01-01

    The potential of solid phase extraction (SPE) clean-up has been assessed to reduce matrix effects (signal suppression or enhancement) in the liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis of lipophilic marine toxins. A large array of ion-exchange, silica-based, and mixed-function

  6. Solid-supported enzymatic synthesis of pectic oligogalacturonides and their analysis by MALDI-TOF mass spectrometry

    DEFF Research Database (Denmark)

    Guillaumie, Fanny; Sterling, J.D.; Jensen, K.J.

    2003-01-01

    Solid-phase biosynthetic reactions, followed by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry analysis (MALDI-TOF), was used to gain insight into the biosynthesis of pectin oligomers. Sepharose supports bearing long pectic oligogalacturonides (OGAs) anchored through...... into the liquid phases by MALDI-TOF mass spectrometry. In time course studies conducted with an immobilized (alpha-D-GalA)(14) and limiting amounts of the glycosyl donor, the predominant product was an OGA extended by one GalA residue at the non-reducing end (i.e., (GalA)(15)). When UDP-GalA was added...

  7. Classification of soil samples according to their geographic origin using gamma-ray spectrometry and principal component analysis

    International Nuclear Information System (INIS)

    Dragovic, Snezana; Onjia, Antonije

    2006-01-01

    A principal component analysis (PCA) was used for classification of soil samples from different locations in Serbia and Montenegro. Based on activities of radionuclides ( 226 Ra, 238 U, 235 U, 4 K, 134 Cs, 137 Cs, 232 Th and 7 Be) detected by gamma-ray spectrometry, the classification of soils according to their geographical origin was performed. Application of PCA to our experimental data resulted in satisfactory classification rate (86.0% correctly classified samples). The obtained results indicate that gamma-ray spectrometry in conjunction with PCA is a viable tool for soil classification

  8. Simultaneous analysis of amino acid and organic acid by NMR spectrometry, 2. Diagnostic aids for inborn error of metabolism

    Energy Technology Data Exchange (ETDEWEB)

    Koda, Naoya; Yamaguchi, Shuichi; Mori, Takeshi.

    1987-09-01

    Analysis of urine from patients with inborn error of metabolism were studied by /sup 1/H-nuclear magnetic resonance (NMR) spectrometry. Diseases studied were as follows; phenylketonuria, biotin responsive multiple carboxylase deficiency, non-ketotic hyperglycinemia, 3-ketothiolase deficiency, alkaptonuria, methylmalonic acidemia, isovaleric acidemia, glutaric aciduria, argininosuccinic aciduria and hyperornithinemia. In each disease, specific metabolites in urine were recognized by NMR spectrometry. This method is accomplished within 10 minutes with non-treated small volume of urine and will be successfully available for the screening andor diagnosis of inherited metabolic diseases of amino acid and organic acid.

  9. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1988-09-01

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

  11. Glass bottle sampling solid phase microextraction gas chromatography mass spectrometry for breath analysis of drug metabolites.

    Science.gov (United States)

    Lu, Yan; Niu, Wenqi; Zou, Xue; Shen, Chengyin; Xia, Lei; Huang, Chaoqun; Wang, Hongzhi; Jiang, Haihe; Chu, Yannan

    2017-05-05

    Breath analysis is a non-invasive approach which may be applied to disease diagnosis and pharmacokinetic study. In the case of offline analysis, the exhaled gas needs to be collected and the sampling bag is often used as the storage vessel. However, the sampling bag usually releases some extra compounds, which may interfere with the result of the breath test. In this study, a novel breath sampling glass bottle was developed with a syringe needle sampling port for solid phase microextraction (SPME). Such a glass bottle scarcely liberates compounds and can be used to collect exhaled gas for ensuing analysis by gas chromatography-mass spectrometry (GC-MS). The glass bottle sampling SPME-GC-MS analysis was carried out to investigate the breath metabolites of myrtol, a multicompound drug normally used in the treatment of bronchitis and sinusitis. Four compounds, α-pinene, 2,3-dehydro-1,8-cineole, d-limonene and 1,8-cineole were found in the exhaled breath of all eight volunteers who had taken the myrtol. While for other ten subjects who had not used the myrtol, these compounds were undetectable. In the SPME-GC-MS analysis of the headspace of myrtol, three compounds were detected including α-pinene, d-limonene and 1,8-cineole. Comparing the results of breath and headspace analysis, it indicates that 2,3-dehydro-1,8-cineole in the breath is the metabolite of 1,8-cineole. It is the first time that this metabolite was identified in human breath. The study demonstrates that the glass bottle sampling SPME-GC-MS method is applicable to exhaled gas analysis including breath metabolites investigation of drugs like myrtol. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Recent development in mass spectrometry and its hyphenated techniques for the analysis of medicinal plants.

    Science.gov (United States)

    Zhu, Ming-Zhi; Chen, Gui-Lin; Wu, Jian-Lin; Li, Na; Liu, Zhong-Hua; Guo, Ming-Quan

    2018-04-23

    Medicinal plants are gaining increasing attention worldwide due to their empirical therapeutic efficacy and being a huge natural compound pool for new drug discovery and development. The efficacy, safety and quality of medicinal plants are the main concerns, which are highly dependent on the comprehensive analysis of chemical components in the medicinal plants. With the advances in mass spectrometry (MS) techniques, comprehensive analysis and fast identification of complex phytochemical components have become feasible, and may meet the needs, for the analysis of medicinal plants. Our aim is to provide an overview on the latest developments in MS and its hyphenated technique and their applications for the comprehensive analysis of medicinal plants. Application of various MS and its hyphenated techniques for the analysis of medicinal plants, including but not limited to one-dimensional chromatography, multiple-dimensional chromatography coupled to MS, ambient ionisation MS, and mass spectral database, have been reviewed and compared in this work. Recent advancs in MS and its hyphenated techniques have made MS one of the most powerful tools for the analysis of complex extracts from medicinal plants due to its excellent separation and identification ability, high sensitivity and resolution, and wide detection dynamic range. To achieve high-throughput or multi-dimensional analysis of medicinal plants, the state-of-the-art MS and its hyphenated techniques have played, and will continue to play a great role in being the major platform for their further research in order to obtain insight into both their empirical therapeutic efficacy and quality control. Copyright © 2018 John Wiley & Sons, Ltd.

  13. Correlation analysis of measurement result between accelerator mass spectrometry and gamma counter

    International Nuclear Information System (INIS)

    Minamimoto, Ryogo; Cheng, C.; Oka, Takashi; Inoue, Tomio; Hamabe, Yoshimi; Shimoda, Marika

    2010-01-01

    The guidelines for microdosing in clinical trials were published in Japan in 2008 following the guidelines of the European Medicines Agency and the Food and Drug Administration. They recommend utilizing accelerator mass spectrometry (AMS) and positron emission tomography as candidates for monitoring drug metabolites in preclinical studies. We correlate the two methods by measuring appropriately labeled tissue samples from various mouse organs using both AMS and gamma counter. First, we measured the 14 C background levels in mouse organs using the AMS system. We then clarified the relationship between AMS and gamma counter by simultaneously administering 14 C-2-fluoro-2-deoxyglucose ( 14 C-FDG) and 18 F-2-fluoro-2-deoxyglucose ( 18 F-FDG). Tissue distribution was examined after 30 min, 1 h, 2 h and 4 h using the AMS system for 14 C-FDG and gamma counter for 18 F-FDG. Background 14 C levels were subtracted from the data obtained with radiotracer administration. The background 14 C concentration differed with tissue type measured. Background 14 C concentration in mouse liver was higher than in other organs, and was approximately 1.5-fold that in blood. The correlation coefficient (r) of the measurements between AMS ( 14 C-FDG) and gamma counter ( 18 F-FDG) was high in both normal (0.99 in blood, 0.91 in brain, 0.61 in liver and 0.78 in kidney) and tumor-bearing mice (0.95 in blood and 0.99 in tumor). The clearance profile of 18 F-FDG was nearly identical to that of 14 C-FDG measured with AMS. Accelerator mass spectrometry analysis has an excellent correlation with biodistribution measurements using gamma counter. Our results suggest that the combination of AMS and positron emission tomography (PET) can act as a complementary approach to accelerate drug development. (author)

  14. Liquid chromatography/mass spectrometry analysis of exhaled leukotriene B4 in asthmatic children

    Directory of Open Access Journals (Sweden)

    Barnes Peter J

    2005-10-01

    Full Text Available Abstract Background The role of leukotriene (LT B4, a potent inflammatory mediator, in atopic asthmatic and atopic nonasthmatic children is largely unknown. The lack of a gold standard technique for measuring LTB4 in exhaled breath condensate (EBC has hampered its quantitative assessment in this biological fluid. We sought to measure LTB4 in EBC in atopic asthmatic children and atopic nonasthmatic children. Exhaled nitric oxide (NO was measured as an independent marker of airway inflammation. Methods Fifteen healthy children, 20 atopic nonasthmatic children, 25 steroid-naïve atopic asthmatic children, and 22 atopic asthmatic children receiving inhaled corticosteroids were studied. The study design was of cross-sectional type. Exhaled LTB4 concentrations were measured using liquid chromatography/mass spectrometry-mass spectrometry (LC/MS/MS with a triple quadrupole mass spectrometer. Exhaled NO was measured by chemiluminescence with a single breath on-line method. LTB4 values were expressed as the total amount (in pg of eicosanoid expired in the 15-minute breath test. Kruskal-Wallis test was used to compare groups. Results Compared with healthy children [87.5 (82.5–102.5 pg, median and interquartile range], exhaled LTB4 was increased in steroid-naïve atopic asthmatic [255.1 (175.0–314.7 pg, p 4 than steroid-naïve asthmatics [125.0 (25.0–245.0 pg vs 255.1 (175.0–314.7 pg, p Conclusion In contrast to exhaled NO concentrations, exhaled LTB4 values are selectively elevated in steroid-naïve atopic asthmatic children, but not in atopic nonasthmatic children. Although placebo control studies are warranted, inhaled corticosteroids seem to reduce exhaled LTB4 in asthmatic children. LC/MS/MS analysis of exhaled LTB4 might provide a non-invasive, sensitive, and quantitative method for airway inflammation assessment in asthmatic children.

  15. Data on coffee composition and mass spectrometry analysis of mixtures of coffee related carbohydrates, phenolic compounds and peptides

    Directory of Open Access Journals (Sweden)

    Ana S.P. Moreira

    2017-08-01

    Full Text Available The data presented here are related to the research paper entitled “Transglycosylation reactions, a main mechanism of phenolics incorporation in coffee melanoidins: inhibition by Maillard reaction” (Moreira et al., 2017 [1]. Methanolysis was applied in coffee fractions to quantify glycosidically-linked phenolics in melanoidins. Moreover, model mixtures mimicking coffee beans composition were roasted and analyzed using mass spectrometry-based approaches to disclose the regulatory role of proteins in transglycosylation reactions extension. This article reports the detailed chemical composition of coffee beans and derived fractions. In addition, it provides gas chromatography–mass spectrometry (GC–MS chromatograms and respective GC–MS spectra of silylated methanolysis products obtained from phenolic compounds standards, as well as the detailed identification of all compounds observed by electrospray mass spectrometry (ESI-MS analysis of roasted model mixtures, paving the way for the identification of the same type of compounds in other samples.

  16. Determination of multi-element profiles of soil at Visakhapatnam using EDXRF technique

    International Nuclear Information System (INIS)

    Sandeep, P.; Kothai, P.; Dusane, C.B.; Sahu, S.K.; Pandit, G.G.

    2014-01-01

    In the present study attempt has been made to generate elemental profile database for major sources of soil pollution, specific to Visakhapatnam. Representative road dust and soil samples from major industrial locations were collected and analyzed for various metals distribution using EDXRF. Analysis results indicate that V and Ni were predominant at PR and Zn was found to be dominating in road dust samples. Higher concentration of Arsenic was observed at TPP as compared to all other sites. Cr was found to be dominating at TPP and SP. I geo calculations suggest that soil is highly contaminated with heavy metal pollutants. (author)

  17. OpenMSI Arrayed Analysis Toolkit: Analyzing Spatially Defined Samples Using Mass Spectrometry Imaging

    Energy Technology Data Exchange (ETDEWEB)

    de Raad, Markus [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); de Rond, Tristan [Univ. of California, Berkeley, CA (United States); Rübel, Oliver [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Keasling, Jay D. [Univ. of California, Berkeley, CA (United States); Joint BioEnergy Inst. (JBEI), Emeryville, CA (United States); Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Technical Univ. of Denmark, Lyngby (Denmark); Northen, Trent R. [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); USDOE Joint Genome Institute (JGI), Walnut Creek, CA (United States); Bowen, Benjamin P. [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); USDOE Joint Genome Institute (JGI), Walnut Creek, CA (United States)

    2017-05-03

    Mass spectrometry imaging (MSI) has primarily been applied in localizing biomolecules within biological matrices. Although well-suited, the application of MSI for comparing thousands of spatially defined spotted samples has been limited. One reason for this is a lack of suitable and accessible data processing tools for the analysis of large arrayed MSI sample sets. In this paper, the OpenMSI Arrayed Analysis Toolkit (OMAAT) is a software package that addresses the challenges of analyzing spatially defined samples in MSI data sets. OMAAT is written in Python and is integrated with OpenMSI (http://openmsi.nersc.gov), a platform for storing, sharing, and analyzing MSI data. By using a web-based python notebook (Jupyter), OMAAT is accessible to anyone without programming experience yet allows experienced users to leverage all features. OMAAT was evaluated by analyzing an MSI data set of a high-throughput glycoside hydrolase activity screen comprising 384 samples arrayed onto a NIMS surface at a 450 μm spacing, decreasing analysis time >100-fold while maintaining robust spot-finding. The utility of OMAAT was demonstrated for screening metabolic activities of different sized soil particles, including hydrolysis of sugars, revealing a pattern of size dependent activities. Finally, these results introduce OMAAT as an effective toolkit for analyzing spatially defined samples in MSI. OMAAT runs on all major operating systems, and the source code can be obtained from the following GitHub repository: https://github.com/biorack/omaat.

  18. Application of secondary ion mass spectrometry (SIMS) to biological sample analysis

    International Nuclear Information System (INIS)

    Tamura, Hifumi

    1990-01-01

    Some major issues and problems related with the analysis of biological samples are discussed, focusing on demonstrated and possible solutions and the application of secondary ion mass spectrometry (SIMS) to investigation of the composition of biological samples. The effective use of secondary electrons in combination with negative ions is most practical for the analysis of biological samples. Regardless of whether positive or negative ions are used, the electric potential at the surface of a sample stays around a constant value because of the absense of the accumulation of electric charges at the surface, leading to almost complete avoidance of the charging of the biological sample. A soft tissue sample can suffer damage to the tissue or migration of atoms in removing water from the sample. Some processes including fixation and freeze drying are available to prevent this. The application of SIMS to biological analysis is still in the basic research stage and further studies will be required to develop practical methods. Possible areas of its application include medicine, pathology, toxicology, pharmacology, plant physiology and other areas related with marine life and marine contamination. (N.K.)

  19. Atmospheric pressure chemical ionization Fourier transform ion cyclotron resonance mass spectrometry for complex thiophenic mixture analysis

    KAUST Repository

    Hourani, Nadim

    2013-10-01

    Rationale Polycyclic aromatic sulfur heterocycles (PASHs) are detrimental species for refining processes in petroleum industry. Current mass spectrometric Methods that determine their composition are often preceded by derivatization and dopant addition approaches. Different ionization Methods have different impact on the molecular assignment of complex PASHs. The analysis of such species under atmospheric pressure chemical ionization (APCI) is still considered limited due to uncontrolled ion generation with low- and high-mass PASHs. Methods The ionization behavior of a model mixture of five selected PASH standards was investigated using an APCI source with nitrogen as the reagent gas. A complex thiophenic fraction was separated from a vacuum gas oil (VGO) and injected using the same method. The samples were analyzed using Fourier transform ion cyclotron resonance mass spectrometry (FTICR MS). RESULTS PASH model analytes were successfully ionized and mainly [M + H]+ ions were produced. The same ionization pattern was observed for the real thiophenic sample. It was found that S1 class species were the major sulfur-containing species found in the VGO sample. These species indicated the presence of alkylated benzothiophenic (BT), dibenzothiophenic (DBT) and benzonaphthothiophenic (BNT) series that were detected by APCI-FTICR MS. CONCLUSIONS This study provides an established APCI-FTICR MS method for the analysis of complex PASHs. PASHs were detected without using any derivatization and without fragmentation. The method can be used for the analysis of S-containing crude oil samples. © 2013 John Wiley & Sons, Ltd.

  20. Monoacylglycerol Analysis Using MS/MSALL Quadruple Time of Flight Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Fei Gao

    2016-08-01

    Full Text Available Monoacylglycerols (MAGs are structural and bioactive metabolites critical for biological function. Development of facile tools for measuring MAG are essential to understand its role in different diseases and various pathways. A data-independent acquisition method, MS/MSALL, using electrospray ionization (ESI coupled quadrupole time of flight mass spectrometry (MS, was utilized for the structural identification and quantitative analysis of individual MAG molecular species. Compared with other acylglycerols, diacylglycerols (DAG and triacylglycerols (TAG, MAG characteristically presented as a dominant protonated ion, [M + H]+, and under low collision energy as fatty acid-like fragments due to the neutral loss of the glycerol head group. At low concentrations (<10 pmol/µL, where lipid-lipid interactions are rare, there was a strong linear correlation between ion abundance and MAG concentration. Moreover, using the MS/MSALL method the major MAG species from human plasma and mouse brown and white adipose tissues were quantified in less than 6 min. Collectively, these results demonstrate that MS/MSALL analysis of MAG is an enabling strategy for the direct identification and quantitative analysis of low level MAG species from biological samples with high throughput and sensitivity.

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

    Energy Technology Data Exchange (ETDEWEB)

    Shu, Li; Jian, Jia; Xiaoguang, Gao; Xiuli, He [State Key Laboratory of Transducer Technology, Institute of Electronics, Chinese Academy of Sciences, Beijing 100190 (China); Li Jianping, E-mail: jpli@mail.ie.ac.cn [State Key Laboratory of Transducer Technology, Institute of Electronics, Chinese Academy of Sciences, Beijing 100190 (China)

    2012-03-30

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

  2. Direct Analysis in Real Time Mass Spectrometry for Characterization of Large Saccharides.

    Science.gov (United States)

    Ma, Huiying; Jiang, Qing; Dai, Diya; Li, Hongli; Bi, Wentao; Da Yong Chen, David

    2018-03-06

    Polysaccharide characterization posts the most difficult challenge to available analytical technologies compared to other types of biomolecules. Plant polysaccharides are reported to have numerous medicinal values, but their effect can be different based on the types of plants, and even regions of productions and conditions of cultivation. However, the molecular basis of the differences of these polysaccharides is largely unknown. In this study, direct analysis in real time mass spectrometry (DART-MS) was used to generate polysaccharide fingerprints. Large saccharides can break down into characteristic small fragments in the DART source via pyrolysis, and the products are then detected by high resolution MS. Temperature was shown to be a crucial parameter for the decomposition of large polysaccharide. The general behavior of carbohydrates in DART-MS was also studied through the investigation of a number of mono- and oligosaccharide standards. The chemical formula and putative ionic forms of the fragments were proposed based on accurate mass with less than 10 ppm mass errors. Multivariate data analysis shows the clear differentiation of different plant species. Intensities of marker ions compared among samples also showed obvious differences. The combination of DART-MS analysis and mechanochemical extraction method used in this work demonstrates a simple, fast, and high throughput analytical protocol for the efficient evaluation of molecular features in plant polysaccharides.

  3. MALDI-TOF mass spectrometry for quantitative gene expression analysis of acid responses in Staphylococcus aureus.

    Science.gov (United States)

    Rode, Tone Mari; Berget, Ingunn; Langsrud, Solveig; Møretrø, Trond; Holck, Askild

    2009-07-01

    Microorganisms are constantly exposed to new and altered growth conditions, and respond by changing gene expression patterns. Several methods for studying gene expression exist. During the last decade, the analysis of microarrays has been one of the most common approaches applied for large scale gene expression studies. A relatively new method for gene expression analysis is MassARRAY, which combines real competitive-PCR and MALDI-TOF (matrix-assisted laser desorption/ionization time-of-flight) mass spectrometry. In contrast to microarray methods, MassARRAY technology is suitable for analysing a larger number of samples, though for a smaller set of genes. In this study we compare the results from MassARRAY with microarrays on gene expression responses of Staphylococcus aureus exposed to acid stress at pH 4.5. RNA isolated from the same stress experiments was analysed using both the MassARRAY and the microarray methods. The MassARRAY and microarray methods showed good correlation. Both MassARRAY and microarray estimated somewhat lower fold changes compared with quantitative real-time PCR (qRT-PCR). The results confirmed the up-regulation of the urease genes in acidic environments, and also indicated the importance of metal ion regulation. This study shows that the MassARRAY technology is suitable for gene expression analysis in prokaryotes, and has advantages when a set of genes is being analysed for an organism exposed to many different environmental conditions.

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

    International Nuclear Information System (INIS)

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

    1991-01-01

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

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  6. Headspace Analysis of Philippine Civet Coffee Beans Using Gas Chromatography-Mass Spectrometry and Electronic Nose

    Science.gov (United States)

    Ongo, E.; Sevilla, F.; Antonelli, A.; Sberveglieri, G.; Montevecchi, G.; Sberveglieri, V.; de Paola, E. L.; Concina, I.; Falasconi, M.

    2011-11-01

    Civet coffee, the most expensive and best coffee in the world, is an economically important export product of the Philippines. With a growing threat of food adulteration and counterfeiting, a need for quality authentication is essential to protect the integrity and strong market value of Philippine civet coffee. At present, there is no internationally accepted method of verifying whether a bean is an authentic civet coffee. This study presented a practical and promising approach to identify and establish the headspace qualitative profile of Philippine civet coffee using electronic nose (E-nose) and gas chromatography-mass spectrometry (GC-MS). E-nose analysis revealed that aroma characteristic is one of the most important quality indicators of civet coffee. The findings were supported by GC-MS analysis. Principal component analysis (PCA) exhibited a clearly separated civet coffees from their control beans. The chromatographic fingerprints indicated that civet coffees differed with their control beans in terms of composition and concentration of individual volatile constituents.

  7. Analysis of volatile compounds by open-air ionization mass spectrometry.

    Science.gov (United States)

    Meher, Anil Kumar; Chen, Yu-Chie

    2017-05-08

    This study demonstrates a simple method for rapid and in situ identification of volatile and endogenous compounds in culinary spice samples through mass spectrometry (MS). This method only requires a holder for solid spice sample (2-3 mm) that is placed close to a mass spectrometer inlet, which is applied with a high voltage. Volatile species responsible for the aroma of the spice samples can be readily detected by the mass spectrometer. Sample pretreatment is not required prior to MS analysis, and no solvent was used during MS analysis. The high voltage applied to the inlet of the mass spectrometer induces the ionization of volatile compounds released from the solid spice samples. Furthermore, moisture in the air also contributes to the ionization of volatile compounds. Dried spices including cinnamon and cloves are used as the model sample to demonstrate this straightforward MS analysis, which can be completed within few seconds. Furthermore, we also demonstrate the suitability of the current method for rapid screening of cinnamon quality through detection of the presence of a hepatotoxic agent, i.e. coumarin. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Ionization Suppression and Recovery in Direct Biofluid Analysis Using Paper Spray Mass Spectrometry

    Science.gov (United States)

    Vega, Carolina; Spence, Corina; Zhang, Chengsen; Bills, Brandon J.; Manicke, Nicholas E.

    2016-04-01

    Paper spray mass spectrometry is a method for the direct analysis of biofluid samples in which extraction of analytes from dried biofluid spots and electrospray ionization occur from the paper on which the dried sample is stored. We examined matrix effects in the analysis of small molecule drugs from urine, plasma, and whole blood. The general method was to spike stable isotope labeled analogs of each analyte into the spray solvent, while the analyte itself was in the dried biofluid. Intensity of the labeled analog is proportional to ionization efficiency, whereas the ratio of the analyte intensity to the labeled analog in the spray solvent is proportional to recovery. Ion suppression and recovery were found to be compound- and matrix-dependent. Highest levels of ion suppression were obtained for poor ionizers (e.g., analytes lacking basic aliphatic amine groups) in urine and approached -90%. Ion suppression was much lower or even absent for good ionizers (analytes with aliphatic amines) in dried blood spots. Recovery was generally highest in urine and lowest in blood. We also examined the effect of two experimental parameters on ion suppression and recovery: the spray solvent and the sample position (how far away from the paper tip the dried sample was spotted). Finally, the change in ion suppression and analyte elution as a function of time was examined by carrying out a paper spray analysis of dried plasma spots for 5 min by continually replenishing the spray solvent.

  9. Solution of multi-element LED light sources development automation problem

    Science.gov (United States)

    Chertov, Aleksandr N.; Gorbunova, Elena V.; Korotaev, Valery V.; Peretyagin, Vladimir S.

    2014-09-01

    The intensive development of LED technologies resulted in the creation of multicomponent light sources in the form of controlled illumination devices based on usage of mentioned LED technologies. These light sources are used in different areas of production (for example, in the food industry for sorting products or in the textile industry for quality control, etc.). The use of LED lighting products in the devices used in specialized lighting, became possible due to wide range of colors of light, LED structures (which determines the direction of radiation, the spatial distribution and intensity of the radiation, electrical, heat, power and other characteristics), and of course, the possibility of obtaining any shade in a wide dynamic range of brightness values. LED-based lighting devices are notable for the diversity of parameters and characteristics, such as color radiation, location and number of emitters, etc. Although LED technologies have several advantages, however, they require more attention if you need to ensure a certain character of illumination distribution and/or distribution of the color picture at a predetermined distance (for example, at flat surface, work zone, area of analysis or observation). This paper presents software designed for the development of the multicomponent LED light sources. The possibility of obtaining the desired color and energy distribution at the zone of analysis by specifying the spatial parameters of the created multicomponent light source and using of real power, spectral and color parameters and characteristics of the LEDs is shown as well.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2001-07-01

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

  11. Multi-element determinations of N,N-dimethylformamide (DMF) coal slurries using ICP-OES

    Energy Technology Data Exchange (ETDEWEB)

    M. Mujuru; R.I. McCrindle; B.M. Botha; P.P. Ndibewu [Tshwane University of Technology, Pretoria (South Africa). Department of Chemistry

    2009-04-15

    A slurry nebulisation technique was applied for elemental analysis of bituminous coals SARM 18, SARM 19 and four coals from three different seams in Witbank, South Africa, by inductively coupled plasma optical emission spectroscopy (ICP-OES). Major elements (Al, Ca, Fe, Mg, S, Si and Ti) and trace elements (Ba, Cr, Mn, Ni, Sr, V, Zn and Zr) in coal were determined. Various slurry preparations were evaluated using two dispersants (glycerol and Triton X-100) and by varying the concentration of dispersants, between 0.1% and 1.0% (v/v). The effect of initially solubilising the ground coal in N,N-dimethylformamide (DMF) was investigated by varying the volume of DMF added. The effect of wet grinding with DMF was investigated. Wet grinding with DMF was shown to drastically reduce particle sizes (50.0% < 0.28 m and 90.0% < 6.17 {mu}m) as compared to dry grinding (50.0% < 5.25 {mu}m and 90.0% < 11.1 {mu}m). The reduced particle sizes and increased transport efficiency of the coal slurries led to improved analytical recoveries of elements in the reference coal, SARM 18. The best analytical recoveries for all elements were achieved using 0.1% Triton X-100 with 10.0% DMF. Results obtained by ICP-OES after wet grinding of the coal with DMF, using 0.1% Triton X-100, also gave excellent recoveries (Al, 100%; Ca, 103%; Cr, 106%; Fe, 102%; Mg, 100%; Mn, 104%; Ni, 109%; Si, 102%; Ti, 95.0%; and V, 108%). The results obtained with 10.0% DMF and 0.1% Triton X-100 were in agreement with certified values for all selected elements according to paired t-test at the 95.0% confidence level. Selected elements (Al, Ca, Fe, Mg, Mn, Si, Ti and V) were also analysed with X-ray fluorescence for comparison with results obtained from ICP-OES. Analysis by ICP-OES of microwave digested coal was also carried out. It is suggested that the DMF slurry technique could be used for routine analysis of bituminous coals. 27 refs., 4 figs., 4 tabs.

  12. Quantitation of mycotoxins using direct analysis in real time (DART)-mass spectrometry (MS)

    Science.gov (United States)

    Ambient ionization represents a new generation of mass spectrometry ion sources which is used for rapid ionization of small molecules under ambient conditions. The combination of ambient ionization and mass spectrometry allows analyzing multiple food samples with simple or no sample treatment, or in...

  13. Atomic spectrometry based on metallic tube atomizers heated by flame: Innovative strategies from fundamentals to analysis

    International Nuclear Information System (INIS)

    Arruda, Marco Aurelio Zezzi; Figueiredo, Eduardo Costa

    2009-01-01

    This review describes recent developments in atomic absorption spectrometry using metallic tube atomizers heated by flames. Sample introduction in spray or gaseous form is emphasized, describing some proposed systems for this task and the fundamentals involved in each context. The latest challenges and future possibilities for use of metallic tubes in atomic/mass spectrometry are also considered.

  14. Mass Spectrometry Market: Value chain and stakeholder analysis up to 2024

    OpenAIRE

    Smita Deshmukh

    2016-01-01

    Transparency Market Research Reports incorporated a definite business overview and investigation inclines on "Mass Spectrometry Market". This report likewise incorporates more illumination about fundamental review of the business including definitions, requisitions and worldwide business sector industry structure. Read Full Report: http://www.transparencymarketresearch.com/mass-spectrometry-market.html

  15. Getting to the core of protein pharmaceuticals – comprehensive structure analysis by mass spectrometry

    DEFF Research Database (Denmark)

    Leurs, Ulrike; Mistarz, Ulrik Hvid; Rand, Kasper Dyrberg

    2015-01-01

    . Mass spectrometry has evolved as a powerful tool for the characterization of both primary and higher order structures of protein pharmaceuticals. Furthermore, the chemical and physical stability of protein drugs, as well as their pharmacokinetics are nowadays routinely determined by mass spectrometry...

  16. An Assessment of the Icing Blade and the SEA Multi-Element Sensor for Liquid Water Content Calibration of the NASA GRC Icing Research Tunnel

    Science.gov (United States)

    Steen, Laura E.; Ide, Robert F.; Van Zante, Judith Foss

    2017-01-01

    The Icing Research Tunnel at NASA Glenn has recently switched to from using the Icing Blade to using the SEA Multi-Element Sensor (also known as the multi-wire) for its calibration of cloud liquid water content. In order to perform this transition, tests were completed to compare the Multi-Element Sensor to the Icing Blade, particularly with respect to liquid water content, airspeed, and drop size. The two instruments were found to compare well for the majority of Appendix C conditions. However, it was discovered that the Icing Blade under-measures when the conditions approach the Ludlam Limit. This paper also describes data processing procedures for the Multi-Element Sensor in the IRT, including collection efficiency corrections, mounting underneath a splitter plate, and correcting for a jump in the compensation wire power. Further data is presented to describe the repeatability of the IRT with the Multi-Element sensor, health-monitoring checks for the instrument, and a sensing-element configuration comparison.

  17. X-ray fluorescence and gamma-ray spectrometry combined with multivariate analysis for topographic studies in agricultural soil

    International Nuclear Information System (INIS)

    Castilhos, Natara D.B. de; Melquiades, Fábio L.; Thomaz, Edivaldo L.; Bastos, Rodrigo Oliveira

    2015-01-01

    Physical and chemical properties of soils play a major role in the evaluation of different geochemical signature, soil quality, discrimination of land use type, soil provenance and soil degradation. The objectives of the present study are the soil elemental characterization and soil differentiation in topographic sequence and depth, using Energy Dispersive X-Ray Fluorescence (EDXRF) as well as gamma-ray spectrometry data combined with Principal Component Analysis (PCA). The study area is an agricultural region of Boa Vista catchment which is located at Guamiranga municipality, Brazil. PCA analysis was performed with four different data sets: spectral data from EDXRF, spectral data from gamma-ray spectrometry, concentration values from EDXRF measurements and concentration values from gamma-ray spectrometry. All PCAs showed similar results, confirmed by hierarchical cluster analysis, allowing the data grouping into top, bottom and riparian zone samples, i.e. the samples were separated due to its landscape position. The two hillslopes present the same behavior independent of the land use history. There are distinctive and characteristic patterns in the analyzed soil. The methodologies presented are promising and could be used to infer significant information about the region to be studied. - Highlights: • Characterization of topographic sequence of two hillslopes from agricultural soil. • Employment of EDXRF and gamma-ray spectrometry data combined with PCA. • The combination of green analytical methodologies with chemometric studies allowed soil differentiation. • The innovative methodology is promising for direct characterization of agricultural catchments

  18. Analysis of perfluoroalkyl substances in cord blood by turbulent flow chromatography coupled to tandem mass spectrometry

    International Nuclear Information System (INIS)

    Llorca, Marta; Pérez, Francisca; Farré, Marinella; Agramunt, Sílvia; Kogevinas, Manolis; Barceló, Damià

    2012-01-01

    A fast on-line analytical method based on turbulent flow chromatography (TFC) in combination with tandem mass spectrometry has been applied for the first time for the analysis of eighteen perfluoroalkyl substances (PFASs), in cord blood. A simple and rapid sample pre-treatment was optimised consisting on protein precipitation of 100 μL of sample with acetonitrile (1:1) followed by centrifugation during 10 min. The method was adapted to be sensitive enough and robust with minimum sample injection volume requirements (20 μL). The optimised methodology presented method limits of detection (MLOD) between 0.031 and 0.76 μg/L, detection capabilities (CCα) in the range between 0.005 and 0.99 μg/L and decision limits (CCβ) ranging from 0.006 to 1.16 μg/L. The recoveries in blank blood were calculated by spiking experiments with a mixture of 18 PFASs and established between 70 and 126% for most of compounds. Isotopic dilution was carried out for quantification of selected analytes. In-house validation of this new approach was carried out according to the requirements in the 2002/657/EC Decision. Finally the good applicability of this new approach was proved by the analysis of 60 cord blood samples from two different Mediterranean cities, Barcelona (Spain) and Heraklion (Greece). Ions perfluorohexanesulfonate (PFHxS) and perfluorooctanesulfonate (PFOS) were found at highest concentration and the more frequently compounds were PFHxS, PFOS and perfluorooctanoic acid (PFOA). The newly developed method proved to be suitable for large-scale epidemiologic studies, and to the data on PFASs exposure during pregnancy. -- Highlights: ► An on-line method has been developed for the analysis of 18 perfluoroalkyl substances. ► The method is based on turbulent flow chromatography tandem mass spectrometry. ► The method was applied in 60 cord blood samples from 2 Mediterranean cities. ► Acidic compounds were more frequently found and the method was proved to be suitable for

  19. Analysis of perfluoroalkyl substances in cord blood by turbulent flow chromatography coupled to tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Llorca, Marta; Perez, Francisca [Department of Environmental Chemistry, IDAEA-CSIC, Barcelona (Spain); Farre, Marinella, E-mail: mfuqam@cid.csic.es [Department of Environmental Chemistry, IDAEA-CSIC, Barcelona (Spain); Agramunt, Silvia [Centre for Research in Environmental Epidemiology (CREAL), Barcelona (Spain); IMIM (Hospital del Mar Research Institute), Barcelona (Spain); Kogevinas, Manolis [Centre for Research in Environmental Epidemiology (CREAL), Barcelona (Spain); IMIM (Hospital del Mar Research Institute), Barcelona (Spain); CIBER Epidemiologia y Salud Publica (CIBERESP), Barcelona (Spain); National School of Public Health, Athens (Greece); Barcelo, Damia [Department of Environmental Chemistry, IDAEA-CSIC, Barcelona (Spain); Catalan Institute for Water Research (ICRA), Girona (Spain); King Saud University, Riyadh (Saudi Arabia)

    2012-09-01

    A fast on-line analytical method based on turbulent flow chromatography (TFC) in combination with tandem mass spectrometry has been applied for the first time for the analysis of eighteen perfluoroalkyl substances (PFASs), in cord blood. A simple and rapid sample pre-treatment was optimised consisting on protein precipitation of 100 {mu}L of sample with acetonitrile (1:1) followed by centrifugation during 10 min. The method was adapted to be sensitive enough and robust with minimum sample injection volume requirements (20 {mu}L). The optimised methodology presented method limits of detection (MLOD) between 0.031 and 0.76 {mu}g/L, detection capabilities (CC{alpha}) in the range between 0.005 and 0.99 {mu}g/L and decision limits (CC{beta}) ranging from 0.006 to 1.16 {mu}g/L. The recoveries in blank blood were calculated by spiking experiments with a mixture of 18 PFASs and established between 70 and 126% for most of compounds. Isotopic dilution was carried out for quantification of selected analytes. In-house validation of this new approach was carried out according to the requirements in the 2002/657/EC Decision. Finally the good applicability of this new approach was proved by the analysis of 60 cord blood samples from two different Mediterranean cities, Barcelona (Spain) and Heraklion (Greece). Ions perfluorohexanesulfonate (PFHxS) and perfluorooctanesulfonate (PFOS) were found at highest concentration and the more frequently compounds were PFHxS, PFOS and perfluorooctanoic acid (PFOA). The newly developed method proved to be suitable for large-scale epidemiologic studies, and to the data on PFASs exposure during pregnancy. -- Highlights: Black-Right-Pointing-Pointer An on-line method has been developed for the analysis of 18 perfluoroalkyl substances. Black-Right-Pointing-Pointer The method is based on turbulent flow chromatography tandem mass spectrometry. Black-Right-Pointing-Pointer The method was applied in 60 cord blood samples from 2 Mediterranean cities

  20. Hierarchical cluster analysis of technical replicates to identify interferents in untargeted mass spectrometry metabolomics.

    Science.gov (United States)

    Caesar, Lindsay K; Kvalheim, Olav M; Cech, Nadja B

    2018-08-27

    Mass spectral data sets often contain experimental artefacts, and data filtering prior to statistical analysis is crucial to extract reliable information. This is particularly true in untargeted metabolomics analyses, where the analyte(s) of interest are not known a priori. It is often assumed that chemical interferents (i.e. solvent contaminants such as plasticizers) are consistent across samples, and can be removed by background subtraction from blank injections. On the contrary, it is shown here that chemical contaminants may vary in abundance across each injection, potentially leading to their misidentification as relevant sample components. With this metabolomics study, we demonstrate the effectiveness of hierarchical cluster analysis (HCA) of replicate injections (technical replicates) as a methodology to identify chemical interferents and reduce their contaminating contribution to metabolomics models. Pools of metabolites with varying complexity were prepared from the botanical Angelica keiskei Koidzumi and spiked with known metabolites. Each set of pools was analyzed in triplicate and at multiple concentrations using ultraperformance liquid chromatography coupled to mass spectrometry (UPLC-MS). Before filtering, HCA failed to cluster replicates in the data sets. To identify contaminant peaks, we developed a filtering process that evaluated the relative peak area variance of each variable within triplicate injections. These interferent peaks were found across all samples, but did not show consistent peak area from injection to injection, even when evaluating the same chemical sample. This filtering process identified 128 ions that appear to originate from the UPLC-MS system. Data sets collected for a high number of pools with comparatively simple chemical composition were highly influenced by these chemical interferents, as were samples that were analyzed at a low concentration. When chemical interferent masses were removed, technical replicates clustered in