WorldWideScience

Sample records for microprobe mass analysis

  1. Using the ion microprobe mass analyser for trace element analysis

    Schilling, J.H.

    1978-01-01

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

  2. Data acquisition and analysis system for the ion microprobe mass analyzer

    Darby, D.M.; Cristy, S.S.

    1979-02-01

    A computer was interfaced to an ion microprobe mass analyzer for more rapid data acquisition and analysis. The interface is designed to allow data acquisition, independent of the computer. A large data analysis package was developed and implemented. Performance of the computerized system was evaluated and compared to manual operation

  3. Laser microprobe mass spectrometry: Potential and limitations for inorganic and organic micro-analysis. Pt. 2

    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.)

  4. Laser microprobe mass spectrometry: Potential and limitations for inorganic and organic micro-analysis. Pt. 1

    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.)

  5. Cometary and interstellar dust grains - Analysis by ion microprobe mass spectrometry and other techniques

    Zinner, Ernst

    1991-01-01

    A survey of microanalytical measurements on interplanetary dust particles (IDPs) and interstellar dust grains from primitive meteorites is presented. Ion-microprobe mass spectrometry with its capability to determine isotopic compositions of many elements on a micron spatial scale has played a special role. Examples are measurements of H, N, and O isotopes and refractory trace elements in IDPs; C, N, Mg, and Si isotopes in interstellar SiC grains; and C and N isotopes and H, N, Al, and Si concentrations in interstellar graphite grains.

  6. Materials analysis with a nuclear microprobe

    Maggiore, C.J.

    1980-01-01

    The ability to produce focused beams of a few MeV light ions from Van de Graaff accelerators has resulted in the development of nuclear microprobes. Rutherford backscattering, nuclear reactions, and particle-induced x-ray emission are used to provide spatially resolved information from the near surface region of materials. Rutherford backscattering provides nondestructive depth and mass resolution. Nuclear reactions are sensitive to light elements (Z < 15). Particle-induced x-ray analysis is similar to electron microprobe analysis, but 2 orders of magnitude more sensitive. The focused beams are usually produced with specially designed multiplets of magnetic quadrupoles. The LASL microprobe uses a superconducting solenoid as a final lens. The data are acquired by a computer interfaced to the experiment with CAMAC. The characteristics of the information acquired with a nuclear microprobe are discussed; the means of producing the beams of nuclear particles are described; and the limitations and applications of such systems are given

  7. Microprobe analysis in human pathology

    Baker, D.; Kupke, K.G.; Ingram, P.; Roggli, V.L.; Shelburne, J.D.

    1985-01-01

    This tutorial paper reviews the literature on the application of microprobe analysis to practical problems in diagnostic human pathology. The goal is to allow the reader ready access to the literature on specific clinical problems. Specimen preparation and commonly encountered artifacts are also considered. It is concluded that energy dispersive x-ray microanalysis and back-scattered electron imaging are at present the most generally useful microprobe techniques for clinical work, and are no longer solely research tools. The findings often have diagnostic, therapeutic, and/or legal implications. 332 references

  8. Microprobe analysis of human fibroblasts

    Allan, G.L.; Zhu, J.; Legge, G.J.F.

    1985-01-01

    The Melbourne Proton Microprobe has been used to study the copper content in human skin fibroblast cells derived from patients with the genetic disease Menkes Syndrome. Both normal and diseased cells have been studied to investigate any elemental differences occurring between the two cell types. This paper details the preparatory techniques necessary for individual cell analysis and presents the elemental information with a new three dimensional contour mapping technique. These maps are used to highlight elemental differences between normal and mutant fibroblasts. The work also confirms the expected copper excess found in the Menkes cell and indicates that the microprobe can be used for rapid identification of a Menkes carrier

  9. Ion microprobe mass analysis of plagioclase from 'non-mare' lunar samples

    Meyer, C., Jr.; Anderson, D. H.; Bradley, J. G.

    1974-01-01

    The ion microprobe was used to measure the composition and distribution of trace elements in lunar plagioclase, and these analyses are used as criteria in determining the possible origins of some nonmare lunar samples. The Apollo 16 samples with metaclastic texture and high-bulk trace-element contents contain plagioclase clasts with extremely low trace-element contents. These plagioclase inclusions represent unequilibrated relicts of anorthositic, noritic, or troctolitic rocks that have been intermixed as a rock flour into the KREEP-rich matrix of these samples. All of the plagioclase-rich inclusions which were analyzed in the KREEP-rich Apollo 14 breccias were found to be rich in trace elements. This does not seem to be consistent with the interpretation that the Apollo 14 samples represent a pre-Imbrium regolith, because such an ancient regolith should have contained many plagioclase clasts with low trace-element contents more typical of plagioclase from the pre-Imbrium crust. Ion-microprobe analyses for Ba and Sr in large plagioclase phenocrysts in 14310 and 68415 are consistent with the bulk compositions of these rocks and with the known distribution coefficients for these elements. The distribution coefficient for Li (basaltic liquid/plagioclase) was measured to be about 2.

  10. Biological analysis with a nuclear microprobe

    Cookson, J.A.; Legge, G.J.F.

    1975-01-01

    Most low-energy nuclear accelerators are now partly used on analytical studies in support of sciences other than nuclear physics. This paper gives a short review of such analytical techniques (X-ray analysis, elastic scattering analysis, nuclear reaction analysis, and the nuclear microprobe) with particular reference to biological applications and also emphasizes the role of the positional analysis that can be performed with a focused beam of ions - the nuclear microprobe. (author)

  11. Laser microprobe mass analysis (LAMMA) of aluminum and lead in fine roots and their ectomycorrhizal mantles of Norway spruce (Picea abies (L.) Karst.).

    Eeckhaoudt, S; Vandeputte, D; Van Praag, H; Van Grieken, R; Jacob, W

    1992-03-01

    Fine roots and ectomycorrhizal root tips were sampled in a Norway spruce (Picea abies (L.) Karst.) stand in the eastern part of the Belgian Ardennes. The cellular and partly subcellular localizations of aluminum and lead were identified by the micro-analytical laser microprobe mass analysis (LAMMA) technique. In fine roots with secondary structure, localization of aluminum was limited to the peripheral cell layers. Lead was found in the outer layers, and also in the primary phloem. Aluminum penetrated the mycorrhizal mantle, but lead was seldom detected in ectomycorrhizae.

  12. Analysis of corrosions-products in tissue samples near surgical implants by means of LAMMA (Laser Microprobe Mass Analyzer) and ICP-MS (Inductively Coupled Plasma Mass Spectrometer)

    Schlagenhaufen, C.

    1996-08-01

    In this work corrosion products of surgical implants in tissue samples were identified. For the characterization of the corrosion products the LAMMA 500 (Laser Microprobe Mass Analyzer) was used. Additional analysis were made with the ICP-MS (Inductively Coupled Plasma Mass Spectrometer) to determine the concentration of chromium, cobalt, nickel, and molybdenum in the tissues. In the first part several synthetic chromium- and molybdenum compounds were investigated with LAMMA. With the anionic mass spectra of the chromium-compounds it is possible to the oxidation state of chromium. The mass spectra of the synthetic compounds were used to identify, the compounds in the corrosion products. In the second part thin sections prepared from the tissue samples from the surrounding of the implants were analyzed. Several embedding and cutting methods were tested. Histological staining methods and LAMMA spectra were used to characterize the deposits in the tissue. Three different deposits were found in the tissue. In all tissues metal splinters from the implant were found. In most of the tissues iron-rich deposits were found, that were identified as iron-phosphate. As definitive corrosion products of the implant mixtures of chromium(III)phosphate, calcium molybdate, calcium phosphate and chromium(III) molybdate were identified. The ICP-MS results show in comparison to normal values, very high concentrations for chromium, nickel, cobalt and molybdenum. These results support the conclusions based on LAMMA results. The results of these investigations clearly indicate, that stainless steel implants, are not corrosion-resistant in the body. Relatively high amounts of the constituents, of the implant dissolved, and are deposited as solid compounds in the tissue next to the implant. (author)

  13. Microprobe analysis of carbon gradients

    Lamothe, M.; Convert, F.

    1987-01-01

    Problems arising in carbon analysis and how they are solved are presented: sample pollution limitation using cold trap and gas jet cleaning sample preparation, carbon content determination and calibration, automation and optimization. Examples given include concentration monitoring. Carbon homogeneity after complete cementation and decarburization by heat treatment. 6 refs, 14 figs [fr

  14. Looking into individual coffee beans during the roasting process: direct micro-probe sampling on-line photo-ionisation mass spectrometric analysis of coffee roasting gases.

    Hertz-Schünemann, Romy; Streibel, Thorsten; Ehlert, Sven; Zimmermann, Ralf

    2013-09-01

    A micro-probe (μ-probe) gas sampling device for on-line analysis of gases evolving in confined, small objects by single-photon ionisation time-of-flight mass spectrometry (SPI-TOFMS) was developed. The technique is applied for the first time in a feasibility study to record the formation of volatile and flavour compounds during the roasting process within (inside) or in the direct vicinity (outside) of individual coffee beans. A real-time on-line analysis of evolving volatile and semi-volatile organic compounds (VOC and SVOC) as they are formed under the mild pyrolytic conditions of the roasting process was performed. The soft-ionisation mass spectra depict a molecular ion signature, which is well corresponding with the existing knowledge of coffee roasting and evolving compounds. Additionally, thereby it is possible to discriminate between Coffea arabica (Arabica) and Coffea canephora (Robusta). The recognized differences in the roasting gas profiles reflect the differences in the precursor composition of the coffee cultivars very well. Furthermore, a well-known set of marker compounds for Arabica and Robusta, namely the lipids kahweol and cafestol (detected in their dehydrated form at m/z 296 and m/z 298, respectively) were observed. If the variation in time of different compounds is observed, distinctly different evolution behaviours were detected. Here, phenol (m/z 94) and caffeine (m/z 194) are exemplary chosen, whereas phenol shows very sharp emission peaks, caffeine do not have this highly transient behaviour. Finally, the changes of the chemical signature as a function of the roasting time, the influence of sampling position (inside, outside) and cultivar (Arabica, Robusta) is investigated by multivariate statistics (PCA). In summary, this pilot study demonstrates the high potential of the measurement technique to enhance the fundamental knowledge of the formation processes of volatile and semi-volatile flavour compounds inside the individual coffee bean.

  15. Microprobe channeling analysis of pyrite crystals

    Jamieson, D.N.; Ryan, C.G.

    1992-01-01

    Nuclear microprobe analysis has provided much useful information about the composition of microscopic inclusions in minerals, mainly through the use of Particle Induced X-ray Emission (PIXE). However this technique, while powerful, does not provide any direct information about the chemical state, in particular the lattice location, of the elements in the mineral. This information is often of crucial importance in understanding the ore genesis. The technique of ion channeling may be used to identify lattice location, but many minerals occur as microscopic crystals. Therefore it is necessary to utilize a nuclear microprobe with the technique of Channeling Contrast Microscopy (CCM). As many minerals contain interesting trace elements, it is necessary to measure both the yield of backscattered particles and the induced x-rays to get a clear picture of the lattice location of the elements in the crystal. CCM with PIXE was used to analyse natural pyrite crystals containing a variety of substitutional and non-substitutional elements and natural pyrite crystals from a gold bearing ore. In the latter case, evidence was obtained for two habits for Au in the 400 μm crystals: one as inclusions of Au rich minerals, the other substituted on the pyrite lattice sites. 31 refs., 3 tabs., 6 figs

  16. Electron microprobe analysis of tantalum--nitride thin films

    Stoltz, D.L.; Starkey, J.P.

    1979-06-01

    Quantitative chemical analysis of 500- and 2000-angstrom tantalum--nitride films on glass substrates has been accomplished using an electron microprobe x-ray analyzer. In order to achieve this analysis, modifications to the microprobe were necessary. A description of the calibration procedure, the method of analysis, and the quantitative results are discussed

  17. Ion microprobe analysis of metallic pigments

    Pelicon, P.; Simcic, J.; Budnar, M.; Klanjsek-Gunde, M.; Kunavaer, M.

    2001-01-01

    Full text: Metallic paints consist of metallic flakes dispersed m a resinous binder, i.e. a light-element polymer matrix. The spatial distribution and orientation of metallic flakes inside the matrix determines the covering efficiency of the paint, glossiness, and its angular-dependent properties such as lightness flop or color flop (two-tone). Such coatings are extensively used for a functional (i.e. security) as well as decorative purpose. The ion microbeam analysis of two types of silver paint with imbedded metallic flake has been performed to test the ability of the ion microbeam spectroscopic methods on this type of samples. The average sizes of the aluminium flakes were 23 (size distribution 10-37) and 49 (size distribution 34-75) micrometers, respectively. The proton beam with the size of 2x2 micrometers at Ljubljana ion microprobe has been used to scan the surface of the pigments. PIXE mapping of Al Kα map shows lateral distribution of the aluminum flakes, whereas the RBS slicing method reveals tomographic image of the flakes in uppermost 5 micrometers of the pigment layer. The flake distribution in the larger layer depths has been accessed by RBS analysis in a point mode. (author)

  18. Synchrotron radiation microprobe quantitative analysis method for biomedical specimens

    Xu Qing; Shao Hanru

    1994-01-01

    Relative changes of trace elemental content in biomedical specimens are obtained easily by means of synchrotron radiation X-ray fluorescence microprobe analysis (SXRFM). However, the accurate assignment of concentration on a g/g basis is difficult. Because it is necessary to know both the trace elemental content and the specimen mass in the irradiated volume simultaneously. the specimen mass is a function of the spatial position and can not be weighed. It is possible to measure the specimen mass indirectly by measuring the intensity of Compton scattered peak for normal XRF analysis using a X-ray tube with Mo anode, if the matrix was consisted of light elements and the specimen was a thin sample. The Compton peak is not presented in fluorescence spectrum for white light SXRFM analysis. The continuous background in the spectrum was resulted from the Compton scattering with a linear polarization X-ray source. Biomedical specimens for SXRFM analysis, for example biological section and human hair, are always a thin sample for high energy X-ray, and they consist of H,C,N and O etc. light elements, which implies a linear relationship between the specimen mass and the Compton scattering background in the high energy region of spectrum. By this way , it is possible to carry out measurement of concentration for SXRFM analysis

  19. A digital squarer system for positive mass identification on the ARL ion microprobe mass analyser

    Woods, K.N.; Grant, L.D.V.; Rawsthorne, E.D.; Strydom, H.J.; Gries, W.H.

    1984-01-01

    The original analogue squarer for mass scale linearisation in the Ion Microprobe Mass Analyser (IMMA) has been replaced by a programmable digital squarer system which permits reliable mass number identification throughout the tested range 1 to 240. The digital squarer provides signals to both a digital direct reading mass number display and to an X-Y recorder where it provides a linear mass scale correct to within 0,3 mass units. An additional output to a computer can provide binary or BCD mass number data

  20. U/Th dating by SHRIMP RG ion-microprobe mass spectrometry using single ion-exchange beads

    Bischoff, J.L.; Wooden, J.; Murphy, F.; Williams, Ross W.

    2005-01-01

    We present a new analytical method for U-series isotopes using the SHRIMP RG (Sensitive High mass Resolution Ion MicroProbe) mass spectrometer that utilizes the preconcentration of the U-series isotopes from a sample onto a single ion-exchange bead. Ion-microprobe mass spectrometry is capable of producing Th ionization efficiencies in excess of 2%. Analytical precision is typically better than alpha spectroscopy, but not as good as thermal ionization mass spectroscopy (TIMS) and inductively coupled plasma multicollector mass spectrometry (ICP-MS). Like TIMS and ICP-MS the method allows analysis of small samples sizes, but also adds the advantage of rapidity of analysis. A major advantage of ion-microprobe analysis is that U and Th isotopes are analyzed in the same bead, simplifying the process of chemical separation. Analytical time on the instrument is ???60 min per sample, and a single instrument-loading can accommodate 15-20 samples to be analyzed in a 24-h day. An additional advantage is that the method allows multiple reanalyses of the same bead and that samples can be archived for reanalysis at a later time. Because the ion beam excavates a pit only a few ??m deep, the mount can later be repolished and reanalyzed numerous times. The method described of preconcentrating a low concentration sample onto a small conductive substrate to allow ion-microprobe mass spectrometry is potentially applicable to many other systems. Copyright ?? 2005 Elsevier Ltd.

  1. Multidimensional elemental analysis with the Sandia nuclear microprobe

    Doyle, B.L.

    1988-01-01

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

  2. Examination of Laser Microprobe Vacuum Ultraviolet Ionization Mass Spectrometry with Application to Mapping Mars Returned Samples

    Burton, A. S.; Berger, E. L.; Locke, D. R.; Lewis, E. K.; Moore, J. F.

    2018-04-01

    Laser microprobe of surfaces utilizing a two laser setup whereby the desorption laser threshold is lowered below ionization, and the resulting neutral plume is examined using 157nm Vacuum Ultraviolet laser light for mass spec surface mapping.

  3. Proton microprobe analysis of pancreatic. beta. cells

    Lindh, U [Uppsala Univ. (Sweden). Gustaf Werner Inst.; Juntti-Berggren, L; Berggren, P O; Hellman, B [Uppsala Univ. (Sweden)

    1985-01-01

    Freeze-dried pancreas sections from obese hyperglycemic mice were subjected to proton bombardment and the elemental contents in the ..beta.. cells and the exocrine part were obtained from the characteristic X-rays emitted. Quantitative data were provided for 18 different elements. The mole ratio between K and Na exceeded 10, implying that neither the sample preparation nor the irradiation had induced significant diffuse changes. With the demonstration of this high K/Na ratio it seems likely that also the ..beta.. cells are equipped with an efficient Na/sup +//K/sup +/ pump. The ..beta.. cells contained about 70 mmoles Cl per litre cell water. Observed amounts of Ca and Mg were equivalent to those previously recorded by electrothermal atomic absorption spectroscopy. The significant role of Zn for the storage of insulin was emphasized by the demonstration of 3 times as much of this element in the ..beta.. cells as compared with the exocrine pancreas. In addition, the sensitivity of the proton microprobe enabled measurements of various trace elements such as Rb, Cr, Cu, Al and Pb not previously demonstrated in the pancreatic ..beta.. cells.

  4. U and Pb isotope analysis of uraninite and galena by ion microprobe

    Evins, L.Z.; Sunde, T.; Schoeberg, H. [Swedish Museum of Natural History, Stockholm (Sweden). Laboratory for Isotope Geology; Fayek, M. [Univ. of Tennessee, Knoxville, TN (United States). Dept. of Geological Sciences

    2001-10-01

    Accurate isotopic analysis of minerals by ion microprobe, or SIMS (Secondary Ion Mass Spectrometry) usually requires a standard to correct for instrumental mass bias effects that occur during analysis. We have calibrated two uraninite crystals and one galena crystal to be used as ion probe standards. As part of this study we describe the analytical procedures and problems encountered while trying to establish fractionation factors for U and Pb isotopes measured in galena and uraninite. Only the intra-element isotopic mass fractionation is considered and not the interelement fractionation. Galena and uraninite were analysed with TIMS (Thermal Ionisation Mass Spectrometry) prior to SIMS. One uraninite crystal (P88) comes from Sweden and is ca 900 Ma old, the other from Maine, USA (LAMNH-30222) and is ca 350 Ma old. The galena sample comes from the Paleoproterozoic ore district Bergslagen in Sweden. SIMS analyses were performed at two different laboratories: the NORDSM facility in Stockholm, which has a high resolution Cameca IMS 1270 ion microprobe, and the Oak Ridge National Laboratory (ORNL) in Tennessee, which has a Cameca IMS 4f ion microprobe. The results show that during the analysis of galena, Pb isotopes fractionate in favour of the lighter isotope by as much as 0.5%/amu. A Pb isotope fractionation factor for uraninite was more difficult to calculate, probably due to the formation of hydride interferences encountered during analysis with the Cameca IMS 1270 ion microprobe. However, drying the sample in vacuum prior to analysis, and using high-energy filtering and a cold trap during analysis can minimise these hydride interferences. A large fractionation of U isotopes of ca 1.4%/amu in favour of the lighter isotope was calculated for uraninite.

  5. U and Pb isotope analysis of uraninite and galena by ion microprobe

    Evins, L.Z.; Sunde, T.; Schoeberg, H.; Fayek, M.

    2001-10-01

    Accurate isotopic analysis of minerals by ion microprobe, or SIMS (Secondary Ion Mass Spectrometry) usually requires a standard to correct for instrumental mass bias effects that occur during analysis. We have calibrated two uraninite crystals and one galena crystal to be used as ion probe standards. As part of this study we describe the analytical procedures and problems encountered while trying to establish fractionation factors for U and Pb isotopes measured in galena and uraninite. Only the intra-element isotopic mass fractionation is considered and not the interelement fractionation. Galena and uraninite were analysed with TIMS (Thermal Ionisation Mass Spectrometry) prior to SIMS. One uraninite crystal (P88) comes from Sweden and is ca 900 Ma old, the other from Maine, USA (LAMNH-30222) and is ca 350 Ma old. The galena sample comes from the Paleoproterozoic ore district Bergslagen in Sweden. SIMS analyses were performed at two different laboratories: the NORDSM facility in Stockholm, which has a high resolution Cameca IMS 1270 ion microprobe, and the Oak Ridge National Laboratory (ORNL) in Tennessee, which has a Cameca IMS 4f ion microprobe. The results show that during the analysis of galena, Pb isotopes fractionate in favour of the lighter isotope by as much as 0.5%/amu. A Pb isotope fractionation factor for uraninite was more difficult to calculate, probably due to the formation of hydride interferences encountered during analysis with the Cameca IMS 1270 ion microprobe. However, drying the sample in vacuum prior to analysis, and using high-energy filtering and a cold trap during analysis can minimise these hydride interferences. A large fractionation of U isotopes of ca 1.4%/amu in favour of the lighter isotope was calculated for uraninite

  6. X-ray Microprobe for Fluorescence and Diffraction Analysis

    Ice, G.E.

    2005-01-01

    X-ray diffraction (see unit 1.1) and x-ray excited fluorescence analysis are powerful techniques for the nondestructive measurement of crystal structure and chemical composition. X-ray fluorescence analysis is inherently nondestructive with orders of magnitude lower power deposited for the same detectable limit as with fluorescence excited by charged particle probes (Sparks, 1980). X-ray diffraction analysis is sensitive to crystal structure with orders-of-magnitude greater sensitivity to crystallographic strain than electron probes (Rebonato, et al. 1989). When a small-area x-ray microbeam is used as the probe, chemical composition (Z>14), crystal structure, crystalline texture, and crystalline strain distributions can be determined. These distributions can be studied both at the surface of the sample and deep within the sample (Fig. 1). Current state-of-the-art can achieve an ∼1 mm-D x-ray microprobe and an ∼0.1 mm-D x-ray microprobe has been demonstrated (Bilderback, et al., 1994). Despite their great chemical and crystallographic sensitivities, x-ray microprobe techniques have until recently been restricted by inefficient x-ray focusing optics and weak x-ray sources; x-ray microbeam analysis was largely superseded by electron techniques in the 50's. However, interest in x-ray microprobe techniques has now been revived (Howells, et al., 1983; Ice and Sparks, 1984; Chevallier, et al., 1997; Riekel 1992; Thompson, el al., 1992; and Making and Using... 1997) by the development of efficient x-ray focusing optics and ultra-high intensity synchrotron x-ray sources (Buras and Tazzari, 1984; Shenoy, et al., 1988). These advances have increased the achievable microbeam flux by more than 11 orders of magnitude (Fig. 2) (Ice, 1997); the flux in a tunable 1 mm-D beam on a 'so called' 3rd-generation synchrotron source such as the APS can exceed the flux in a fixed-energy mm2 beam on a conventional source. These advances make x-ray microfluorescence and x

  7. On the identification of carbonaceous aerosols via 14C accelerator mass spectrometry, and laser microprobe mass spectrometry

    Currie, L.A.; Fletcher, R.A.; Klouda, G.A.

    1987-01-01

    Carbon isotopic measurements ( 12 C, 14 C), derived from chemical measurements of total carbon plus AMS measurements of 14 C/ 12 C have become an accepted means for estimating fossil and contemporary carbon source contributions to atmospheric carbon. Because of the limited sensitivity of these techniques, however, such measurements are restricted to 'bulk' samples comprising at least 10-100 μg of carbon. Laser microprobe mass spectrometry (LMMS) offers an important complementary opportunity to investigate the chemical nature of individual particles as small as 0.1 μm in diameter. Although there is little hope to measure 14 C/ 12 C in such small samples, the compositional and structural information available with the laser microprobe is of interest for possible source discrimination. Also, the analysis of individual particles, which may reflect individual sources, yields significant potential increases in spatial, temporal and source resolution, in comparison to bulk sample analysis. Results of our exploratory investigation of known sources of carbonaceous particles, using LMMS, are presented. By applying multivariate techniques to laser mass spectra of soot from the combustion of heptane and wood, we found striking differences in the alkali metals (notably potassium) in the positive ion mass spectra. For ambient particles, 14 C has proved to be a crucial adjunct for the development and validation of the LMMS approach to single particle source assignment via carbon cluster pattern recognition. The combined techniques offer great promise for objective modeling (number and types of carbon sources) and for extension of the dichotomous carbon apportionment (fossil, contemporary) to subclasses such as soot from wood and agricultural burning, and that from coal and petroleum combustion. (orig.)

  8. Microprobe PIXE analysis and EDX analysis on the brain of patients with Alzheimer's disease

    Yumoto, S.; Horino, Y.; Mokuno, Y.; Fujii, K.; Kakimi, S.; Mizutani, T.; Matsushima, H.; Ishikawa, A.

    1996-01-01

    To investigate the cause of Alzheimer's disease (senile dementia of Alzheimer's disease type), we examined aluminium (Al) in the brain (hippocampus) of patients with Alzheimer's disease using heavy ion (5 MeV Si 3+ ) microprobe particle-induced X-ray emission (PIXE) analysis. Heavy ion microprobes (3 MeV Si 2+ ) have several times higher sensitivity for Al detection than 2 MeV proton microprobes. We also examined Al in the brain of these patients by energy dispersive X-ray spectroscopy (EDX). (1) Al was detected in the cell nuclei isolated from the brain of patients with Alzheimer's disease using 5 MeV Si 3+ microprobe PIXE analysis, and EDX analysis. (2) EDX analysis demonstrated high levels of Al in the nucleolus of nerve cells in frozen sections prepared from the brain of these patients. Our results support the theory that Alzheimer's disease is caused by accumulation of Al in the nuclei of brain cells. (author)

  9. Analysis of biological materials using a nuclear microprobe

    Mulware, Stephen Juma

    The use of nuclear microprobe techniques including: Particle induced x-ray emission (PIXE) and Rutherford backscattering spectrometry (RBS) for elemental analysis and quantitative elemental imaging of biological samples is especially useful in biological and biomedical research because of its high sensitivity for physiologically important trace elements or toxic heavy metals. The nuclear microprobe of the Ion Beam Modification and Analysis Laboratory (IBMAL) has been used to study the enhancement in metal uptake of two different plants. The roots of corn (Zea mays) have been analyzed to study the enhancement of iron uptake by adding Fe (II) or Fe(III) of different concentrations to the germinating medium of the seeds. The Fe uptake enhancement effect produced by lacing the germinating medium with carbon nanotubes has also been investigated. The aim of this investigation is to ensure not only high crop yield but also Fe-rich food products especially from calcareous soil which covers 30% of world's agricultural land. The result will help reduce iron deficiency anemia, which has been identified as the leading nutritional disorder especially in developing countries by the World Health Organization. For the second plant, Mexican marigold (Tagetes erecta ), the effect of an arbuscular mycorrhizal fungi (Glomus intraradices ) for the improvement of lead phytoremediation of lead contaminated soil has been investigated. Phytoremediation provides an environmentally safe technique of removing toxic heavy metals (like lead), which can find their way into human food, from lands contaminated by human activities like mining or by natural disasters like earthquakes. The roots of Mexican marigold have been analyzed to study the role of arbuscular mycorrhizal fungi in enhancement of lead uptake from the contaminated rhizosphere.

  10. Milliprobe and microprobe analysis of gold items of ancient jewellery

    Demortier, G.; Hackens, T.

    It has long been accepted that the presence of cadmium implies a condemnation of the authenticity of an ancient gold object, or at least, of the part of the object where the cadmium is detected. An analysis in Paris of a recently excavated object from Roman times has shown cadmium. Meanwhile, systematic observations were made at L.A.R.N. on objects dating from Hellenistic to Byzantine times with different given origins (objects from a museum and from private collections). By using PIXE with a 3 MeV proton milliprobe (700 μm beam diameter) in a non vacuum geometry, relative amounts of copper, silver, cadmium and gold at the surface of more than 30 gold objects expected to be ancient have been determined. Traces or significant concentrations of cadmium have been detected at several points on or in the neighbourhood of solders on many objects which seem to be from Roman to early Byzantine times. Cadmium concentrations range between 2 to 100 parts per thousand. This range of variations and the relative concentrations of Au, Ag, Cu and Cd at the surface of the objects studied are often different from the figures obtained during analyses of modern soldering alloys. Experiments with the L.A.R.N. proton microprobe (5 μm x 10 μm area) allow a still better topographical resolution and more significative comparison of the relative amounts of the elements of interest in modern soldering alloys and supposedly old solders. The usefulness of the microprobe is demonstrated. (author)

  11. Proton microprobe analysis of zinc in skeletal tissues

    Doty, S. B.; Jones, K. W.; Kraner, H. W.; Shroy, R. E.; Hanson, A. L.

    1981-03-01

    A proton microprobe with windowless exit port has been used to study zinc distributions in various types of skeletal tissues. The use of an external beam facilitated positioning of the targets for examination of particular points of interest. The proton microprobe is uniquely suited to this work since it combines high sensitivity for zinc determination in thick samples with good spatial resolution. Our measurements on rat and rabbit Achilles tendon showed a significant increase in zinc concentrations as the beam moved from the unmineralized collagen into the mineralized attachment site. Cartilage gave a similar result, with calcified cartilage having a greater zinc level than the articular surface on unmineralized epiphyseal cartilage.

  12. Proton microprobe analysis of zinc in skeletal tissues

    Doty, S.B.; Jones, K.W.; Kraner, H.W.; Shroy, R.E.; Hanson, A.L.

    1980-06-01

    A proton microprobe with windowless exit port was used to study zinc distributions in various types of skeletal tissues. The use of an external beam facilitated positioning of the targets for examination of particular points of interest. The proton microprobe is uniquely suited to this work since it combines high sensitivity for zinc determinations in thick samples with good spatial resolution. Measurements on rat and rabbit Achilles tendon showed a significant increase in zinc concentrations as the beam moved from the unmineralized collagen into the mineralized attachment site. Cartilage gave a similar result, with calcified cartilage having a greater zinc level than the articular surface on unmineralized epiphyseal cartilage

  13. Elemental composition of paint cross sections by nuclear microprobe analysis

    Nens, B.; Trocellier, P.; Engelmann, C.; Lahanier, C.

    1982-09-01

    Physico-chemical characterization of pigments used in artistic painting give precious indications on age of paintings and sometimes on geographical origin of ores. After recalling the principle of protons microprobe, first results obtained by microanalysis of painting cross sections for non destructive microanalysis of impurities in white lead are given [fr

  14. Microprobe PIXE analysis and EDX analysis on the brain of patients with Alzheimer`s disease

    Yumoto, S. [Tokyo Univ. (Japan). Faculty of Medicine; Horino, Y.; Mokuno, Y.; Fujii, K.; Kakimi, S.; Mizutani, T.; Matsushima, H.; Ishikawa, A.

    1996-12-31

    To investigate the cause of Alzheimer`s disease (senile dementia of Alzheimer`s disease type), we examined aluminium (Al) in the brain (hippocampus) of patients with Alzheimer`s disease using heavy ion (5 MeV Si{sup 3+}) microprobe particle-induced X-ray emission (PIXE) analysis. Heavy ion microprobes (3 MeV Si{sup 2+}) have several times higher sensitivity for Al detection than 2 MeV proton microprobes. We also examined Al in the brain of these patients by energy dispersive X-ray spectroscopy (EDX). (1) Al was detected in the cell nuclei isolated from the brain of patients with Alzheimer`s disease using 5 MeV Si{sup 3+} microprobe PIXE analysis, and EDX analysis. (2) EDX analysis demonstrated high levels of Al in the nucleolus of nerve cells in frozen sections prepared from the brain of these patients. Our results support the theory that Alzheimer`s disease is caused by accumulation of Al in the nuclei of brain cells. (author)

  15. Applications of heavy ion microprobe for single event effects analysis

    Reed, Robert A.; Vizkelethy, Gyorgy; Pellish, Jonathan A.; Sierawski, Brian; Warren, Kevin M.; Porter, Mark; Wilkinson, Jeff; Marshall, Paul W.; Niu, Guofu; Cressler, John D.; Schrimpf, Ronald D.; Tipton, Alan; Weller, Robert A.

    2007-01-01

    The motion of ionizing-radiation-induced rogue charge carriers in a semiconductor can create unwanted voltage and current conditions within a microelectronic circuit. If sufficient unwanted charge or current occurs on a sensitive node, a variety of single event effects (SEEs) can occur with consequences ranging from trivial to catastrophic. This paper describes the application of heavy ion microprobes to assist with calibration and validation of SEE modeling approaches

  16. Laser ablation microprobe inductively coupled plasma mass spectrometry study on diffusion of uranium into cement materials

    Sugiyama, D.; Chida, T.; Cowper, M.

    2008-01-01

    The diffusion of uranium (U(VI)) in solid cement monoliths of ordinary portland cement (OPC) and low-heat portland cement containing 30 wt.% fly ash (FAC) was measured by an in-diffusion technique. Detailed sharp depth profiles of uranium in the solid cement matrices were successively and quantitatively measured using laser ablation microprobe inductively coupled plasma mass spectrometry (LAMP-ICP-MS), and the apparent (D a ) and effective (D e ) diffusion coefficient of uranium in cement matrix were calculated as: D a =∝ 4 x 10 -16 m 2 s -1 and D e =∝ 3 x 10 -11 m 2 s -1 for OPC, and D a =∝ 2 x 10 -17 m 2 s -1 and D e =∝ 6 x 10 -13 m 2 s -1 for FAC. (orig.)

  17. Proton microprobe analysis of zinc in skeletal tissues

    Doty, S.B.; Jones, K.W.; Kraner, H.W.; Shroy, R.E.; Hanson, A.L.

    1981-01-01

    A proton microprobe with windowless exit port has been used to study zinc distributions in various types of skeletal tissues. The use of an external beam facilitated positioning of the targets for examination of particular points of interest. The proton micorprobe is uniquely suited to this work since it combines high sensitivity for zinc determinations in thick samples with good spatial resolution. Our measurements on rat and rabbit Achilles tendon showed a significant increase in zinc concentrations as the beam moved from the unmineralized collagen into the mineralized attachment site. Cartilage gave a similar result, with calcified cartilage having a greater zinc level than the articular surface on unmineralized epiphyseal cartilage. (orig.)

  18. Cryosystem for cathodoluminescence investigations by means of electron microprobe analysis

    Schreiber, J.

    1982-01-01

    A cryosystem is presented which has been designed as auxiliary equipment for electron beam microprobes used in cathodoluminescence studies. The sample holder temperature is adjustable down to 66 K with an accuracy of 0.5 K. Finally, experimental results (transmission spectra and cathodoluminescence spectra of N-doped GaP epitaxial layers at 80 K; changes in microscopic cathodoluminescence distribution at small angle grain boundaries at the (0001) plane of CdS during temperature decrease from 300 to 80 K) obtained by means of the described measuring equipment are given for illustration

  19. Microprobe analysis of teeth by synchrotron radiation: environmental contamination

    Pinheiro, T.; Carvalho, M.L.; Casaca, C.; Barreiros, M.A.; Cunha, A.S.; Chevallier, P.

    1999-01-01

    An X-ray fluorescence set-up with microprobe capabilities, installed at the Laboratoire pour l'Utilisation du Rayonnement Electromagnetique (LURE) synchrotron (France) was used for elemental determination in teeth. To evaluate the influence of living habits in dental elemental composition nine teeth collected post-mortem were analysed, five from a miner and four from a fisherman. All teeth from the fisherman were healthy. From the miner some teeth were carious and one of them was filled with metallic amalgam. Teeth were sliced under the vertical plane and each slice was scanned from the root to the enamel for elemental profile determination. The synchrotron microprobe resolution was of 100 μm and incident photons of 18 keV energy were used. The elemental concentration values found suggest heterogeneity of the teeth material. Moreover, the distinct profiles for Mn, Sr, Br and Pb were found when teeth from the miner and from the fisherman are compared which can be associated with dietary habits and environmental influence. Higher concentrations of Mn and Sr were found for the fisherman teeth. In addition, Br was only observed in this group of teeth. Pb levels are higher for the miner teeth in particular for dentine regions. The influence of amalgam, such as, increase of Zn and Hg contents in the teeth material, is only noticed for the immediate surroundings of the treated cavity

  20. Nuclear microprobe analysis of the standard reference materials

    Jaksic, M.; Fazinic, S.; Bogdanovic, I.; Tadic, T.

    2002-01-01

    Most of the presently existing Standard Reference Materials (SRM) for nuclear analytical methods are certified for the analyzed mass of the order of few hundred mg. Typical mass of sample which is analyzed by PIXE or XRF methods is very often below 1 mg. By the development of focused proton or x-ray beams, masses which can be typically analyzed go down to μg or even ng level. It is difficult to make biological or environmental SRMs which can give desired homogeneity at such low scale. However, use of fundamental parameter quantitative evaluation procedures (absolute method), minimize needs for SRMs. In PIXE and micro PIXE setup at our Institute, fundamental parameter approach is used. For exact calibration of the quantitative analysis procedure just one standard sample is needed. In our case glass standards which showed homogeneity down to micron scale were used. Of course, it is desirable to use SRMs for quality assurance, and therefore need for homogenous materials can be justified even for micro PIXE method. In this presentation, brief overview of PIXE setup calibration is given, along with some recent results of tests of several SRMs

  1. Nuclear microprobe analysis of lead profile in crocodile bones

    Orlic, I. E-mail: ivo@ansto.gov.au; Siegele, R.; Hammerton, K.; Jeffree, R.A.; Cohen, D.D

    2003-09-01

    Elevated concentrations of lead were found in Australian free ranging saltwater crocodile (Crocodylus porosus) bone and flesh. Lead shots were found as potential source of lead in these animals. ANSTO's heavy ion nuclear microprobe was used to measure the distribution of Pb in a number of bones and osteoderms. The aim was to find out if elevated Pb concentration remains in growth rings and if the concentration is correlated with the blood levels recorded at the time. Results of our study show a very distinct distribution of accumulated Pb in bones and osteoderms as well as good correlation with the level of lead concentration in blood. To investigate influence of ion species on detection limits measurements of the same sample were performed by using 3 MeV protons, 9 MeV He ions and 20 MeV carbon ions. Peak to background ratios, detection limits and the overall 'quality' of obtained spectra are compared and discussed.

  2. Nuclear micro-probe analysis of Arabidopsis thaliana leaves

    Ager, F.J.; Ynsa, M.D.; Dominguez-Solis, J.R.; Lopez-Martin, M.C.; Gotor, C.; Romero, L.C.

    2003-01-01

    Phytoremediation is a cost-effective plant-based approach for remediation of soils and waters which takes advantage of the remarkable ability of some plants to concentrate elements and compounds from the environment and to metabolize various molecules in their tissues, such as toxic heavy metals and organic pollutants. Nowadays, phytoremediation technology is becoming of paramount importance when environmental decontamination is concerned, due to the emerging knowledge of its physiological and molecular mechanisms and the new biological and engineering strategies designed to optimize and improve it. In addition, the feasibility of using plants for environmental cleanup has been confirmed by many different trials around the world. Arabidopsis thaliana plants can be used for basic studies to improve the technology on phytoremediation. Making use of nuclear microscopy techniques, in this paper we study leaves of wild type and transgenic A. thaliana plants grown in a cadmium-rich environment under different conditions. Micro-PIXE, RBS and SEM analyses, performed on the scanning proton micro-probe at the CNA in Seville (Spain), prove that cadmium is preferentially sequestered in the central region of epidermal trichome and allow comparing the effects of genetic modifications

  3. Dedicated accelerator and microprobe line

    Malmqvist, K.G.; Hylten, G.; Hult, M.; Haakansson, K.; Knox, J.M.; Larsson, N.P.O.; Nilsson, C.; Pallon, J.; Schofield, R.; Swietlicki, E.; Tapper, U.A.S.; Yang Changyi

    1993-01-01

    The development of a dedicated facility for nuclear microprobe analysis and the experiences from using it are discussed. The general properties of the present Lund nuclear microprobe will be described and the advantages of using a dedicated accelerator discussed. (orig.)

  4. IMAP: A complete Ion Micro-Analysis Package for the nuclear microprobe

    Antolak, A.J.; Hildner, M.L.; Morse, D.H.; Bench, G.S.

    1993-01-01

    Microprobe techniques using scanned, focused MeV ions are routinely used in Livermore for materials characterization. Comprehensive data analysis with these techniques is accomplished with the computer software package IMAP, for Ion Micro-Analysis Package. IMAP consists of a set of command language procedures for data processing and quantitative spectral analysis. Deconvolution of the data is achieved by spawning sub-processes within IMAP which execute analysis codes for each specific microprobe technique. IMAP is structured to rapidly analyze individual spectra or multi-dimensional data blocks which classify individual events by the two scanning dimensions, the energy of the detected radiation and, when necessary, one sample rotation dimension. Several examples are presented to demonstrate the utility of the package

  5. False colour backscatter electron images and their application during electron microprobe analysis of ores and host rocks

    Cousens, D.R.; French, D.H.; Ramsden, A.R.

    1989-01-01

    The limited contrast range of conventional black and white imaging does not enable full use to be made of the dynamic range of the video signal obtained from a scanning electron microscope or microprobe. The use of false colour substantially increases the information that can be derived from such images enabling relationships to be displayed that cannot be observed in black and white. This capability is now used extensively in combination with quantitative electron microprobe analysis as a research tool for ore characterization and host rocks studies related to minerals exploration in the CSIRO Div.sion of Exploration Geoscience. Thus the CAMEBAX scanning electron microprobe has been modified to allow digital images acquisition and software (IMAGE) developed which allows false colour backscatter electron (BSE) images to be obtained during the course of routine electron microprobe analysis. 1 fig

  6. Redeposition of sputtered material in a glow-discharge lamp measured by means of an ion microprobe mass analyser

    Ferreira, N.P.; Bueger, P.A.

    1978-01-01

    The redeposition of sputtered material on the target in a Grimm-type glow-discharge lamp was studied by means of an ion microprobe mass analyser (IMMA) using 16 O 2 + ions as bombarding species. The target was an aluminium disc with a cylindrical copper insertion, one mm in diameter. The lamp was operated at currents of 50 mA and 100 mA and a voltage of 1200 V. It is estimated that 17% of the copper atoms sputtered are redeposited and may be resputtered. (orig.) [de

  7. Electron Microprobe

    Federal Laboratory Consortium — The JEOL JXA-8600 is a conventional hairpin filament thermal emission electron microprobe that is more than 20 years old. It is capable of performing qualitative and...

  8. Application of tomographic techniques to two-dimensional surface analysis using the Harwell nuclear microprobe

    Huddleston, J.; Hutchinson, I.G.; Pierce, T.B.

    1983-01-01

    Nuclear methods of surface analysis are discussed briefly, and the circumstances are described in which a two-dimensional analysis of the sample surface is desirable to enable the surface composition to be mapped accurately. Tomographic techniques of data manipulation are outlined. Data acquisition in the present case is performed by moving the sample in a defined sequence of positions, at each of which analytical data are gathered by the proton microprobe. The method and equipment are outlined. Data processing leading to the reconstruction of the image is summarised. (U.K.)

  9. The new confocal heavy ion microprobe beamline at ANSTO: The first microprobe resolution tests and applications for elemental imaging and analysis

    Pastuovic, Z.; Siegele, R.; Cohen, D. D.; Mann, M.; Ionescu, M.; Button, D.; Long, S.

    2017-08-01

    The Centre for Accelerator Science facility at ANSTO has been expanded with the new NEC 6 MV ;SIRIUS; accelerator system in 2015. In this paper we present a detailed description of the new nuclear microprobe-Confocal Heavy Ion Micro-Probe (CHIMP) together with results of the microprobe resolution testing and the elemental analysis performed on typical samples of mineral ore deposits and hyper-accumulating plants regularly measured at ANSTO. The CHIMP focusing and scanning systems are based on the OM-150 Oxford quadrupole triplet and the OM-26 separated scan-coil doublet configurations. A maximum ion rigidity of 38.9 amu-MeV was determined for the following nuclear microprobe configuration: the distance from object aperture to collimating slits of 5890 mm, the working distance of 165 mm and the lens bore diameter of 11 mm. The overall distance from the object to the image plane is 7138 mm. The CHIMP beamline has been tested with the 3 MeV H+ and 6 MeV He2+ ion beams. The settings of the object and collimating apertures have been optimized using the WinTRAX simulation code for calculation of the optimum acceptance settings in order to obtain the highest possible ion current for beam spot sizes of 1 μm and 5 μm. For optimized aperture settings of the CHIMP the beam brightness was measured to be ∼0.9 pA μm-2 mrad-2 for 3 MeV H+ ions, while the brightness of ∼0.4 pA μm-2 mrad-2 was measured for 6 MeV He2+ ions. The smallest beam sizes were achieved using a microbeam with reduced particle rate of 1000 Hz passing through the object slit apertures several micrometers wide. Under these conditions a spatial resolution of ∼0.6 μm × 1.5 μm for 3 MeV H+ and ∼1.8 μm × 1.8 μm for 6 MeV He2+ microbeams in horizontal (and vertical) dimension has been achieved. The beam sizes were verified using STIM imaging on 2000 and 1000 mesh Cu electron microscope grids.

  10. Characterisation of candidate reference materials by PIXE analysis and nuclear microprobe PIXE imaging

    Jaksic, M.; Pastuovic, Z.; Bogdanovic, I.; Tadic, T.

    2002-01-01

    In order to test whether some candidate reference materials show homogeneity that can satisfy quality control of the PIXE technique, six bottles of each of the two Candidate RM's - Lichen (IAEA 338) and Algae (IAEA 413) were tested. Four different tests were performed. First, two pellets from each bottle were prepared and analysed using broad beam (φ = 5 mm) PIXE. Second and third was analysis of homogeneity using scanning focussed beam at the nuclear microprobe. Scans of 50x50 μm 2 and 240x260 μm 2 were performed. Finally, individual grains with composition differing from the rest of the sample, were analysed using PIXE and RBS. (author)

  11. Applications of petrography and electron microprobe analysis to the study of Indian stone sculpture

    Newman, R.

    1992-01-01

    Examples of research on ancient Indian stone artefacts utilizing petrographic examination coupled with qualitative and quantitative electron beam microprobe analysis of specific minerals are described. Types of artefacts discussed include Gandharan schist sculptures, Pala dynasty phyllite and schist objects from eastern India. Hoysala sculptures from Karnataka state (southern India), and sandstone objects from northern India. In spite of the rich history of stone sculpture in the Indian subcontinent, characterization studies to date have been limited in scope, typically involving unprovenanced artefacts. The examples described point to areas in which more extensive research could produce useful information for the provenancing of artefacts. (author)

  12. Ion beam analysis - development and application of nuclear reaction analysis methods, in particular at a nuclear microprobe

    Sjoeland, K.A.

    1996-11-01

    This thesis treats the development of Ion Beam Analysis methods, principally for the analysis of light elements at a nuclear microprobe. The light elements in this context are defined as having an atomic number less than approx. 13. The work reported is to a large extent based on multiparameter methods. Several signals are recorded simultaneously, and the data can be effectively analyzed to reveal structures that can not be observed through one-parameter collection. The different techniques are combined in a new set-up at the Lund Nuclear Microprobe. The various detectors for reaction products are arranged in such a way that they can be used for the simultaneous analysis of hydrogen, lithium, boron and fluorine together with traditional PIXE analysis and Scanning Transmission Ion Microscopy as well as photon-tagged Nuclear Reaction Analysis. 48 refs

  13. Physical aspects of quantitative particles analysis by X-ray fluorescence and electron microprobe techniques

    Markowicz, A.

    1986-01-01

    The aim of this work is to present both physical fundamentals and recent advances in quantitative particles analysis by X-ray fluorescence (XRF) and electron microprobe (EPXMA) techniques. A method of correction for the particle-size effect in XRF analysis is described and theoretically evaluated. New atomic number- and absorption correction procedures in EPXMA of individual particles are proposed. The applicability of these two correction methods is evaluated for a wide range of elemental composition, X-ray energy and sample thickness. Also, a theoretical model for composition and thickness dependence of Bremsstrahlung background generated in multielement bulk specimens as well as thin films and particles are presented and experimantally evaluated. Finally, the limitations and further possible improvements in quantitative particles analysis by XFR and EPXMA are discussed. 109 refs. (author)

  14. The Melbourne proton microprobe

    Legge, G.J.F.; McKenzie, C.D.; Mazzolini, A.P.

    1979-01-01

    A scanning proton microprobe is described which operates in ultra-high vacuum with a resolution of ten microns. The operating principles and main features of the design are discussed and the ability of such an instrument to detect trace elements down to a few ppm by mass is illustrated

  15. Comparison of laser microprobe mass spectrometry (LMMS) and micro particle induced x-ray emission (micro-PIXE) for the analysis of senile plaques in Alzheimer`s disease. A preliminary study

    Lovell, M A; Robertson, J D; Ehmann, W D [Kentucky Univ., Lexington, KY (United States). Dept. of Chemistry; Markesbery, W R [Kentucky Univ., Lexington, KY (United States); Teesdale, W J; Campbell, J L [Guelph Univ., ON (Canada). Dept. of Physics

    1995-08-01

    Results of micro-PIXE analysis of senile plaques (SP) in Alzheimer`s disease (AD) brain have been utilized to independently confirm levels of iron (Fe) as measured by LMMS in adjacent brain sections. LMMS concentrations were calculated based on the preparation and analysis of an iron calibration curve prepared in our laboratory. The LMMS standards consist of iron cis-dicylclohexano-18-crown-6 ether coordination complexes dissolved in Spurr`s low viscosity embedding medium. To our knowledge, this is the first report of the use of micro-PIXE, with its spatial resolution and detection limits comparable to that of LMMS, in the validation of LMMS results. The agreement observed between results obtained for Fe by micro-PIXE and LMMS indicates that the use of our LMMS standards, at least in the case of Fe, yields accurate results. (author). 6 refs., 1 fig., 1 tab.

  16. Proton microprobe analysis of zinc in skeletal tissues. [Proton induced x-ray emission analysis

    Doty, S B; Jones, K W; Kraner, H W; Shroy, R E; Hanson, A L

    1980-06-01

    A proton microprobe with windowless exit port was used to study zinc distributions in various types of skeletal tissues. The use of an external beam facilitated positioning of the targets for examination of particular points of interest. The proton microprobe is uniquely suited to this work since it combines high sensitivity for zinc determinations in thick samples with good spatial resolution. Measurements on rat and rabbit Achilles tendon showed a significant increase in zinc concentrations as the beam moved from the unmineralized collagen into the mineralized attachment site. Cartilage gave a similar result, with calcified cartilage having a greater zinc level than the articular surface on unmineralized epiphyseal cartilage.

  17. The non-destructive analysis of fluid inclusions in minerals using the proton microprobe

    Ryan, C.G.; Van Achterbergy, E. [Commonwealth Scientific and Industrial Research Organisation (CSIRO), North Ryde, NSW (Australia). Div. of Exploration Geoscience; Heinrich, C.A. [ETH Zentrum, Zurich, (Switzerland). Department Erdwissenschaften; Mernagh, T.P. [Max-Planck-Institut fuer Chemie (Otto-Hahn-Institut), Mainz (Germany); Zaw, K. [Tasmania Univ., Sandy Bay, TAS (Australia)

    1996-12-31

    The study of ore forming fluids trapped as fluid inclusions in minerals is the key to understanding fluid flow paths at the time of ore formation and to predicting the location of ore bodies within large-scale magmatic hydrothermal systems. The large penetration depths and the predictable nature of MeV proton trajectories and X-ray absorption enables reliable modelling of PIXE yields and the development of standardless quantitative analytical methods. This permits quantitative microanalysis of minerals at ppm levels, and more recently has enabled the development of methods for quantitative trace-element imaging and the quantitative, non-destructive analysis of individual fluid inclusions. This paper reports on recent developments in Proton Microprobe techniques with special emphasis on ore systems and fluid inclusion analysis. 6 refs., 2 figs.

  18. The non-destructive analysis of fluid inclusions in minerals using the proton microprobe

    Ryan, C G; Van Achterbergy, E [Commonwealth Scientific and Industrial Research Organisation (CSIRO), North Ryde, NSW (Australia). Div. of Exploration Geoscience; Heinrich, C A [ETH Zentrum, Zurich, (Switzerland). Department Erdwissenschaften; Mernagh, T P [Max-Planck-Institut fuer Chemie (Otto-Hahn-Institut), Mainz (Germany); Zaw, K [Tasmania Univ., Sandy Bay, TAS (Australia)

    1997-12-31

    The study of ore forming fluids trapped as fluid inclusions in minerals is the key to understanding fluid flow paths at the time of ore formation and to predicting the location of ore bodies within large-scale magmatic hydrothermal systems. The large penetration depths and the predictable nature of MeV proton trajectories and X-ray absorption enables reliable modelling of PIXE yields and the development of standardless quantitative analytical methods. This permits quantitative microanalysis of minerals at ppm levels, and more recently has enabled the development of methods for quantitative trace-element imaging and the quantitative, non-destructive analysis of individual fluid inclusions. This paper reports on recent developments in Proton Microprobe techniques with special emphasis on ore systems and fluid inclusion analysis. 6 refs., 2 figs.

  19. Ion channelling analysis of pre-amorphised silicon diodes using a nuclear microprobe

    Thornton, J.; Paus, K.C.

    1988-01-01

    Aligned and random ion channelling analysis was performed on p + n diode structures in silicon, with the Surrey nuclear microprobe. Three different types of diode were investigated, each pre-amorphised by a different ion (Si + , Ge + or Sn + ) before the p + region was formed by BF 2 + implantation. The ion channelling measurements are presented and compared with previously published electrical measurements on these diodes. Relatively large residual disorder and junction leakage currents were found for the Si + pre-amorphised diodes; however, all the diodes were leaky. The results are consistent with dislocation loops within the depletion regions of the diodes causing both the residual disorder and the large leakage currents. Cross-sectional transmission electron microscopy studies support this model. (author)

  20. Elemental analysis of single phytoplankton cells using the Lund nuclear microprobe

    Pallon, Jan; Elfman, Mikael; Kristiansson, Per; Malmqvist, Klas; Graneli, Edna; Sellborn, Anders; Karlsson, Chatarina

    1999-01-01

    The occurrence of annual marine phytoplankton blooms is becoming a global problem. In Europe, the NUTOX project supported by the EC investigates if unbalanced nutrient compositions in the water promote the dominance of harmful phytoplankton species. One of the tasks is the determination of the elemental composition of single phytoplankton cells. This is carried out using the Lund Nuclear Microprobe with a special focus on C, N, P and K. The overall aim is to understand the mechanism leading to toxin production, model it and eventually propose a counteracting method. The preparative method, used to isolate single living cells while reducing their salt environment, is an important part of the analytical procedure. A comparison of light element detection using backscattering from protons and nuclear reaction analysis using deuterons is made

  1. Experimental investigations into sample preparation of Alzheimer tissue specimens for nuclear microprobe analysis

    Pinheiro, T [CEC-JRC, Central Bureau for Nuclear Measurements, Geel (Belgium); Tapper, U A.S. [Dept. of Nuclear Physics, Lund Inst. of Science and Tech. (Sweden); Sturesson, K; Brun, A [Div. of Neuropathology, Dept. of Pathology, Lund University Hospital (Sweden)

    1991-03-01

    Nuclear microprobe analysis was applied to the study of elemental distribution in brains sections of patients with a diagnosis of Alzheimer's disease. Stained and nonstained cryosections were studied. The work carried out shows that serious elemental losses follow the sample staining procedure. Major losses occurred in a simple rinse of the tissue section, probably reducing most of the in-vivo gradients, which show that generally very little information can be gained from stained sections. However, in many cases stained sections are compulsory because of the requirement to recognize the area which is to be studied. All the elemental maps obtained for the neurofibrillary deposits indicate a localized concentration for Si and probably also Al, associated with the senile plaque core. Neither of these elements were found in the staining solutions used. The validity of the results is discussed as well as the possible link of Al and/or Si in the development of Alzheimer's desease. (orig.).

  2. Microprobe and SEM Analysis of a Meteorite from the Campo del Cielo Fall

    Cabanillas, E. D.; Palacios, T. A.

    2003-01-01

    Full Text: Meteorites are unique pieces in nature having not only the enigmatic connotations of the unknown but also are the easier obtained samples of the exterior universe. Furthermore they are the unique alloys that suffered modifications done during enormous periods of time in space and in land The Campo del Cielo fall, occurred more than 5000 years ago, gave hundredths of pieces some of them well studied. We have studied one of the minor pieces from the fall and with microprobe and scanning electronic microscopy analysis we determined the composition of Schreibersite and Rhabdite phosphides of iron and nickel. This study was performed to establish relationships between the duration of alloys and the design of disposal of high level and long lived radioactive waste

  3. Nuclear microprobe analysis of muscle biopsies: Applications in pathology and clinic

    Moretto, Ph.; Coquet, M.; Gherardi, R.K.; Stoedzel, P.

    2000-01-01

    The nuclear microprobe analysis of muscle biopsy sections has been recently applied to investigate different muscle disorders. This technique, employed as a complementary examination in the frame of pathological studies, permitted to confirm the diagnosis for a first pathology and to elucidate the cause of a second. In skeletal muscles of a young patient suffering from a slow progressive myopathy, calcium accumulations have been demonstrated in histologically abnormal fibers. These findings have been compared to histopathological characteristics previously described. On the other hand, we have evaluated muscle sections from two patients who presented symptoms of an inflammatory myopathy, a rare pathology that recently emerged in France. The chemical analyses permitted us to highlight local aluminium infiltration in muscles. The hypothesis of an unusual reaction to intramuscular aluminium accumulation has been advanced. These studies demonstrate the capability for ion beam microanalytical techniques to address acute problems in pathology

  4. Nuclear microprobe analysis of serpentine from the mid-Atlantic ridge

    Orberger, Beate; Metrich, Nicole; Mosbah, Michelle; Mevel, Catherine; Fouquet, Yves

    1999-01-01

    At mid-ocean ridges, ultramafic rocks are serpentinized by interaction with seawater-derived fluids. Elements, dissolved in large quantities in seawater, e.g., Na, K, Cl, Br, Ca and Sr, can be, in small amounts, incorporated as traces into the crystal structure of the various serpentine minerals (Mg 3 Si 2 O 5 (OH) 4 ). These trace elements can be used to track the composition of the reacting fluids and to constrain physico-chemical conditions. This paper represents the first application of particle-induced X- and γ-ray emission (PIXE/PIGE) analysis to serpentine using the nuclear microprobe at the Laboratoire Pierre Suee (CEA-CNRS). Three types of serpentine, belonging to two different serpentinization generations, have been analysed in samples collected from the Mid-Atlantic Ridge (14 deg. 45'N/45 deg. W) that exposes serpentinized peridotites on which the Logachev black smoker is placed. The trace elements Cl, F, S, Cu, Zn, Ca, K, Ni, Cr and Mn were detected from several tens to several thousands of ppm. Bromine, As and Sr are close to the detection limit of about 5 ppm. The trace element concentrations and interelement relationships in serpentines vary (a) with the serpentine type and (b) with the geographic location to the black smoker. Chlorine and in part S originated from seawater, whereas Cu, Zn, Ca, K, Ni, Cr and Fe and the major amount of S were mobilized from the unaltered host rock and partitioned between the serpentine and the aqueous solution

  5. Metallographic study of ferrite → sigma transformation using ferromagnetic colloid, microprobe analysis, and color etching

    Gray, R.J.; Crouse, R.S.; Sikka, V.K.; King, R.T.

    1976-01-01

    The mechanical properties of ferrite-containing austenitic stainless steel base metal and weldments are usually adversely affected by prolonged exposure to temperatures in the 482-900 0 C (900-1652 0 F) range. One cause of the property alteration is related to the transformation of relatively ductile delta-ferrite to less ductile sigma-phase. Attempts to identify sigma and delta ferrite phases by color staining techniques alone are well documented; however, the results are often questionable due to the difficulty in maintaining consistent color identifications. This investigation is concerned with the microstructural responses of the ferromagnetic delta-ferrite phase and the paramagnetic sigma-phase to a ferromagnetic iron colloid in a magnetic field. Such positive or negative responses of the two phases to the colloid offer a more definitive identification. With this technique, the identification of small amounts of these phases in the microstructure is limited only by the highest magnification and resolution of the optical microscope. The procedure is substantiated in this metallographic study with microprobe analysis and color metallography. Several examples of the correlative use of these three techniques in identifying varying amounts of delta-ferrite yields sigma transformation are presented

  6. Evaluation of the odd-even effect in limits of detection for electron microprobe analysis of natural minerals

    Verma, Surendra P., E-mail: spv@cie.unam.mx [Departamento de Sistemas Energeticos, Centro de Investigacion en Energia, Universidad Nacional Autonoma de Mexico, Priv. Xochicalco s/no., Col Centro, A.P. 34, Temixco, Mor. 62580 (Mexico); Pandarinath, Kailasa [Departamento de Sistemas Energeticos, Centro de Investigacion en Energia, Universidad Nacional Autonoma de Mexico, Priv. Xochicalco s/no., Col Centro, A.P. 34, Temixco, Mor. 62580 (Mexico); Velasco-Tapia, Fernando [Facultad de Ciencias de la Tierra, Universidad Autonoma de Nuevo Leon, Carretera Linares-Cerro Prieto km. 8, Linares, N.L. 67700 (Mexico); Rodriguez-Rios, Rodolfo [Facultad de Ingenieria e Instituto de Geologia, Universidad Autonoma de San Luis Potosi, Av. Dr. Manuel Nava No. 8, Zona Universitaria, San Luis Potosi, S.L.P. 78240 (Mexico)

    2009-04-13

    Limit of detection (LOD), being a fundamental quality parameter for analytical techniques, has been recently investigated and a systematic behavior has been observed for most odd-even element pairs for many techniques. However, to the best of our knowledge very few LOD data are available in published literature for electron microprobe analysis; these consist of three papers, two being on rare-earth elements and the third covering a large number of elements of atomic number between 21 and 92. These data confirm the systematic behavior of LODs for many odd-even pairs. To initiate to full this gap, we determined LODs for several major rock-forming chemical elements from Na to Fe with atomic numbers between 11 and 26, during the microprobe analysis of common minerals (olivine, plagioclase, pyroxene, amphibole, quartz, and opaques) in volcanic rocks. The odd-even effect of nuclear stability seems to be present in LOD data for most odd-even pairs investigated. Nevertheless, the experimental strategy concerning the reference materials, calibration procedure, and blank measurements, should be substantially modified to better evaluate the systematic behavior of LOD values in microprobe analysis.

  7. Evaluation of the odd-even effect in limits of detection for electron microprobe analysis of natural minerals

    Verma, Surendra P.; Pandarinath, Kailasa; Velasco-Tapia, Fernando; Rodriguez-Rios, Rodolfo

    2009-01-01

    Limit of detection (LOD), being a fundamental quality parameter for analytical techniques, has been recently investigated and a systematic behavior has been observed for most odd-even element pairs for many techniques. However, to the best of our knowledge very few LOD data are available in published literature for electron microprobe analysis; these consist of three papers, two being on rare-earth elements and the third covering a large number of elements of atomic number between 21 and 92. These data confirm the systematic behavior of LODs for many odd-even pairs. To initiate to full this gap, we determined LODs for several major rock-forming chemical elements from Na to Fe with atomic numbers between 11 and 26, during the microprobe analysis of common minerals (olivine, plagioclase, pyroxene, amphibole, quartz, and opaques) in volcanic rocks. The odd-even effect of nuclear stability seems to be present in LOD data for most odd-even pairs investigated. Nevertheless, the experimental strategy concerning the reference materials, calibration procedure, and blank measurements, should be substantially modified to better evaluate the systematic behavior of LOD values in microprobe analysis.

  8. Application of PIXE analysis to environmental samples stable element distribution in sea algae by scanning microprobe analysis

    Ishikawa, M.; Kitao, K.; Imaseki, H.; Ishii, T.; Uchida, S.

    1984-01-01

    The resolution of a 33+-3 μm microprobe focussed with quadrupole doublet installed at the 3 MV Van de Graaff of the National Institute of Radiological Sciences, Japan, was used for the present analysis. Brown algae, Hizikia fusiforme was the sample target bombarded with a 2 MeV proton beam collimated mechanically into a rectangular image of 100 μm x 700 μm. Scanning across the sample target prepared into a longitudinal section from the caulis of the algae provided the following observations. More than 12 elements such as Al, Si, P, Cl, Ca, Mn, Fe, Cu, Zn, As, Br and Sr were determined simultaneously, together with their distributional information across the diameter. In the medullary layer, Mn and Zn were specific in their accumulation, while the deposition of Fe, Cu, As and Br were observed to be high in the epithelial layer, especially Fe and Cu which were found on the surface, where they contacted ambient sea water, but no significant change in pattern was indicated for such elements as Al, P and Cl. The PIXE microprobe analysis was, therefore, effective in its detectability for elements below a few ppm level, resultantly providing further possibilities for collecting information from bio-medical and environmental samples on trace characterization of elements. (author)

  9. Nuclear microprobe analysis and source apportionment of individual atmospheric aerosol particles

    Artaxo, P.; Rabello, M.L.C.; Watt, F.; Grime, G.; Swietlicki, E.

    1993-01-01

    In atmospheric aerosol reserach, one key issue is to determine the sources of the airborne particles. Bulk PIXE analysis coupled with receptor modeling provides a useful, but limited view of the aerosol sources influencing one particular site or sample. The scanning nuclear microprobe (SNM) technique is a microanalytical technique that gives unique information on individual aerosol particles. In the SNM analyses a 1.0 μm size 2.4 MeV proton beam from the Oxford SNM was used. The trace elements with Z>11 were measured by the particle induced X-ray emission (PIXE) method with detection limits in the 1-10 ppm range. Carbon, nitrogen and oxygen are measured simultaneously using Rutherford backscattering spectrometry (RBS). Atmospheric aerosol particles were collected at the Brazilian Antarctic Station and at biomass burning sites in the Amazon basin tropical rain forest in Brazil. In the Antarctic samples, the sea-salt aerosol particles were clearly predominating, with NaCl and CaSO 4 as major compounds with several trace elements as Al, Si, P, K, Mn, Fe, Ni, Cu, Zn, Br, Sr, and Pb. Factor analysis of the elemental data showed the presence of four components: 1) Soil dust particles; 2) NaCl particles; 3) CaSO 4 with Sr; and 4) Br and Mg. Strontium, observed at 20-100 ppm levels, was always present in the CaSO 4 particles. The hierarchical cluster procedure gave results similar to the ones obtained through factor analysis. For the tropical rain forest biomass burning aerosol emissions, biogenic particles with a high organic content dominate the particle population, while K, P, Ca, Mg, Zn, and Si are the dominant elements. Zinc at 10-200 ppm is present in biogenic particles rich in P and K. The quantitative aspects and excellent detection limits make SNM analysis of individual aerosol particles a very powerful analytical tool. (orig.)

  10. Ion microprobes

    Coles, J.N.; Long, J.V.P.

    1977-01-01

    An ion microprobe is described that has an ion extraction arrangement comprising two separate paths for ions and electrons diverging from a common point. A cone shaped or pyramidal guard electrode surrounds each path the apex angles being equal and coinciding with the said point. The guard electrodes are positioned to lie tangentially to each other and to a planar surface including the said point. An aperture is provided for the two paths at the apexes of both guard electrodes, and electrical connections between the guard electrodes enable the same potential to be applied to both guard electrodes. Means are provided for generating oppositely polarised electric fields within the guard electrodes, together with means for causing a focused ion beam to strike the common point without suffering astigmatism. The means for causing a focused ion beam to strike the said point includes an ion gun for directing an ion beam along one of the paths and means to provide an axial accelerating field there along. Optical viewing means are also provided. Existing designs enable only ions or electrons, but not both, to be extracted at any one time. (U.K.)

  11. Nuclear microprobe analysis of serpentine from the mid-Atlantic ridge

    Orberger, Beate E-mail: orberger@geol.u-psud.fr; Metrich, Nicole; Mosbah, Michelle E-mail: mosbah@drecam.cea.fr; Mevel, Catherine; Fouquet, Yves

    1999-09-02

    At mid-ocean ridges, ultramafic rocks are serpentinized by interaction with seawater-derived fluids. Elements, dissolved in large quantities in seawater, e.g., Na, K, Cl, Br, Ca and Sr, can be, in small amounts, incorporated as traces into the crystal structure of the various serpentine minerals (Mg{sub 3}Si{sub 2}O{sub 5}(OH){sub 4}). These trace elements can be used to track the composition of the reacting fluids and to constrain physico-chemical conditions. This paper represents the first application of particle-induced X- and {gamma}-ray emission (PIXE/PIGE) analysis to serpentine using the nuclear microprobe at the Laboratoire Pierre Suee (CEA-CNRS). Three types of serpentine, belonging to two different serpentinization generations, have been analysed in samples collected from the Mid-Atlantic Ridge (14 deg. 45'N/45 deg. W) that exposes serpentinized peridotites on which the Logachev black smoker is placed. The trace elements Cl, F, S, Cu, Zn, Ca, K, Ni, Cr and Mn were detected from several tens to several thousands of ppm. Bromine, As and Sr are close to the detection limit of about 5 ppm. The trace element concentrations and interelement relationships in serpentines vary (a) with the serpentine type and (b) with the geographic location to the black smoker. Chlorine and in part S originated from seawater, whereas Cu, Zn, Ca, K, Ni, Cr and Fe and the major amount of S were mobilized from the unaltered host rock and partitioned between the serpentine and the aqueous solution.

  12. Rapid rock analysis and microprobe scanning of dermatological material using proton-induced x-ray and γ-ray emission

    Carlsson, L.E.

    1983-01-01

    The dissertation report comprises 6 articles that have or will appear in open literature. The use of PIXE and PIGE analysis techniques on geological materials, and also on drill cores, is discussed. The accuracy of the methods have been tested on standards. The effect of sample thickness has been studied. A proton microprobe has been compared with an electron microprobe on human skin sections. Both probes give highly reproducible results, but a small systematic deviation between the probes is found. (author)

  13. U-Pb geochronology of zircons form lunar Breccia 73217 using a sensitive high mass-resolution ion microprobe

    Compston, W.; Williams, I.S.

    1984-01-01

    U-Pb age determinations on four lunar zircons from existing thin-sections of one highland breccia, 73217, using the recently constructed ion microprobe SHRIMP, are reported. The analytical reproducibility of SHRIMP is demonstrated, and procedures for measuring Pb/U, Th/U, and corecting for initial Pb are explained. Electron microprobe analyses for the zircons are also reported. The results show that the four zircons survived the lunar cataclysm without any identifiable effects on their U-Pb systematics. All four indicate a single age of 4356 +23 or -14 m.y. The zircons have experienced small variable amounts of Pb loss since crystallization, from almost zero up to about 10 percent. If this occurred during one later event, then age of the latter is between 1100 and 2300 m.y. 18 references

  14. Trace elemental analysis of bituminous coals using the Heidelberg proton microprobe

    Chen, J R; Kneis, H; Martin, B; Nobiling, R; Traxel, K [Max-Planck-Institut fuer Kernphysik, Heidelberg (Germany, F.R.); Heidelberg Univ. (Germany, F.R.). Physikalisches Inst.); Chao, E C.T.; Minkin, J A [Geological Survey, Reston, VA (USA)

    1981-03-01

    Trace elements in coal can occur as components of either the organic constituents (macerals) or the inorganic constituents (minerals). Studies of the concentrations and distribution of the trace elements are vital to understanding the geochemical milieu in which the coal was formed and in evaluating the attempts to recover rare but technologically valuable metals. In addition, information on the trace element concentrations is important in predicting the environmental impact of burning particular coals, as many countries move toward greater utilization of coal reserves for energy production. Traditionally, the optical and the electron microscopes and more recently the electron microprobe have been used in studying the components of coal. The proton-induced X-ray emission (PIXE) microprobe offers a new complementary approach with an order of magnitude or more better minimum detection limit. We present the first measurements with a PIXE microprobe of the trace element concentrations of bituminous coal samples. Elemental analyses of the coal macerals-vitrinite, exinite, and inertinite - are discussed for three coal samples from the Eastern U.S.A., three samples from the Western U.S.A., and one sample from the Peoples Republic of China.

  15. Characterization of flux-grown Trace-element-doped titanite using the high-mass-resolution ion microprobe (SHRIMP-RG)

    Mazdab, F.K.

    2009-01-01

    Crystals of titanite can be readily grown under ambient pressure from a mixture of CaO, TiO2 and SiO2 in the presence of molten sodium tetraborate. The crystals produced are euhedral and prismatic, lustrous and transparent, and up to 5 mm in length. Titanite obtained by this method contains approximately 4300 ppm Na and 220 ppm B contributed from the flux. In addition to dopant-free material, titanite containing trace alkali and alkaline earth metals (K, Sr, Ba), transition metals (Sc, Cr, Ni, Y, Zr, Nb, Hf and Ta), rare-earth elements (REE), actinides (Th, U) and p-block elements (F, S, Cl, Ge, Sn and Pb) have been prepared using the same procedure. Back-scattered electron (BSE) imaging accompanied by ion-microprobe (SHRIMP-RG) analysis confirms significant incorporation of selected trace-elements at structural sites. Regardless of some zonation, the large size of the crystals and broad regions of chemical homogeneity make these crystals useful as experimental starting material, and as matrix-matched trace-element standards for a variety of microbeam analytical techniques where amorphous titanite glass, heterogeneous natural titanite or a non-titanite standard may be less than satisfactory. Trace-element-doped synthetic crystals can also provide a convenient proxy for a better understanding of trace-element incorporation in natural titanite. Comparisons with igneous, authigenic and high-temperature metasomatic titanite are examined. The use of high-mass-resolution SIMS also demonstrates the analytical challenges inherent to any in situ mass-spectrometry-based analysis of titanite, owing to the production of difficult-to-resolve molecular interferences. These interferences are dominated by Ca-Ca, Ca-Ti and Ti-Ti dimers that are significant in the mass range of 80-100, affecting all isotopes of Sr and Zr, as well as 89Y and 93Nb. Methods do exist for the evaluation of interferences by these dimers and of polyatomic interferences on the LREE.

  16. Use of a synchrotron radiation x-ray microprobe for elemental analysis at the National Synchrotron Light Source

    Gordon, B.M.

    1980-01-01

    The National Synchrotron Light Source (NSLS) is a facility consisting of a 700 MeV and a 2.5 GeV electron storage ring and dedicated to providing synchrotron radiation in the energy range from the vacuum ultraviolet to high energy x rays. Some of the properties of synchrotron radiation that contribute to its usefulness for x-ray fluorescence are: a continuous, tunable energy spectrum, strong collimation in the horizontal plane, high polarization in the storage ring plane, and relatively low energy deposition. The highest priority is for the development of an x-ray microprobe beam line capable of trace analysis in the parts per million range with spatial resolution as low as one micrometer. An eventual capability for bulk sample analysis is also planned with sensitivities in the more favorable cases beings low as 50 parts per billion in dry biological tissue. The microprobe technique has application to a variety of fields including the geological, medical, materials and environmental sciences. Examples of investigations include multielemental trace analysis across grain boundaries for the study of diffusion and cooling processes in geological and materials sciences samples; in leukocytes and other types of individual cells for studying the relationship between trace element concentrations and disease or nutrition; and in individual particles in air pollution samples

  17. Microprobe analysis of PuO2--UO2 nuclear fuel

    Clark, W.I.; Rasmussen, D.E.; Carlson, R.L.; Highley, D.M.

    1977-01-01

    For the preirradiation characterization of FFTF UO 2 --PuO 2 fuel, a program was developed to determine the preirradiation porosity, grain structure, and microcomposition of the fuel. Two computer programs, MITRAN and MERIT, were developed to evaluate the homogeneity of the fuel. These programs use elemental composition data generated by the electron microprobe. MITRAN determines information on the size and frequency of individual regions, whereas MERIT provides an index of the thermal performance of the fuel and calculated statistical data for comparison to other fuel batches

  18. Automated electron microprobe

    Thompson, K.A.; Walker, L.R.

    1986-01-01

    The Plant Laboratory at the Oak Ridge Y-12 Plant has recently obtained a Cameca MBX electron microprobe with a Tracor Northern TN5500 automation system. This allows full stage and spectrometer automation and digital beam control. The capabilities of the system include qualitative and quantitative elemental microanalysis for all elements above and including boron in atomic number, high- and low-magnification imaging and processing, elemental mapping and enhancement, and particle size, shape, and composition analyses. Very low magnification, quantitative elemental mapping using stage control (which is of particular interest) has been accomplished along with automated size, shape, and composition analysis over a large relative area

  19. Optically continuous silcrete quartz cements of the St. Peter Sandstone: High precision oxygen isotope analysis by ion microprobe

    Kelly, Jacque L.; Fu, Bin; Kita, Noriko T.; Valley, John W.

    2007-08-01

    A detailed oxygen isotope study of detrital quartz and authigenic quartz overgrowths from shallowly buried (ratio by laser fluorination, resulting in an average δ 18O of 10.0 ± 0.2‰ (1SD, n = 109). Twelve thin sections were analyzed by CAMECA-1280 ion microprobe (6-10 μm spot size, analytical precision better than ±0.2‰, 1SD). Detrital quartz grains have an average δ 18O of 10.0 ± 1.4‰ (1SD, n = 91) identical to the data obtained by laser fluorination. The ion microprobe data reveal true variability that is otherwise lost by homogenization of powdered samples necessary for laser fluorination. Laser fluorination uses samples that are one million times larger than the ion microprobe. Whole rock (WR) samples from the 53 rocks were analyzed by laser fluorination, giving δ 18O between 9.8‰ and 16.7‰ ( n = 110). Quartz overgrowths in thin sections from 10 rocks were analyzed by ion microprobe and average δ 18O = 29.3 ± 1.0‰ (1SD, n = 161). Given the similarity, on average, of δ 18O for all detrital quartz grains and for all quartz overgrowths, samples with higher δ 18O(WR) values can be shown to have more cement. The quartz cement in the 53 rocks, calculated by mass balance, varies from outlier at 33 vol.% cement. Eolian samples have an average of 11% cement compared to marine samples, which average 4% cement. Two models for quartz cementation have been investigated: high temperature (50-110 °C) formation from ore-forming brines related to Mississippi Valley Type (MVT) mineralization and formation as silcretes at low temperature (10-30 °C). The homogeneity of δ 18O for quartz overgrowths determined by ion microprobe rules out a systematic regional variation of temperature as predicted for MVT brines and there are no other known heating events in these sediments that were never buried to depths >1 km. The data in this study suggest that quartz overgrowths formed as silcretes in the St. Peter Sandstone from meteoric water with δ 18O values of -10

  20. Quantitative analysis of chemical elements in single cells using nuclear microprobe and nano-probe

    Deves, Guillaume

    2010-01-01

    The study of the role of trace elements at cellular level requires the use of state-of-the-art analytical tools that could achieve enough sensitivity and spatial resolution. We developed a new methodology for the accurate quantification of chemical element distribution in single cells based on a combination of ion beam analysis techniques STIM, PIXE and RBS. The quantification procedure relies on the development of a STIM data analysis software (Paparamborde). Validity of this methodology and limits are discussed here. The method allows the quantification of trace elements (μg/g) with a 19.8 % uncertainty in cellular compartments with mass below 0.1 ng. The main limit of the method lies in the poor number of samples that can be analyzed, due to long irradiation times required and limited access to ion beam analysis facilities. This is the reason why we developed a database for cellular chemical composition capitalization (BDC4). BDC4 has been designed in order to use cellular chemical composition as a tracer for biological activities and is expected to provide in the future reference chemical compositions for any cellular type or compartment. Application of the STIM-PIXE-RBS methodology to the study of nuclear toxicology of cobalt compounds is presented here showing that STIM analysis is absolutely needed when organic mass loss appears during PIXE-RBS irradiation. (author)

  1. Planktonic foraminiferal oxygen isotope analysis by ion microprobe technique suggests warm tropical sea surface temperatures during the Early Paleogene

    Kozdon, Reinhard; Kelly, D. Clay; Kita, Noriko T.; Fournelle, John H.; Valley, John W.

    2011-09-01

    Cool tropical sea surface temperatures (SSTs) are reported for warm Paleogene greenhouse climates based on the δ18O of planktonic foraminiferal tests. These results are difficult to reconcile with models of greenhouse gas-forced climate. It has been suggested that this "cool tropics paradox" arises from postdepositional alteration of foraminiferal calcite, yielding erroneously high δ18O values. Recrystallization of foraminiferal tests is cryptic and difficult to quantify, and the compilation of robust δ18O records from moderately altered material remains challenging. Scanning electron microscopy of planktonic foraminiferal chamber-wall cross sections reveals that the basal area of muricae, pustular outgrowths on the chamber walls of species belonging to the genus Morozovella, contain no mural pores and may be less susceptible to postdepositional alteration. We analyzed the δ18O in muricae bases of morozovellids from the central Pacific (Ocean Drilling Program Site 865) by ion microprobe using 10 μm pits with an analytical reproducibility of ±0.34‰ (2 standard deviations). In situ measurements of δ18O in these domains yield consistently lower values than those published for conventional multispecimen analyses. Assuming that the original δ18O is largely preserved in the basal areas of muricae, this new δ18O record indicates Early Paleogene (˜49-56 Ma) tropical SSTs in the central Pacific were 4°-8°C higher than inferred from the previously published δ18O record and that SSTs reached at least ˜33°C during the Paleocene-Eocene thermal maximum. This study demonstrates the utility of ion microprobe analysis for generating more reliable paleoclimate records from moderately altered foraminiferal tests preserved in deep-sea sediments.

  2. Elemental analysis of some West Malaysian limestones using neutron activation, delayed neutron and electron microprobe analysis

    Amin, Y.M.; Kamaluddin, B.; Mahat, R.H.

    1990-01-01

    Limestone stratigraphy in Malaysia has been and is dependent almost entirely in palaeontology. However fossil localities are sporadic and as such a new fossil discovery mean the necessity for a complete re-appraisal of the stratigraphy. The almost complete dependence upon palaeontology results from the difficulties of stratigraphy correlation of isolated outcrops, from the cover of tropical vegetation and from the often complex folding and faulting which has been imposed on the geosyn-clinical rocks by the Indonesian-Thai-Malayan orogeny. So by studying the elemental composition of limestones accurately, we would be able to correlate outcrops and other stratigraphic samples independent of fossil finds. The use of delayed neutron analysis would also determine the concentration of uranium and thorium accurately. This study, in conjunction with thermoluminescence and fission track studies, would able us to date the age of the limestones

  3. Positron annihilation microprobe

    Canter, K F [Brandeis Univ., Waltham, MA (United States)

    1997-03-01

    Advances in positron annihilation microprobe development are reviewed. The present resolution achievable is 3 {mu}m. The ultimate resolution is expected to be 0.1 {mu}m which will enable the positron microprobe to be a valuable tool in the development of 0.1 {mu}m scale electronic devices in the future. (author)

  4. The Stanford-U.S. Geological Survey SHRIMP ion microprobe--a tool for micro-scale chemical and isotopic analysis

    Bacon, Charles R.; Grove, Marty; Vazquez, Jorge A.; Coble, Matthew A.

    2012-01-01

    Answers to many questions in Earth science require chemical analysis of minute volumes of minerals, volcanic glass, or biological materials. Secondary Ion Mass Spectrometry (SIMS) is an extremely sensitive analytical method in which a 5–30 micrometer diameter "primary" beam of charged particles (ions) is focused on a region of a solid specimen to sputter secondary ions from 1–5 nanograms of the sample under high vacuum. The elemental abundances and isotopic ratios of these secondary ions are determined with a mass spectrometer. These results can be used for geochronology to determine the age of a region within a crystal thousands to billions of years old or to precisely measure trace abundances of chemical elements at concentrations as low as parts per billion. A partnership of the U.S. Geological Survey and the Stanford University School of Earth Sciences operates a large SIMS instrument, the Sensitive High-Resolution Ion Microprobe with Reverse Geometry (SHRIMP–RG) on the Stanford campus.

  5. Applications of the ion microprobe to geochemistry and cosmochemistry

    Shimizu, N.; Hart, S.R.

    1982-01-01

    When a solid surface is subjected to a bombardment of energetic ions, material is ejected from the surface in a process known as sputtering. A part of the sputtered material is ionized and these secondary ions can be analyzed with a mass spectrometer according to a technique known as secondary ion mass spectrometry (SIMS). A description is presented of the present status of geochemical and cosmochemical applications of the ion microprobe. Attention is given to the sputtering event, molecular ion interferences, aspects of isotopic fractionation, secondary ion intensities in polycomponent materials, and questions of trace element analysis. Geochemical applications of the ion microprobe are based on certain advantages over other analytical techniques. These advantages are related to high sensitivity, low background, and the capability of in situ analysis of isotopic composition. The distribution of trace elements in minerals is considered, along with isotope anomalies, isotope zoning, diffusion studies, and depth profiling

  6. The laser microprobe mass analyser for determining partitioning of minor and trace elements among intimately associated macerals: an example from the Swallow Wood coal bed, Yorkshire, UK

    Lyons, P.C.; Morelli, J.J.; Hercules, D.M.; Lineman, D.; Thompson-Rizer, C. L.; Dulong, F.T.

    1990-01-01

    A study of the elemental composition of intimately associated coal macerals in the English Swallow Wood coal bed was conducted using a laser microprobe mass analyser, and indicated a similar trace and minor elemental chemistry in the vitrinite and cutinite and a different elemental signature in the fusinite. Three to six sites were analysed within each maceral during the study by laser micro mass spectrometry (LAMMS). Al, Ba, Ca, Cl, Cr, Dy, F, Fe, Ga, K, Li, Mg, Na, S, Si, Sr, Ti, V, and Y were detected by LAMMS in all three macerals but not necessarily at each site analysed. The signal intensities of major isotopic peaks were normalized to the signal intensity of the m z 85 peak (C7H) to determine the relative minor- and trace-element concentrations among the three dominant macerals. The vitrinite and the cutinite were depleted in Ba, Ca, Dy, Li, Mg, Sr, and Y relative to their concentrations observed in the fusinite. The cutinite was distinguished over vitrinite by less Ti, V, Cr and Ca, and K Ca $ ??1 (relative signal intensities). The fusinite, relative to the cutinite and vitrinite, was relatively depleted in Cr, Sc, Ti, and V. The fusinite, as compared with both the cutinite and vitrinite, was relatively enriched in Ba, Ca, Dy, Li, Mg, Sr, and Y, and also showed the most intense m z 64, 65, 66 signals (possibly S2+, HS2+, H2S2+, respectively). The LAMMS data indicate a common source for most elements and selective loss from the maceral precursors in the peat or entrapment of certain elements as mineral matter, most likely during the peat stage or during early diagenesis. The relatively high amounts of Ba, Ca, Dy, Li, Mg, Sr, and Y in the fusinite are consistent with micron and submicron mineral-matter inclusions such as carbonates and Ca-Al phosphates (probably crandallite group minerals). Mineralogical data on the whole coal, the LAMMS chemistry of the vitrinite and cutinite, and scanning electron microscopy/energy dispersive X-ray analysis (SEM/EDAX) of

  7. Nuclear scanning microprobe: state of the art, applications and progress trends

    Ponomarev, A.G.

    2011-01-01

    The physical principles of nuclear scanning microprobe are considered. The analysis of state of the art of the microprobe setup from point of view of its spatial resolution and sensitivity of microanalysis techniques is given. The regions of nuclear microprobe applications are reviewed. The ways of spatial resolution and data acquisition system improvement under consideration of microprobe setup progress trends are considered. (authors)

  8. Microscopic and microprobe analysis of fine roots in healthy and declining spruce (Picea abies (L. ) Karst. ) from different sites

    Stienen, H; Bauch, J; Barckhausen, R; Schaub, H

    1984-09-01

    In order to contribute to the identification of primary causes of the spruce decline - evident in many regions of the Federal Republic of Germany - fine roots of 30 trees from altogether 14 healthy and damage forest locations were investigated microscopically, anatomically, histometrically and by cellular microprobe analysis. In addition, fine roots of young plants grown in hydroponic cultures at different pH levels and Al input were studied. Fine roots of declining trees developed cortex cells with a reduced diameter and at the same time thicker cell walls; in addition accessory compounds were accumulated in this presumably protective tissue. Tannins were deposited in the parenchyma of the vascular cylinder of fine roots from declining trees, and many pit membranes of the primary xylem often did not differentiate fully. The X-ray energy-dispersive analysis of individual cells revealed, in particular, an insufficient uptake of Ca and Mg in the fine roots of declining trees. Compared with healthy trees, the concentration of aluminium increased in the cortex of the fine roots; this, in turn, had an antagonistic effect on the uptake of Ca and Mg. Moreover, the concentration of iron and sulphur increased in the fine roots of declining trees. This evidence of alterations and damages in the fine roots of damaged spruce indicates that, besides the direct detrimental impact on the needles through the atmosphere serious damage is inflicted also indirectly through the soil.

  9. PIXE and light element analysis (C,N) in glass inclusions trapped in meteorites with the nuclear microprobe

    Varela, M.E.; Mosbah, M.; Metrich, N.; Duraud, J.P.; Kurat, G.

    1999-01-01

    Proton-induced X-ray emission (PIXE) and light element analysis have been performed with the nuclear microprobe at the Laboratoire Pierre Suee (Saclay-France) in glass inclusions of the carbonaceous chondrites: Allende, Kaba and Renazzo, and in the achondrite meteorite: Chassigny. Carbon contents in olivine of chondrules are below the nuclear reactions analysis (NRA) detection limit, however, glasses from glass inclusions hosted by these grains, contain an appreciable and highly variable quantities of carbon (200-1600 ppm). This could indicate variable amounts of C trapped during glass inclusion formation. On the other hand, nitrogen is present in highly variable amounts in glasses of both, chondrites and achondrites minerals. Its abundance, correlated with depth from the section surface which suggests loss of N during analyses and therefore the possible existence of a very mobile (volatile?) species. A chondritic Rb/Sr and K/Rb ratio obtained by PIXE analyses in the glass-bearing inclusions of the Chassigny meteorite points towards a primitive source for the glass precursor of Chassigny inclusions

  10. Quantitative microanalysis with a nuclear microprobe

    Themner, Klas.

    1989-01-01

    The analytical techniques of paticle induced X-ray emission (PIXE) and Rutherford backscattering (RBS), together with the nuclear microprobe, form a very powerful tool for performing quantitative microanalysis of biological material. Calibration of the X-ray detection system in the microprobe set-up has been performed and the accuracy of the quantitative procedure using RBS for determination of the areal mass density was investigated. The accuracy of the analysis can be affected by alteration in the elemental concentrations during irradiation due to the radiation damage induced by the very intense beams of ionixing radiation. Loss of matrix elements from freeze-dried tissue sections and polymer films have been studied during proton and photon irradiation and the effect on the accuracy discussed. Scanning the beam over an area of the target, with e.g. 32x32 pixels, in order to produce en elemental map, yields a lot of information and, to be able to make an accurate quantitatification, a fast algorithm using descriptions of the different spectral contributions is of need. The production of continuum X-rays by 2.55 MeV protons has been studied and absolute cross-sections for the bremsstrahlung production from thin carbon and some polymer films determined. For the determination of the bremsstrahlung background knowledge of the amounts of the matrix elements is important and a fast program for the evaluation of spectra of proton back- and forward scattering from biological samples has been developed. Quantitative microanalysis with the nuclear microprobe has been performed on brain tissue from rats subjected to different pathological conditions. Increase in calcium levels and decrease in potssium levels for animals subjected to crebral ischaemia and for animals suffering from epileptic seizures were observed coincidentally with or, in some cases before, visible signs of cell necrosis. (author)

  11. Technique Development to Support Clean-up and/or Disposal of Actinide Contaminated Soils and Sediments: Coupling Fission Tract Analysis with Synchroton X-ray Microprobe Analysis

    Sue Clark

    2003-01-01

    The overall goal of this project was to develop quantitative FTA to provide images of the microscale spatial distributions of high fissile actinides sorbed to environmental particles such as sediments and colloids. We developed methods to provide absolute actinide surface concentrations on the particles, regardless of particle size. We are also working to provide particle size information by our approach. We also coupled our newly devised FTA methods with the quantitative determination of stable element distributions in the same particles using synchrotron x-ray microprobe analysis

  12. Distribution of elements in rat peripheral axons and nerve cell bodies determined by x-ray microprobe analysis

    LoPachin, R.M. Jr.; Lowery, J.; Eichberg, J.; Kirkpatrick, J.B.; Cartwright, J. Jr.; Saubermann, A.J.

    1988-09-01

    X-ray microprobe analysis was used to determine concentrations (millimoles of element per kilogram dry weight) of Na, P, Cl, K, and Ca in cellular compartments of frozen, unfixed sections of rat sciatic and tibial nerves and dorsal root ganglion (DRG). Five compartments were examined in peripheral nerve (axoplasm, mitochondria, myelin, extraaxonal space, and Schwann cell cytoplasm), and four were analyzed in DRG nerve cell bodies (cytoplasm, mitochondria, nucleus, and nucleolus). Each morphological compartment exhibited characteristic concentrations of elements. The extraaxonal space contained high concentrations of Na, Cl, and Ca, whereas intraaxonal compartments exhibited lower concentrations of these elements but relatively high K contents. Nerve axoplasm and axonal mitochondria had similar elemental profiles, and both compartments displayed proximodistal gradients of decreasing levels of K, Cl, and, to some extent, Na. Myelin had a selectively high P concentration with low levels of other elements. The elemental concentrations of Schwann cell cytoplasm and DRG were similar, but both were different from that of axoplasm, in that K and Cl were markedly lower whereas P was higher. DRG cell nuclei contained substantially higher K levels than cytoplasm. The subcellular distribution of elements was clearly shown by color-coded images generated by computer-directed digital x-ray imaging. The results of this study demonstrate characteristic elemental distributions for each anatomical compartment, which doubtless reflect nerve cell structure and function.

  13. Detection of delta-ferrite to sigma transformation using metallographic techniques involving ferromagnetic colloid, color etching, and microprobe analysis

    Gray, R.J.; Sikka, V.K.; King, R.T.

    1976-01-01

    The mechanical properties of ferrite-containing austenitic stainless steel base metal and weldments are usually adversely affected by prolonged exposure to temperatures in the 482 to 900 0 C (900 to 1652 0 F) range. One cause of the property alteration is related to the transformation of relatively ductile delta-ferrite to less ductile sigma-phase. Attempts to identify sigma and delta-ferrite phases by color staining techniques alone are well documented; however, the results are often questionable due to the difficulty in maintaining consistent color identifications. This investigation is concerned with the microstructural responses of the ferromagnetic delta-ferrite phase and the paramagnetic sigma-phase to a ferromagnetic iron colloid in a magnetic field. Such positive or negative responses of the two phases to the colloid offer a more definitive identification. With this technique, the identification of small amounts of these phases in the microstructure is limited only by the highest magnification and resolution of the optical microscope. The procedure is substantiated in this metallographic study with microprobe analysis and color metallography. Several examples of the correlative use of these three techniques in identifying varying amounts of delta-ferrite → sigma transformation are presented

  14. PROTON MICROPROBE ANALYSIS OF TRACE-ELEMENT VARIATIONS IN VITRINITES IN THE SAME AND DIFFERENT COAL BEDS.

    Minkin, J.A.; Chao, E.C.T.; Blank, Herma; Dulong, F.T.

    1987-01-01

    The PIXE (proton-induced X-ray emission) microprobe can be used for nondestructive, in-situ analyses of areas as small as those analyzed by the electron microprobe, and has a sensitivity of detection as much as two orders of magnitude better than the electron microprobe. Preliminary studies demonstrated that PIXE provides a capability for quantitative determination of elemental concentrations in individual coal maceral grains with a detection limit of 1-10 ppm for most elements analyzed. Encouraged by the earlier results, we carried out the analyses reported below to examine trace element variations laterally (over a km range) as well as vertically (cm to m) in the I and J coal beds in the Upper Cretaceous Ferron Sandstone Member of the Mancos Shale in central Utah, and to compare the data with the data from two samples of eastern coals of Pennsylvanian age.

  15. In situ titanium dioxide nanoparticles quantitative microscopy in cells and in C. elegans using nuclear microprobe analysis

    Le Trequesser, Quentin [Université de Bordeaux, CENBG, Chemin du solarium, 33175 Gradignan (France); CNRS, UMR 5797, CENBG, Chemin du solarium, 33175 Gradignan (France); CNRS, Université de Bordeaux, ICMCB, 87 avenue du Dr. A. Schweitzer, Pessac F-33608 (France); Saez, Gladys; Devès, Guillaume; Michelet, Claire; Barberet, Philippe [Université de Bordeaux, CENBG, Chemin du solarium, 33175 Gradignan (France); CNRS, UMR 5797, CENBG, Chemin du solarium, 33175 Gradignan (France); Delville, Marie-Hélène [CNRS, Université de Bordeaux, ICMCB, 87 avenue du Dr. A. Schweitzer, Pessac F-33608 (France); Seznec, Hervé, E-mail: herve.seznec@cenbg.in2p3.fr [Université de Bordeaux, CENBG, Chemin du solarium, 33175 Gradignan (France); CNRS, UMR 5797, CENBG, Chemin du solarium, 33175 Gradignan (France)

    2014-12-15

    Detecting and tracking nanomaterials in biological systems is challenging and essential to understand the possible interactions with the living. In this context, in situ analyses were conducted on human skin cells and a multicellular organism (Caenorhabditiselegans) exposed to titanium dioxide nanoparticles (TiO{sub 2} NPs) using nuclear microprobe. Coupled to conventional methods, nuclear microprobe was found to be suitable for accurate description of chemical structure of biological systems and also for detection of native TiO{sub 2} NPs. The method presented herein opens the field to NPs exposure effects analyses and more generally to toxicological analyses assisted by nuclear microprobe. This method will show applications in key research areas where in situ imaging of chemical elements is essential.

  16. Use of electron microprobe x-ray analysis for determination of low calcium concentrations across leaves deficient in calcium

    Barta, D. J.; Tibbitts, T. W.

    1991-01-01

    An electron microprobe with wavelength-dispersive x-ray spectrometry (WDS) was found to be useful for the determination of Ca concentrations in leaf tissue deficient in Ca. WDS effectively detected Ca concentrations as low as 0.2 mg/g dry wt in the presence of high levels of K and Mg (120 and 50 mg/g dry wt, respectively). Leaf specimens were prepared for analysis by quick-freezing in liquid nitrogen and freeze-drying at -20 degrees C to maintain elemental integrity within the tissue. Because dry material was analyzed, sample preparation was simple and samples could be stored for long periods before analysis. A large beam diameter of 50 gm was used to minimize tissue damage under the beam and analyze mineral concentrations within several cells at one time. Beam penetration was between 50 and 55 microns, approximately one-third of the thickness of the leaf. For analysis of concentrations in interveinal areas, analyses directed into the abaxial epidermis were found most useful. However, because of limited beam penetration, analyses of veinal areas would require use of cross sections [correction of crosssections]. Solid mineral standards were used for instrument standardization. To prevent measurement errors resulting from differences between the matrix of the mineral standards and the analyzed tissue, concentrations in leaves were corrected using gelatin standards prepared and analyzed under the same conditions. WDS was found to be useful for documenting that very low Ca levels occur in specific areas of lettuce leaves exhibiting the Ca deficiency injury termed tipburn.

  17. Trace element analysis in geochemistry using a nuclear microprobe. Ionoluminescence and particle induced X-ray emission

    Homman, P.

    1994-01-01

    In PIXE analysis of geological specimens based on X-ray detection with Si(Li) detectors, effects of detector tailing, pulse pileup, and gamma-ray production are pronounced. In this work the tailing effect has been addressed through characterization of the response function of a Si(Li) detector using an absorber technique. The pileup interval, in the pulse forming electronics of a PIXE detection system, has been improved to 100 ns X-ray energies above 8 keV by means of pulse shape analysis. Pulses due to tailing effects were also isolated but no major improvement was obtained. A means of reducing the increased background in the PIXE spectrum due to Compton scattering of high energetic gamma-rays in the Si(Li) crystal has been investigated by installation of an anti-Compton shield consisting of an organic scintillator mounted inside the detector cryostat and read out by a photomultiplier. Ionoluminescence, a new analytical technique for the nuclear microprobe, has shown to be a technique that can be employed as a fast diagnostic tool in imaging applications. The technique is based on analysis of the light that often can be observed when an ion beam impinges on a geological specimen. This light, luminescence, can often be associated with impurities in the crystal lattice or other structural defects. It can therefore be employed for revealing some chemical information about the specimens in contradiction to PIXE which is rather insensitive to chemical variations. The potential of the method is demonstrated and discussed both as an imaging tool and for spectroscopic studies. 19 refs, 10 figs

  18. Quantitative X-ray fluorescence analysis at the ESRF ID18F microprobe

    Vekemans, B; Somogyi, A; Drakopoulos, M; Kempenaers, L; Simionovici, A; Adams, F

    2003-01-01

    The new ID18F end-station at the European synchrotron radiation facility (ESRF) in Grenoble (France) is dedicated to sensitive and accurate quantitative micro-X-ray fluorescence (XRF) analysis at the ppm level with accuracy better than 10% for elements with atomic numbers above 18. For accurate quantitative analysis, given a high level of instrumental stability, major steps are the extraction and conversion of experimental X-ray line intensities into elemental concentrations. For this purpose a two-step quantification approach was adopted. In the first step, the collected XRF spectra are deconvoluted on the basis of a non-linear least-squares fitting algorithm (AXIL). The extracted characteristic line intensities are then used as input for a detailed Monte Carlo (MC) simulation code dedicated to XRF spectroscopy taking into account specific experimental conditions (excitation/detection) as well as sample characteristics (absorption and enhancement effects, sample topology, heterogeneity etc.). The iterative u...

  19. X-ray microprobe analysis of platelets. Principles, methods and review of the literature.

    Yarom, R

    1983-01-01

    Platelets are well suited to X-ray microanalysis as there is no need for chemical fixation or sectioning, and the concentrations of calcium and phosphorus are above 10(-3). The principles of the technique, the methods of specimen preparation, instrumental conditions during analysis and ways of quantitation are described. This is followed by a review of published reports and a brief summary of the author's own work in the field.

  20. Oxidation kinetics and auger microprobe analysis of some oxidized zirconium alloys

    Ploc, R.A.

    1989-01-01

    Oxidation kinetics at 300 o C in dry oxygen of 0.5 wt% binary alloys of iron, nickel, and chromium in zirconium were determined for several surface preparations. Further, chemical profiles of the oxides as they existed on the matrix and on the precipitates were obtained by sputtering and Auger electron analysis. The appearance of 'breakaway' oxidation was controlled by the surface finish of the alloy, a variable that could be used to eliminate the phenomenon for all alloys except the Zr/Ni binary, which required β-quenching to accomplish the same purpose. (author)

  1. Study of metal bioaccumulation by nuclear microprobe analysis of algae fossils and living algae cells

    Guo, P.; Wang, J.; Li, X.; Zhu, J.; Reinert, T.; Heitmann, J.; Spemann, D.; Vogt, J.; Flagmeyer, R.-H.; Butz, T.

    2000-01-01

    Microscopic ion-beam analysis of palaeo-algae fossils and living green algae cells have been performed to study the metal bioaccumulation processes. The algae fossils, both single cellular and multicellular, are from the late Neoproterozonic (570 million years ago) ocean and perfectly preserved within a phosphorite formation. The biosorption of the rare earth element ions Nd 3+ by the green algae species euglena gracilis was investigated with a comparison between the normal cells and immobilized ones. The new Leipzig Nanoprobe, LIPSION, was used to produce a proton beam with 2 μm size and 0.5 nA beam current for this study. PIXE and RBS techniques were used for analysis and imaging. The observation of small metal rich spores (<10 μm) surrounding both of the fossils and the living cells proved the existence of some specific receptor sites which bind metal carrier ligands at the microbic surface. The bioaccumulation efficiency of neodymium by the algae cells was 10 times higher for immobilized algae cells. It confirms the fact that the algae immobilization is an useful technique to improve its metal bioaccumulation

  2. Quantitative X-ray fluorescence analysis at the ESRF ID18F microprobe

    Vekemans, B.; Vincze, L.; Somogyi, A.; Drakopoulos, M.; Kempenaers, L.; Simionovici, A.; Adams, F.

    2003-01-01

    The new ID18F end-station at the European synchrotron radiation facility (ESRF) in Grenoble (France) is dedicated to sensitive and accurate quantitative micro-X-ray fluorescence (XRF) analysis at the ppm level with accuracy better than 10% for elements with atomic numbers above 18. For accurate quantitative analysis, given a high level of instrumental stability, major steps are the extraction and conversion of experimental X-ray line intensities into elemental concentrations. For this purpose a two-step quantification approach was adopted. In the first step, the collected XRF spectra are deconvoluted on the basis of a non-linear least-squares fitting algorithm (AXIL). The extracted characteristic line intensities are then used as input for a detailed Monte Carlo (MC) simulation code dedicated to XRF spectroscopy taking into account specific experimental conditions (excitation/detection) as well as sample characteristics (absorption and enhancement effects, sample topology, heterogeneity etc.). The iterative use of the MC code gives a 'no-compromise' solution for the quantification problem

  3. Quantitative X-ray fluorescence analysis at the ESRF ID18F microprobe

    Vekemans, B. E-mail: vekemans@uia.ua.ac.be; Vincze, L.; Somogyi, A.; Drakopoulos, M.; Kempenaers, L.; Simionovici, A.; Adams, F

    2003-01-01

    The new ID18F end-station at the European synchrotron radiation facility (ESRF) in Grenoble (France) is dedicated to sensitive and accurate quantitative micro-X-ray fluorescence (XRF) analysis at the ppm level with accuracy better than 10% for elements with atomic numbers above 18. For accurate quantitative analysis, given a high level of instrumental stability, major steps are the extraction and conversion of experimental X-ray line intensities into elemental concentrations. For this purpose a two-step quantification approach was adopted. In the first step, the collected XRF spectra are deconvoluted on the basis of a non-linear least-squares fitting algorithm (AXIL). The extracted characteristic line intensities are then used as input for a detailed Monte Carlo (MC) simulation code dedicated to XRF spectroscopy taking into account specific experimental conditions (excitation/detection) as well as sample characteristics (absorption and enhancement effects, sample topology, heterogeneity etc.). The iterative use of the MC code gives a 'no-compromise' solution for the quantification problem.

  4. Freeze-drying and related preparation techniques for biological microprobe analysis

    Wroblewski, R.; Wroblewski, J.; Anniko, M.; Edstroem, L.P.

    1985-01-01

    An X-ray microanalytical and morphological investigation has been carried out on rapidly frozen, freeze-dried or freeze-substituted tissues. A comparison was made between different embedding and polymerization procedures following freeze-substitution and freeze-drying. The investigation also included an analysis of specimens infiltrated, embedded and polymerized by ultraviolet irradiation at low temperatures with Lowicryl HM20. The morphological preservation of Lowicryl embedded tissue was adequate for the identification of different cell structures like nuclei, mitochondria, lysosomes and different types of endoplasmic reticulum. X-ray microanalytical investigation of low temperature embedded material displayed an elemental composition of cells and organelles similar to that found in freeze-dried cyosections. Compared with freeze-dried cryosections, low temperature embedded material could be sectioned for light microscopy and area of interest chosen for further thin sectioning. This is of great importance in work with tissues with complicated morphology and heterogenous cell populations

  5. Ion microprobe Sr isotope analysis of carbonates with about 5 {mu}m spatial resolution: An example from an ayu otolith

    Sano, Yuji [Center for Advanced Marine Research, Ocean Research Institute, University of Tokyo, Nakano-ku, Tokyo 164-8639 (Japan)], E-mail: ysano@ori.u-tokyo.ac.jp; Shirai, Kotaro [International Coastal Research Center, Ocean Research Institute, University of Tokyo, Otsuchi, Iwate 028-1102 (Japan); Takahata, Naoto; Amakawa, Hiroshi [Center for Advanced Marine Research, Ocean Research Institute, University of Tokyo, Nakano-ku, Tokyo 164-8639 (Japan); Otake, Tsuguo [International Coastal Research Center, Ocean Research Institute, University of Tokyo, Otsuchi, Iwate 028-1102 (Japan)

    2008-08-15

    A high lateral resolution secondary ion mass spectrometer (NanoSIMS NS50 ion microprobe) has been used to measure {sup 87}Sr/{sup 86}Sr ratios in natural CaCO{sub 3} samples. A {approx}2 nA O{sup -} primary beam was used to sputter a 5-7-{mu}m diameter crater on the sample surface and secondary positive ions were extracted for mass analysis using an accelerating voltage of 8 kV and a Mattauch-Herzog geometry. The multi-collector system was adjusted to detect {sup 43}Ca{sup +} (by a detector EM2), {sup 80}Ca{sub 2}{sup +} (EM3), {sup 86}Sr{sup +} (EM4), and {sup 87}Sr{sup +} (EM4b) ions at the same time. Then the magnetic field was scanned for the EM4 to detect {sup 85}Rb{sup +}, {sup 86}Sr{sup +} and {sup 87}Sr{sup +}, while the EM4b can measure {sup 86}Sr{sup +}, {sup 87}Sr{sup +} and {sup 88}Sr{sup +}, respectively. A mass resolution of 3600 at 10% peak height was attained with a flat peak top, while the sensitivity of Sr was about 10 cps/nA/ppm. An aragonite sample (coral skeleton standard; JCp-1) was used as a reference for Sr isotope ratio calibration. Repeated analyses of the JCp-1 show that the {sup 87}Sr/{sup 86}Sr ratio agrees well with the seawater signature within a precision of 0.3 per mille at 2{sigma}, after the series of corrections such as the Ca dimer, {sup 87}Rb, and a mass bias estimated by the {sup 88}Sr/{sup 86}Sr ratio. The method was applied to an otolith (ear-stone) from ayu (Plecoglossus altivelis altivelis) collected from the Yodo river, Japan. Although experimental errors are relatively large, up to 3 per mille at 2{sigma}, the ratios of the core region are higher than the seawater signature while more distal values agree well with seawater. The very outermost part again shows the relatively higher {sup 87}Sr/{sup 86}Sr ratios. The spatial variation of {sup 87}Sr/{sup 86}Sr ratios was consistent with amphidromous migration of the fish, namely, born in the lake and grown in the coastal sea and finally collected in a river.

  6. Ion microprobe Sr isotope analysis of carbonates with about 5 μm spatial resolution: An example from an ayu otolith

    Sano, Yuji; Shirai, Kotaro; Takahata, Naoto; Amakawa, Hiroshi; Otake, Tsuguo

    2008-01-01

    A high lateral resolution secondary ion mass spectrometer (NanoSIMS NS50 ion microprobe) has been used to measure 87 Sr/ 86 Sr ratios in natural CaCO 3 samples. A ∼2 nA O - primary beam was used to sputter a 5-7-μm diameter crater on the sample surface and secondary positive ions were extracted for mass analysis using an accelerating voltage of 8 kV and a Mattauch-Herzog geometry. The multi-collector system was adjusted to detect 43 Ca + (by a detector EM2), 80 Ca 2 + (EM3), 86 Sr + (EM4), and 87 Sr + (EM4b) ions at the same time. Then the magnetic field was scanned for the EM4 to detect 85 Rb + , 86 Sr + and 87 Sr + , while the EM4b can measure 86 Sr + , 87 Sr + and 88 Sr + , respectively. A mass resolution of 3600 at 10% peak height was attained with a flat peak top, while the sensitivity of Sr was about 10 cps/nA/ppm. An aragonite sample (coral skeleton standard; JCp-1) was used as a reference for Sr isotope ratio calibration. Repeated analyses of the JCp-1 show that the 87 Sr/ 86 Sr ratio agrees well with the seawater signature within a precision of 0.3 per mille at 2σ, after the series of corrections such as the Ca dimer, 87 Rb, and a mass bias estimated by the 88 Sr/ 86 Sr ratio. The method was applied to an otolith (ear-stone) from ayu (Plecoglossus altivelis altivelis) collected from the Yodo river, Japan. Although experimental errors are relatively large, up to 3 per mille at 2σ, the ratios of the core region are higher than the seawater signature while more distal values agree well with seawater. The very outermost part again shows the relatively higher 87 Sr/ 86 Sr ratios. The spatial variation of 87 Sr/ 86 Sr ratios was consistent with amphidromous migration of the fish, namely, born in the lake and grown in the coastal sea and finally collected in a river

  7. High current pulsed positron microprobe

    Howell, R.H.; Stoeffl, W.; Kumar, A.; Sterne, P.A.; Cowan, T.E.; Hartley, J.

    1997-01-01

    We are developing a low energy, microscopically focused, pulsed positron beam for defect analysis by positron lifetime spectroscopy to provide a new defect analysis capability at the 10 10 e + s -l beam at the Lawrence Livermore National Laboratory electron linac. When completed, the pulsed positron microprobe will enable defect specific, 3-dimensional maps of defect concentrations with sub-micron resolution of defect location. By coupling these data with first principles calculations of defect specific positron lifetimes and positron implantation profiles we will both map the identity and concentration of defect distributions

  8. San Francisco Estuary Striped Bass Migration History Determined by Electron-microprobe Analysis of Otolith Sr/Ca Ratio

    Ostrach, D J; Phillis, C C; Weber, P K; Ingram, B L; Zinkl, J G

    2004-09-17

    Habitat use has been shown to be an important factor in the bioaccumulation of contaminants in striped bass. This study examines migration in striped bass as part of a larger study investigating bioaccumulation and maternal transfer of xenobiotics to progeny in the San Francisco Estuary system. Habitat use, residence time and spawning migration over the life of females (n = 23) was studied. Female striped bass were collected between Knights Landing and Colusa on the Sacramento River during the spawning runs of 1999 and 2001. Otoliths were removed, processed and aged via otolith microstructure. Subsequently, otoliths were analyzed for strontium/calcium (Sr/Ca) ratio using an electron-microprobe to measure salinity exposure and to distinguish freshwater, estuary, and marine habitat use. Salinity exposure during the last year before capture was examined more closely for comparison of habitat use by the maternal parent to contaminant burden transferred to progeny. Results were selectively confirmed by ion microprobe analyses for habitat use. The Sr/Ca data demonstrate a wide range of migratory patterns. Age of initial ocean entry differs among individuals before returning to freshwater, presumably to spawn. Some fish reside in freshwater year-round, while others return to more saline habitats and make periodic migrations to freshwater. Frequency of habitat shifts and residence times differs among fish, as well as over the lifetime of individual fish. While at least one fish spent its final year in freshwater, the majority of spawning fish spent their final year in elevated salinity. However, not all fish migrated to freshwater to spawn in the previous year. Results from this investigation concerning migration history in striped bass can be combined with contaminant and histological developmental analyses to better understand the bioaccumulation of contaminants and the subsequent effects they and habitat use have on fish populations in the San Francisco Estuary system.

  9. Application of synchrotron-radiation-based x-ray microprobe techniques for the analysis of recombination activity of metals precipitated at Si/SiGe misfit dislocations

    Vyvenko, O F; Istratov, A A; Weber, E R; Kittler, M; Seifert, W

    2002-01-01

    In this study we report application of synchrotron-radiation-based x-ray microprobe techniques (the x-ray-beam-induced current (XBIC) and x-ray fluorescence (mu-XRF) methods) to the analysis of the recombination activity and space distribution of copper and iron in the vicinity of dislocations in silicon/silicon-germanium structures. A combination of these two techniques enables one to study the chemical nature of the defects and impurities and their recombination activity in situ and to map metal clusters with a micron-scale resolution. XRF analysis revealed that copper formed clearly distinguishable precipitates along the misfit dislocations. A proportional dependence between the XBIC contrast and the number of copper atoms in the precipitates was established. In hydrogen-passivated iron-contaminated samples we observed clusters of iron precipitates which had no recombination activity detectable by the XBIC technique as well as iron clusters which were not completely passivated.

  10. Mass spectroscopic analysis of atmospheric particulate matter

    Wippel, R.

    1997-02-01

    Particulate matter (PM) in the atmosphere vary greatly in origin, in their physical and chemical properties and their effects on climate, atmospheric chemistry and health. Aerosol particles with an aerodynamic diameter less than two μm can enter the respiratory tract of humans when inhaled. Bulk analysis of ambient dust particles was performed using an inductively coupled plasma mass spectrometer (ICP-MS). The size-fractionated collected samples were analyzed after a leaching procedure that simulates the solution reactions occurring in the lungs. A disadvantage of bulk analysis is that it gives no information about the distribution of a certain element within the particles under investigation. A Laser-Microprobe-Mass-Analyzer (LAMMA-500) was used to obtain this information. At sampling sites in Austria and in Zimbabwe, Africa, single particles were sampled using a self-made impactor. One of the final aims in environmental analysis is to successfully apply receptor models that relate the chemical and physical properties of a receptor site to a source. The knowledge of the sources of atmospheric particulate matter is essential for environmental policy makers as well as for epidemiological studies. Artificial neural networks (ANN) have a remarkable ability to handle LAMMA-data. Three ANNs were used as a pattern recognition tool for LAMMA mass spectral data: a back-propagation net, a Kohonen network,and a counter-propagation net. Standard source profiles from the United States Environmental Protection Agency were used as training and test data of the different nets. The elemental patterns of the sum of 100 mass spectra of fine dust particles were presented to the trained nets and satisfactory recognition (> 80 %) was obtained. (author)

  11. The upgraded Amsterdam nuclear microprobe

    Vis, R.D.; Kramer, J.L.A.M.; Tros, G.H.J.; Langevelde, F. van; Mars, L.

    1993-01-01

    The improvement of the facilities at our University consists of three phases. In phase 1, a 1.7 MV NEC tandem-Pelletron accelerator has been installed. The accelerator serves as injector for two beam lines, subsequently for macro- and micro-analysis. Moreover, an interconnection has been made with a beam line from our 400 kV high voltage Van de Graaff accelerator in order to enable injection of these very intense low energy beams in these two lines. Apart from new vacuum equipment and conventional beam steering and focussing elements, the experimental facilities are replaced from the cyclotron experimental hall to the newly organised experimental hall. In the phases 2 and 3, which are not yet completed, a second ion source for the Pelletron and a new or extended focussing unit for the microprobe will complete the overall operation. (orig.)

  12. Metabolite localization by atmospheric pressure high-resolution scanning microprobe matrix-assisted laser desorption/ionization mass spectrometry imaging in whole-body sections and individual organs of the rove beetle Paederus riparius.

    Bhandari, Dhaka Ram; Schott, Matthias; Römpp, Andreas; Vilcinskas, Andreas; Spengler, Bernhard

    2015-03-01

    Mass spectrometry imaging provides for non-targeted, label-free chemical imaging. In this study, atmospheric pressure high-resolution scanning microprobe matrix-assisted laser desorption/ionization mass spectrometry imaging (AP-SMALDI MSI) was used for the first time to describe the chemical distribution of the defensive compounds pederin, pseudopederin, and pederon in tissue sections (16 μm thick) of the rove beetle Paederus riparius. The whole-insect tissue section was scanned with a 20-μm step size. Mass resolution of the orbital trapping mass spectrometer was set to 100,000 at m/z 200. Additionally, organ-specific compounds were identified for brain, nerve cord, eggs, gut, ovaries, and malpighian tubules. To confirm the distribution of the specific compounds, individual organs from the insect were dissected, and MSI experiments were performed on the dissected organs. Three ganglia of the nerve cord, with a dimension of 250-500 μm, were measured with 10-μm spatial resolution. High-quality m/z images, based on high spatial resolution and high mass accuracy were generated. These features helped to assign mass spectral peaks with high confidence. Mass accuracy of the imaging experiments was section. Without any labeling, we assigned key lipids for specific organs to describe their location in the body and to identify morphological structures with a specificity higher than with staining or immunohistology methods.

  13. PIXE macro and microprobe techniques in archaeometry

    Brissaud, I.; Lagarde, G.; Houdayer, A.

    1987-01-01

    PIXE analysis method is applied to archaeometry problems. Advantages and disadvantages are emphasized. Some examples are presented which show the difficulties: especially important heterogeneities of ceramics, old coins and metals restrain from the use of this technique. Other analysis systems, less expensive, like electron microbrobe or x-ray fluorescence spectrometry, are compared with conventional PIXE method. The importance of proton microprobe is explained. (author) 40 refs.; 7 figs.; 5 tabs

  14. Study on mineral components of rat calvaria by means of X-ray powder diffraction analysis and Raman microprobe spectroscopy

    Tamura, Norihiro [Meikai Univ., Sakado, Saitama (Japan). School of Dentistry

    2000-07-01

    The present study was designed to examine the occurrence of the precursor minerals of hydroxyapatite (HA) during the process of HA formation in the rat calvaria. Dried and powdered rat calvaria and synthetic samples, such as HA, dicalcium phosphate dihydrate (DCPD), octacalcium phosphate (OCP), ({beta}-calcium pyrophosphate) and ({beta}-tricalcium phosphate), were used. Determinations were carried out by X-ray powder diffraction and Raman microprobe spectrometry. In general, significant widening of the diffraction peaks was shown to occur after the plasma ashing was performed for the X-ray diffraction. As a result, two adjacent peaks seen normally in the diffraction angles (2 {theta}) 30-35 deg, which is a characteristic feature of HA, were found to fuse with each other, forming a widened single peak. Also, there was a tendency for the intensity of the diffraction peaks to increase with age. With regard to the effect of plasma ashing on the crystallograms of synthetic specimens, all specimens manifested sharp peak patterns except DCPD and OCP. In contrast, a widening of diffraction peaks was observed in the DCPD and OCP samples, indicating that crystallinity had changed during the pretreatment. Results obtained from both vital and synthetic samples after heat treatment at 1000 deg C were as follow: Clearcut diffraction patterns, characteristics of HA, were obtained in all of the calvaria samples. Further, {beta}-TCP was produced by heat treatment of OCP, and its pattern was detected in the samples from rats younger than 6 days of age. Amounts of {beta}-TCP in percentage were disclosed to be 40.2% in embryonal samples, 28.4% in newborn samples, and 18.6% in 6-day-old samples. But no {beta}-TCP could be detected in the 12-week-old samples, indicating that the amount of {beta}-TCP in calvaria decreased with age. We also found that ashing pretreatment did not cause any changes in the samples of HA, {beta}-CPP, and {beta}-TCP. Further, DCPD and {beta}-CPP samples shared

  15. Study on mineral components of rat calvaria by means of X-ray powder diffraction analysis and Raman microprobe spectroscopy

    Tamura, Norihiro

    2000-01-01

    The present study was designed to examine the occurrence of the precursor minerals of hydroxyapatite (HA) during the process of HA formation in the rat calvaria. Dried and powdered rat calvaria and synthetic samples, such as HA, dicalcium phosphate dihydrate (DCPD), octacalcium phosphate (OCP), (β-calcium pyrophosphate) and (β-tricalcium phosphate), were used. Determinations were carried out by X-ray powder diffraction and Raman microprobe spectrometry. In general, significant widening of the diffraction peaks was shown to occur after the plasma ashing was performed for the X-ray diffraction. As a result, two adjacent peaks seen normally in the diffraction angles (2 θ) 30-35 deg, which is a characteristic feature of HA, were found to fuse with each other, forming a widened single peak. Also, there was a tendency for the intensity of the diffraction peaks to increase with age. With regard to the effect of plasma ashing on the crystallograms of synthetic specimens, all specimens manifested sharp peak patterns except DCPD and OCP. In contrast, a widening of diffraction peaks was observed in the DCPD and OCP samples, indicating that crystallinity had changed during the pretreatment. Results obtained from both vital and synthetic samples after heat treatment at 1000 deg C were as follow: Clearcut diffraction patterns, characteristics of HA, were obtained in all of the calvaria samples. Further, β-TCP was produced by heat treatment of OCP, and its pattern was detected in the samples from rats younger than 6 days of age. Amounts of β-TCP in percentage were disclosed to be 40.2% in embryonal samples, 28.4% in newborn samples, and 18.6% in 6-day-old samples. But no β-TCP could be detected in the 12-week-old samples, indicating that the amount of β-TCP in calvaria decreased with age. We also found that ashing pretreatment did not cause any changes in the samples of HA, β-CPP, and β-TCP. Further, DCPD and β-CPP samples shared the same diffraction pattern, and OCP

  16. Phospholipid Topography of Whole-Body Sections of the Anopheles stephensi Mosquito, Characterized by High-Resolution Atmospheric-Pressure Scanning Microprobe Matrix-Assisted Laser Desorption/Ionization Mass Spectrometry Imaging.

    Khalil, Saleh M; Römpp, Andreas; Pretzel, Jette; Becker, Katja; Spengler, Bernhard

    2015-11-17

    High-resolution atmospheric-pressure scanning microprobe matrix-assisted laser desorption/ionization mass spectrometry imaging (AP-SMALDI MSI) has been employed to study the molecular anatomical structure of rodent malaria vector Anopheles stephensi mosquitoes. A dedicated sample preparation method was developed which suits both, the special tissue properties of the sample and the requirements of high-resolution MALDI imaging. Embedding in 5% carboxymethylcellulose (CMC) was used to maintain the tissue integrity of the whole mosquitoes, being very soft, fragile, and difficult to handle. Individual lipid compounds, specifically representing certain cell types, tissue areas, or organs, were detected and imaged in 20 μm-thick whole-body tissue sections at a spatial resolution of 12 μm per image pixel. Mass spectrometric data and information quality were based on a mass resolution of 70,000 (at m/z 200) and a mass accuracy of better than 2 ppm in positive-ion mode on an orbital trapping mass spectrometer. A total of 67 imaged lipids were assigned by database search and, in a number of cases, identified via additional MS/MS fragmentation studies directly from tissue. This is the first MSI study at 12 μm spatial resolution of the malaria vector Anopheles. The study provides insights into the molecular anatomy of Anopheles stephensi and the distribution and localization of major classes of glycerophospholipids and sphingolipids. These data can be a basis for future experiments, investigating, e.g., the metabolism of Plasmodium-infected and -uninfected Anopheles mosquitoes.

  17. Synchrotron radiation XRF microprobe study of human bone tumor slice

    Huang Yuying; Zhao Limin; Wang Zhouguang; Shao Hanru; Li Guangcheng; Wu Yingrong; He Wei; Lu Jianxin; He Rongguo

    1999-01-01

    The experimental apparatus of X-ray fluorescence (XRF) microprobe analysis at Beijing Synchrotron Radiation Facility (BSRF) is described. Using the bovine liver as the standard reference, the minimum detection limit (MDL) of trace element was measured to determine the capability of biological sample analysis by synchrotron radiation XRF microprobe. The relative change of the content of the major or trace element in the normal and tumor part of human bone tissue slice was investigated. The experimental result relation to the clinical medicine was also discussed. (author)

  18. Arсhaeomineralogy of Ancient Nonferrous Metallurgy Pieces of the Perm Region: Experience of Usage of Electron Microprobe Analysis

    I. I. Chaykovsky

    2016-12-01

    Full Text Available A series of archaeological features has been studied by means of the scanning electronic microscopy. It was shown that due to the oxidation process, the surface layer is enriched with some elements, which were present at unaltered metal (Ag, Pb and those included later (As, Zn, Pb. It imposes meaningful limitation for use of the X-ray fluorescence and spectral analysis, which allow obtaining only total (patina + metal composition. Sixteen minerals (oxides, carbonates, sulphates, chlorides, phosphates, sulfides and native phases are established in patina composition. Tin bronze structure contains the impurities, which may be an evidence of import to Perm Region of tin and silver possibly from Altai, tin and lead possibly from Karelia during "harinsky" and "rodanovsky" cultures respectively. Various composition of the alloys used for casting and filigree witnesses that ancient metallurgists had known about alloys handling. The presence of barium and fluorine can tell us about composition of the used furnacecharge. The obtained data may be the basis for chemical-metallurgical typification of pieces from nonferrous (and noble metals.

  19. X-ray microprobe analysis of the retina and RPE in sheep with ovine ceroid-lipofuscinosis

    Samuelson, D.A.; Armstrong, D.; Jolly, R.

    1990-01-01

    Ovine ceroid-lipofuscinosis (OCL) is one animal model for the human condition, and because autofluorescent lipopigments are prominent in the brain and eye, it may also prove useful as a model for aging. For example, a progressive decline in electrical recording from brain and retina are observed in both aging and OCL. Samples of retinal and retinal pigment epithelial (RPE) tissues were obtained from a young control. 2 animals with OCL and a normal aged sheep. Specimens were cryo-fractured and examined by scanning electron microscopy/x-ray microanalysis. Measurements made of 6 individual cells in the ganglion layer of OCL specimens, the remainder of the retina, and RPE showed age-related changes in zinc, iron, and copper which were associated with lipopigment accumulation in the RPE. There was marked decrease in phosphate, sulfur, and manganese levels, as photoreceptor cells and their outer segments are lost in the disease process. This is the first report of metal analysis in the retina and RPE in a disease entity, and as a function of normal aging

  20. Microprobe analysis, iono- and photo-luminescence of Mn2+ activated ZnGa2O4 fibres

    Santos, N.F.; Fernandes, A.J.S.; Alves, L.C.; Sobolev, N.A.; Alves, E.; Lorenz, K.; Costa, F.M.; Monteiro, T.

    2013-01-01

    Cubic ZnGa 2 O 4 fibres have been grown by the laser floating zone technique with different pulling rates. In fibres activated with manganese ions, the room temperature photo- and iono-luminescence is dominated by an intense green emission which is observed by the naked eye. The green band is due to an overlap of the 4 T 1 → 6 A 1 intraionic transitions of the Mn 2+ ions in different sites in the gallate host. The fibres’ photoluminescence spectra have been found to be dependent on the excitation energy. Additionally, the intensity of the green photo- and iono-luminescence is strongly sensitive to the measurement temperature and proton irradiation time. Micro PIXE analysis was used in order to verify the homogeneous distribution of the Mn luminescence activators and determine its concentration as well as for verification of impurity contents that may have been incorporated during the fibres growth. The potential of ionoluminescence measurements for characterization of optical materials is discussed

  1. Imaging mass spectrometry statistical analysis.

    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.

  2. The CEA nuclear microprobe. Description, possibilities, application examples

    Engelmann, C.; Bardy, J.

    1986-05-01

    The nuclear microprobe installed on one of the beam lines of a 4 MV Van de Graaff located in the Research Center of Bruyeres-le-Chatel is described. The various possibilities, particularly the imaging system, and the performances of the instrument are exposed. Two typical application examples concerning, the first, the determination of the deuterium and tritium in glass microballons, the second, the detection and the localization of carbon and oxygen in the superficial layer of lithium hydride pellets, are given. Preliminary results of some other application examples are also presented. The advantages of the nuclear microprobe over the other ponctual analysis techniques are emphasized. 7 refs, 19 figs [fr

  3. High resolution, high sensitivity imaging and analysis of minerals and inclusions (fluid and melt) using the new CSIRO-GEMOC nuclear microprobe

    Ryan, C.G.; McInnes, B.M.; Van Achterbergh, E.; Williams, P.J.; Dong, G.; Zaw, K.

    1999-01-01

    Full text: The new CSIRO-GEMOC Nuclear Microprobe (NMP) The instrument was designed specifically for minerals analysis and imaging and to achieve ppm to sub-ppm sensitivity at a spatial resolution of 1-2 μm using X-rays and y-rays induced by MeV energy ion beams. The key feature of the design is a unique magnetic quadrupole quintuplet ion focussing system that combines high current with high spatial resolution (Ryan et al., 1999). These design goals have been achieved or exceeded. On the first day of operation, a spot-size of 1.3 μm was obtained at a beam current of 0.5 nA, suitable for fluid inclusion analysis and imaging. The spot-size grows to just 1.8 μm at 10 nA (3 MeV protons), ideal for mineralogical samples with detection limits down to 0.2 ppm achieved in quantitative, high resolution, trace element images. Applications of the NMP include: research into ore deposit processes through trace element geochemistry, mineralogy and fluid inclusion analysis of ancient deposits and active sea-floor environments, ore characterization, and fundamental studies of mantle processes and extraterrestrial material. Quantitative True Elemental Imaging Dynamic Analysis is a method for projecting quantitative major and trace element images from proton-induced X-ray emission (PIXE) data obtained using the NMP (Ryan et al., 1995). The method un-mixes full elemental spectral signatures to produce quantitative images that can be directly interrogated for the concentrations of all elements in selected areas or line projections, etc. Fluid Inclusion Analysis and Imaging The analysis of fluids trapped as fluid inclusions in minerals holds the key to understanding ore metal pathways and ore formation processes. PIXE analysis using the NMP provides a direct non-destructive method to determine the composition of these trapped fluids with detection limits down to 20 ppm. However, some PIXE results have been controversial, such as the strong partitioning of Cu into the vapour phase (e

  4. Use of the ion microprobe in geological dating

    Compston, W.; Williams, I.S.; Black, L.P.

    1983-01-01

    SHRIMP, the Sensitive High Resolution Ion Microprobe with computerised control and data acquisition system, has recently been commissioned. It is used within the Research School of Earth Sciences, Australian National University, for the isotopic analysis of geological samples. Principles of operation and geological applications are outlined. One example described is the application to Pb-U dating of zircon

  5. Mass spectrometric analysis of lithium

    Chitambar, S.A.; Kavimandan, V.D.; Aggarwal, S.K.; Ramasubramanian, P.A.; Shah, P.M.; Almoula, A.I.; Acharya, S.N.; Parab, A.R.; Jain, H.C.; Mathews, C.K.; Ramaniah, M.V.

    1978-01-01

    The details of investigations carried out on the isotopic analysis of lithium using surface ionisation mass spectrometry are presented. Various parameters affecting the precision in isotopic analysis of lithium are discussed. A precision of 1% is achieved in the relative isotope abundance measurement. (author)

  6. New electron microprobe for radioactive materials

    Perrot, M.; Geoffroy, G.; Trotabas, M.

    1989-01-01

    The latest model of CAMECA microprobe SX 50R has just been set up in the high activity laboratory of the Centre d'Etudes Nucleaires de SACLAY. It has been especially designed for the examination of nuclear fuel and irradiated materials. The spectrometers are protected from the radioactivity by an armour plate and the entire equipment has been installed into a special cell in order to protect the operators. The special sample holder allows to examine specimens as large as 80 mm in diameter. One of the interesting uses concerns the quantitative determination of the oxygen content in zircaloy oxidized by steam at high temperature. This analysis was made possible by using the new type of crystals (multilayer)

  7. Protein Analysis by Mass Spectrometry

    Cindic, M.

    2008-04-01

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

  8. Development of a nuclear microprobe and its application to neurobiology

    Tapper, Staffan.

    1989-01-01

    A nuclear microprobe has been developed at the Pelletron accelerator in Lund. The design of the achromatic beam focusing system as well as of the beam scanning system is described. The focusing system consists of three magnetic- and three electrostatic quadrupole lenses together forming an chromatic quadrupole triplet with symmetric focusing properties. The beam quality from the accelerator has been improved by use of ultrathin stripper foils. The nuclear microprobe set-up has been applied to investigation of brain tissue specimens. The elemantal disorder following epileptic seizures has been studied by micro-PIXE analysis. A combination of macro- and micro-PIXE analysis have been utilized in an investigaiton of elemental differences between normal human brain and human brain tumours. In the context of the quantification procedure in micro-PIXE analysis, callibration and X-ray detector response function are discussed. (author)

  9. New generation nuclear microprobe systems

    Jamieson, David N.

    2001-01-01

    Over the past 20 years, the minimum probe size for nuclear microscopy has stayed around 1 μm with only a few groups reporting a sub-micron probe size around 0.5 μm. No breakthroughs in nuclear microprobe design have been forthcoming to produce dramatic improvements in spatial resolution. The difficulties of breaking the constraints that are preventing reduction of the probe size have been well recognised in the past. Over the past 5 years it has become clear that some of these constraints may not be as limiting as first thought. For example, chromatic aberration clearly is not as significant as implied from first-order ion optics calculations. This paper reviews the constraints in view of the increased understanding of the past 5 years and looks at several new approaches, presently being evaluated in Melbourne and elsewhere, on how to make progress. These approaches include modified RF ion sources for improved beam brightness and exploitation of relaxed constraints on some lens aberrations allowing the use of high demagnification probe forming lens systems

  10. 7th international conference on Nuclear microprobe technology and applications

    2000-01-01

    This colloquium gives an up-to-date report on the continuously advancing applications and development of microbeam technology. It presents abstracts and oral contributions in the following domains: microprobes facilities, analysis techniques, imaging techniques, micro-ion beam modification of materials, microelectronics, applications in Material Sciences in Biology in Medicine in earth and planetary Sciences in environment in art in archaeology, alternative techniques. (A.L.B.)

  11. A study of VMS ore deposits by the proton microprobe

    Huston, D.L.; Large, R.R.; Bottril, R.S.; Sie, S.H.; Ryan, C.G.

    1991-01-01

    As part of studies into the mineralogical distribution of gold in volcanogenic massive sulfide (VMS) ore deposits PIXE analysis by the proton microprobe has been used to determine the gold content of pyrite and arsenopyrite from the Rosebery, Mt. Chalmers and Mt. Lyell deposits. In addition, the concentrations of Co, Ni, Cu, Zn, As, Sr, Y, Zr, Mo, Ag, Sb, Te, Au, Tl, Pb and Bi were also determined. 4 refs., 1 tab

  12. Digital pulse processor for ion beam microprobe imaging

    Bogovac, M.; Jaksic, M.; Wegrzynek, D.; Markowicz, A.

    2009-01-01

    Capabilities of spectroscopic ion beam analysis (IBA) techniques that are available in ion microprobe facilities can be greatly improved by the use of digital pulse processing. We report here development of a digital multi parameter data acquisition system suitable for IBA imaging applications. Input signals from charge sensitive preamplifier are conditioned by using a simple circuit and digitized with fast ADCs. The digitally converted signals are processed in real time using FPGA. Implementation of several components of the system is presented.

  13. Novel imaging techniques for the nuclear microprobe

    Saint, A.

    1998-01-01

    Many of the developments of the scanning electron microscope (SEM) have been paralleled during the development of the scanning nuclear microprobe. Secondary electrons were used in the early development of both devices to provide specimen imaging due to the large numbers of secondaries produced per incident charged particle. Other imaging contrast techniques have also been developed on both machines. These include X-ray analysis, scattering contrast, transmission microscopy, channelling induced charge and others. The 'cross-section dependent' imaging techniques such as PIXE, RBS, NRA, etc., rely on the beam current on target for a given resolution. This has prompted research and development of brighter ion sources to maintain probe resolution at high beam current. Higher beam current bring problems with beam damage to the specimen. Low beam current techniques however rely on high countrate data collection systems, but this is only for spectroscopy. To produce an image we can increase beam currents to produce live-time images for specimen manipulation and observation. The work presented here will focus on some developments in live-time imaging with a nuclear micro probe that have taken place recently at the School of Physics, Microanalytical Research Centre (MARC), University of Melbourne

  14. Tin accumulation in spermatozoa of the rats exposed to tributyltin chloride by synchrotron radiation X-ray fluorescence (SR-XRF) analysis with microprobe

    Homma-Takeda, S.; Nishimura, Y.; Terada, Y.; Ueno, S.; Watanabe, Y.; Yukawa, M.

    2005-01-01

    Organotin compounds are widely used in industry and its environmental contamination by these compounds has recently become a concern. It is known that they act as endocrine disruptors but details of the dynamics of Sn in reproductive organs are still unknown. In the present study, we attempted to determine Sn distribution in the testis of rats exposed to tributyltin chloride (TBTC) by inductively coupled argon plasma-mass spectrometry (ICP-MS) for microdissectioned seminiferous tubules and cell-selective metal determination of synchrotron radiation X-ray florescence (SR-XRF) analysis. TBTC was orally administered to rats at a dose of 45 μmol/kg per day for 3 days. One day later, Sn was detected in the microdissectioned seminiferous tubules at a level approximately equivalent to that in the testis. Significant stage-specificity of Sn accumulation was not observed in the experimental model. Sn was also detected in spermatozoa at the stage VIII seminiferous tubule, which are the final step of spermatogenesis in the testis. These data indicate that Sn accumulates in germ cells as well as in spermatozoa in a short period of TBTC exposure

  15. Tin accumulation in spermatozoa of the rats exposed to tributyltin chloride by synchrotron radiation X-ray fluorescence (SR-XRF) analysis with microprobe

    Homma-Takeda, S. [Environmental Radiation Protection Research Group, National Institute of Radiological Sciences, 4-9-1 Anagawa, Inage-ku Chiba 263-8555 (Japan)]. E-mail: shino_ht@nirs.go.jp; Nishimura, Y. [Environmental Radiation Protection Research Group, National Institute of Radiological Sciences, 4-9-1 Anagawa, Inage-ku Chiba 263-8555 (Japan); Terada, Y. [Japan Synchrotron Radiation Research Institute, Mikazuki, Hyogo 679-5198 (Japan); Ueno, S. [School of Veterinary Medicine and Animal Sciences, Kitasato University, Towada, Aomori 034-8628 (Japan); Watanabe, Y. [Environmental Radiation Protection Research Group, National Institute of Radiological Sciences, 4-9-1 Anagawa, Inage-ku Chiba 263-8555 (Japan); Yukawa, M. [Environmental Radiation Protection Research Group, National Institute of Radiological Sciences, 4-9-1 Anagawa, Inage-ku Chiba 263-8555 (Japan)

    2005-04-01

    Organotin compounds are widely used in industry and its environmental contamination by these compounds has recently become a concern. It is known that they act as endocrine disruptors but details of the dynamics of Sn in reproductive organs are still unknown. In the present study, we attempted to determine Sn distribution in the testis of rats exposed to tributyltin chloride (TBTC) by inductively coupled argon plasma-mass spectrometry (ICP-MS) for microdissectioned seminiferous tubules and cell-selective metal determination of synchrotron radiation X-ray florescence (SR-XRF) analysis. TBTC was orally administered to rats at a dose of 45 {mu}mol/kg per day for 3 days. One day later, Sn was detected in the microdissectioned seminiferous tubules at a level approximately equivalent to that in the testis. Significant stage-specificity of Sn accumulation was not observed in the experimental model. Sn was also detected in spermatozoa at the stage VIII seminiferous tubule, which are the final step of spermatogenesis in the testis. These data indicate that Sn accumulates in germ cells as well as in spermatozoa in a short period of TBTC exposure.

  16. Beam optics on the Melbourne proton microprobe

    Jamieson, D.N.; Colman, R.A.; Allan, G.L.; Legge, G.J.F.

    1985-01-01

    This review paper summarises results of ion optics development work conducted on the Melbourne Proton Microprobe and the associated Pelletron accelerator. The properties of a field ionization ion source have been investigated with the aim of replacing the existing R.F. ion source in the accelerator in order to obtain a brighter beam for the microprobe. The electrostatic emitter lens in the terminal of the accelerator has also been investigated with the aim of improving the focus of the accelerated beam. Finally, the aberrations of the probe forming lens system have been studied and it is shown how some of these may be corrected with an octupole lens

  17. Development of a new measurement method for fast breeder reactor fuel burnup using a shielded ion microprobe analyzer

    Mizuno, M.; Enokido, Y.; Itaki, T.; Kono, K.; Unno, I.; Yamanouchi, S.

    1985-01-01

    A new method of burnup measurement using a shielded ion microprobe analyzer (SIMA) has been developed. The method is based on the isotope analysis of uranium, plutonium, and fission products in irradiated mixed oxide fuel by means of secondary ion mass spectrometry (SIMS). Fourteen samples irradiated in the Japanese experimental fast reactor JOYO were examined. The maximum local burnup of JOYO MK-I core fuels was about5.1 at. %. The axial burnup distribution of the fuel pin was in good agreement with that of the sibling pin in the same subassembly, measured by surface ionization mass spectrometry, which requires the chemical separation of fission products and heavy metals. The new method facilitates the rapid and accurate measurement of fast breeder reactor fuel burnup without human radiation exposure during sample preparation and analysis

  18. Mixed beams for the nuclear microprobe

    Saint, A.; Breese, M.B.H.; Legge, G.L.F. [Melbourne Univ., Parkville, VIC (Australia). School of Physics

    1996-12-31

    Recently the Micro-Analytical Research Centre (MARC) at Melbourne University has developed a technique to provide mixed beams of ions for a magnetically focussed nuclear microprobe. Such a mixed beam is defined as two (or more) beams of different species ions that can quickly and easily be made to have the same magnetic rigidity R{sub m} = (mE/q{sup 2}) and therefore be transported, focused and scanned the same in a magnetic nuclear microprobe. The production of mixed beams in an electrostatically focussed micro- probe have already been demonstrated. This paper will show how mixed beams can be produced on a single-ended accelerator. Indications of how to produce them on a tandem will also be given. Applications of these mixed beams in micro-lithography, scanning transmission ion microscopy (STIM) imaging and ion beam induced charge (IBIC) imaging will also be presented. 3 refs., 3 figs.

  19. Mixed beams for the nuclear microprobe

    Saint, A; Breese, M B.H.; Legge, G L.F. [Melbourne Univ., Parkville, VIC (Australia). School of Physics

    1997-12-31

    Recently the Micro-Analytical Research Centre (MARC) at Melbourne University has developed a technique to provide mixed beams of ions for a magnetically focussed nuclear microprobe. Such a mixed beam is defined as two (or more) beams of different species ions that can quickly and easily be made to have the same magnetic rigidity R{sub m} = (mE/q{sup 2}) and therefore be transported, focused and scanned the same in a magnetic nuclear microprobe. The production of mixed beams in an electrostatically focussed micro- probe have already been demonstrated. This paper will show how mixed beams can be produced on a single-ended accelerator. Indications of how to produce them on a tandem will also be given. Applications of these mixed beams in micro-lithography, scanning transmission ion microscopy (STIM) imaging and ion beam induced charge (IBIC) imaging will also be presented. 3 refs., 3 figs.

  20. Biomedical application of the nuclear microprobe

    Lindh, U.

    1987-01-01

    The Studsvik Nuclear Microprobe (SMP) has mainly been devoted to applications in the biomedical field. Its ultimate resolution is reached at 2.9x2.9 μm 2 with a proton current of 100 pA. With this performance the SMP has been used in a wide range of disciplines covering environmental hygiene, toxicology, various aspects of internal medicine and trace element physiology. Examples of recent applications in these fields are described. (orig.)

  1. Development of a nuclear microprobe at IGCAR

    Ramesh, C.; Nair, K.G.M.; Thampi, N.S.; Saha, B.; Mathews, C.K.

    1988-01-01

    A nuclear microprobe is being developed at IGCAR. The system is being built to determine the profiles of light elements, specially carbon in clad and other structural materials of a fast breeder reactor. By scanning a focussed charged particle beam on the sample surface and by detecting the charged particle induced emissions, an elemental map of the surface is obtained. The paper gives the basic design considerations and present status. (author)

  2. Beam developments for the Harwell microprobe system

    Read, P.M.; Cookson, J.A.; Alton, G.D.

    1986-01-01

    A consequence of the rapid development of micron and submicron size electronic devices is the diminished applicability of high energy ion microprobes with their present resolution limitations to the study of such components. Although submicron beams have been reported the available beam current is barely sufficiently for PIXE and is not adequate for RBS. This lack of lateral resolution is due to low beam brightness at the microprobe object and aberrations in the focusing elements. As part of a program to address these problems the Harwell microprobe lens has been relocated on a new 5 MV Laddertron accelerator. The increased brightness and improved stability of this facility has so far led to a reduction in beam size from 3 x 3 μm 2 to about 2 x 2 μm 2 . The feasibility of using a liquid metal ion source has been examined with a view to achieving more substantial increases in brightness. While such sources have brightness approximately 10 5 times greater than conventional gaseous sources the highly divergent nature of the beam presents problems for the beam transport system. The use of a liquid metal source on the accelerator has been successfully demonstrated but it indicates the need for a special low aberration injection lens if brightness is to be maintained

  3. Chemical history with a nuclear microprobe

    Maggiore, C.J.; Benjamin, T.M.; Burnett, D.S.; Hyde, P.J.; Rogers, P.S.Z.; Srinivasan, S.; Tesmer, T.; Woolum, D.S.

    1983-01-01

    A nuclear microprobe cannot give direct information on the chemical state of an element, but the spatial distribution of elements in a specimen is often determined by the chemical history of the sample. Fuel cells and minerals are examples of complex systems whose elemental distributions are determined by past chemical history. The distribution of catalyst in used fuel cell electrodes provides direct information on the chemical stability of dispersed catalysts under operating conditions. The authors have used spatially resolved Rutherford backscattering to measure the migration of platinum and vanadium from intermetallic catalysts and to determine their suitability for use under the extreme operating conditions found in phosphoric acid fuel cells. Geologic materials are complex, heterogeneous samples with small mineral grains. The trace element distribution within the individual mineral grains and between different mineral phases is sensitive to the details of the mineral formation and history. The spatial resolution and sub-100-ppm sensitivity available with a nuclear microprobe open up several new classes of experiments to the geochemist. Geochemistry and electrochemistry are two areas proving particularly fruitful for application of the nuclear microprobe

  4. Analysis of mass spectrometry data in proteomics

    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....

  5. The new Schonland PIXE microprobe and applications to geological and archaeological samples

    Przybylowicz, W J; Watterson, J I.W.; Annegarn, H J; Connell, S H; Fearick, R W; Andeweg, A H; Sellschop, J P.F. [Schonland Research Centre for Nuclear Sciences, Univ. of the Witwatersrand, Johannesburg (South Africa)

    1993-04-01

    The new positive ion microprobe at the Schonland Centre is described and details are given of its configuration, its imaging system and software. In a unique configuration, the microprobe has access to two accelerators, a 6 MV EN tandem and a 2.5 MV single-ended machine. The imaging system uses a CAMAC based system and runs on a personal computer under OS/2. The implementation of PIXE and treatment of thick-target data are presented. Applications discussed are analysis of tin artifacts from the prehistory of metallurgy in South Africa; a diamond-containing rock; carbonado, gold contained in pyrite and cogenetic minerals included in diamond. (orig.).

  6. The new Schonland PIXE microprobe and applications to geological and archaeological samples

    Przybylowicz, W.J.; Watterson, J.I.W.; Annegarn, H.J.; Connell, S.H.; Fearick, R.W.; Andeweg, A.H.; Sellschop, J.P.F.

    1993-01-01

    The new positive ion microprobe at the Schonland Centre is described and details are given of its configuration, its imaging system and software. In a unique configuration, the microprobe has access to two accelerators, a 6 MV EN tandem and a 2.5 MV single-ended machine. The imaging system uses a CAMAC based system and runs on a personal computer under OS/2. The implementation of PIXE and treatment of thick-target data are presented. Applications discussed are analysis of tin artifacts from the prehistory of metallurgy in South Africa; a diamond-containing rock; carbonado, gold contained in pyrite and cogenetic minerals included in diamond. (orig.)

  7. Stained glasses under the nuclear microprobe: A window into history

    Vilarigues, M. [Dep. de Conservacao e Restauro and R and D Unit Vidro e da Ceramica Para as Artes, FCT-UNL, Quinta da Torre, 2829-516 Caparica (Portugal)], E-mail: mgv@fct.unl.pt; Fernandes, P. [Dep. de Conservacao e Restauro and R and D Unit Vidro e da Ceramica Para as Artes, FCT-UNL, Quinta da Torre, 2829-516 Caparica (Portugal); Alves, L.C.; Silva, R.C. da [Dep. Fisica, LFI, ITN, E.N.10, 2686-953 Sacavem (Portugal)

    2009-06-15

    Stained glass fragments from the 15th, 16th and 20th centuries, belonging to Mosteiro de Santa Maria da Vitoria, Batalha (Portugal), were characterised non-destructively in a nuclear microprobe. The work aimed at finding the composition of the glasses and glass paintings and relating these with the corresponding production periods. The elemental compositions of the glass fragments were obtained by means of scanning micro-beam Particle Induced X-ray Emission ({mu}-PIXE) spectrometry in selected cross-sections. These were complemented by micro X-Ray fluorescence spectrometry. Characterisation of colour was performed by optical absorption spectroscopy in the UV-vis range, while the corrosion products were identified by optical microscopy and {mu}-FTIR (Fourier Transform Infra Red) spectroscopy in combination with the data generated by {mu}-PIXE. Nuclear microprobe analysis allowed unveiling the compositions and structures, in particular of glass paintings and corrosion products. While it is not surprising that Fe, Cu and Pb were the main elements identified in the grisaille paintings of all studied periods, as well as Ag and Cu found in the glasses decorated with yellow silver painting, their distribution gave important clues on the materials and techniques used to manufacture these stained glasses. Furthermore, it allowed establishing a definite relation between the compositions found and the periods of production, with the added bonus of correctly reassigning the manufacturing period of some samples.

  8. In vivo analysis of tissue by Raman microprobe: examination of human skin lesions and esophagus Barrett's mucosa on an animal model

    Tfayli, Ali; Piot, Olivier; Derancourt, Sylvie; Cadiot, Guillaume; Diebold, Marie D.; Bernard, Philippe; Manfait, Michel

    2006-02-01

    In the last few years, Raman spectroscopy has been increasingly used for the characterization of normal and pathological tissues. A new Raman system, constituted of optic fibers bundle coupled to an axial Raman spectrometer (Horiba Jobin Yvon SAS), was developed for in vivo investigations. Here, we present in vivo analysis on two tissues: human skin and esophagus mucosa on a rat model. The skin is a directly accessible organ, representing a high diversity of lesions and cancers. Including malignant melanoma, basal cell carcinoma and the squamous cell carcinoma, skin cancer is the cancer with the highest incidence worldwide. Several Raman investigations were performed to discriminate and classify different types of skin lesions, on thin sections of biopsies. Here, we try to characterize in vivo the different types of skin cancers in order to be able to detect them in their early stages of development and to define precisely the exeresis limits. Barrett's mucosa was also studied by in vivo examination of rat's esophagus. Barrett's mucosa, induced by gastro-esophageal reflux, is a pretumoral state that has to be carefully monitored due to its high risk of evolution in adenocarcinoma. A better knowledge of the histological transformation of esophagus epithelium in a Barrett's type will lead to a more efficient detection of the pathology for its early diagnosis. To study these changes, an animal model (rats developing Barrett's mucosa after duodenum - esophagus anastomosis) was used. Potential of vibrational spectroscopy for Barrett's mucosa identification is assessed on this model.

  9. Microprobe to closely examine minerals

    2006-01-01

    The University of South Australia will develop synchrotron-based technology that can determine the structure and chemical composition of mineral samples at microscopic levels. The planned multi-analysis synchrotron X-ray facility Beam-line 11 is for implementing on the Australian Synchrotron. UniSA's Applied Centre for Structural and Synchrotron Studies (ACeSSS) will use Beamline 11 to shed new light on factors that constrain recoveries of copper and gold from typical copper ores. ACeSSS director Professor Andrea Gerson is working with an international team and the Australian Synchrotron on the design of Beamline 11. According to Gerson, there is scope to improve processing and/or increase recoveries in copper, gold and valueless pyrite either through separation, smelting, leaching or electro-processing. Using synchrotron technology, researchers will determine the structure and chemical composition of mineral samples to understand the fundamental behaviour of these materials in order to identify process and : environmental benefits. Three different strategies will be employed: tracing the movement of gold through the mineral processing chain to optimise and increase gold recovery; examining the surface layers formed when copper is leached from the mineral, chalcopyrite, to enhance the understanding of this surface layer formation and ultimately maximise cop-per recovery; and improving environmental remediation by understanding the mineralisation process during acid-rock drainage. ACeSSS will work with the minerals and environmental remediation sectors, building on the I establishment of the Cooperative Research Centre for Contamination Assessment and Remediation of the Environment, and cementing close collaboration with UniSA's Ian Wark Research Institute. Contributions from the SA Premier's Science and Research Fund, BHP Billiton and Rio Tinto, synchrotron partners Advanced Light Source (USA) and the Canadian Light Source Funding totalling $1.38m are available for

  10. Microprobe investigation of brittle segregates in aluminum MIG and TIG welds

    Larssen, P. A.; Miller, E. L.

    1968-01-01

    Quantitative microprobe analysis of segregated particles in aluminum MIG /Metal Inert Gas/ and TIG /Tungsten Inert Gas/ welds indicated that there were about ten different kinds of particles, corresponding to ten different intermetallic compounds. Differences between MIG and TIG welds related to the individual cooling rates of these welds.

  11. Evaluation of an x-ray microprobe technique as a possible aid to detect salmonellae

    Richter, E.R.; Banwart, G.J.

    1982-01-01

    Specific bacterial antigen (Salmonella) increased in phosphorus and sqlfur after reaction with the flukrescain isothiocyanate-tagged anti-Salmonella antibody, while nonspecific antigen (Escherichia coli) did not. X-ray microprobe analysis may be useful in detecting salmonellae or other bacteria by determining increases in the elemental constituents of bacterial cells when reacted with elemental-tagged antibodies

  12. Elemental microanalysis of biological and medical specimens with a scanning proton microprobe

    Legge, G.J.F.; Mazzolini, A.P.

    1979-01-01

    The scanning proton microprobe is shown to be a sensitive instrument for elemental microanalysis of cells and tissues in biological and medical specimens. The preparation of specimens and their behaviour under irradiation are crucial and the application of quantitative scanning analysis to the monitoring of such problems is illustrated

  13. Mass spectrometric analysis of protein interactions

    Borch, Jonas; Jørgensen, Thomas J. D.; Roepstorff, Peter

    2005-01-01

    Mass spectrometry is a powerful tool for identification of interaction partners and structural characterization of protein interactions because of its high sensitivity, mass accuracy and tolerance towards sample heterogeneity. Several tools that allow studies of protein interaction are now...... available and recent developments that increase the confidence of studies of protein interaction by mass spectrometry include quantification of affinity-purified proteins by stable isotope labeling and reagents for surface topology studies that can be identified by mass-contributing reporters (e.g. isotope...... labels, cleavable cross-linkers or fragment ions. The use of mass spectrometers to study protein interactions using deuterium exchange and for analysis of intact protein complexes recently has progressed considerably....

  14. Online open neuroimaging mass meta-analysis

    Nielsen, Finn Årup; Kempton, Matthew J.; Williams, Steven C. R.

    We describe a system for meta-analysis where a wiki stores numerical data in a simple format and a web service performs the numerical computation. We initially apply the system on multiple meta-analyses of structural neuroimaging data results. The described system allows for mass meta-analysis, e...

  15. Phylogenetic Analysis Using Protein Mass Spectrometry.

    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.

  16. Highly multiparametric analysis by mass cytometry.

    Ornatsky, Olga; Bandura, Dmitry; Baranov, Vladimir; Nitz, Mark; Winnik, Mitchell A; Tanner, Scott

    2010-09-30

    This review paper describes a new technology, mass cytometry, that addresses applications typically run by flow cytometer analyzers, but extends the capability to highly multiparametric analysis. The detection technology is based on atomic mass spectrometry. It offers quantitation, specificity and dynamic range of mass spectrometry in a format that is familiar to flow cytometry practitioners. The mass cytometer does not require compensation, allowing the application of statistical techniques; this has been impossible given the constraints of fluorescence noise with traditional cytometry instruments. Instead of "colors" the mass cytometer "reads" the stable isotope tags attached to antibodies using metal-chelating labeling reagents. Because there are many available stable isotopes, and the mass spectrometer provides exquisite resolution between detection channels, many parameters can be measured as easily as one. For example, in a single tube the technique allows for the ready detection and characterization of the major cell subsets in blood or bone marrow. Here we describe mass cytometric immunophenotyping of human leukemia cell lines and leukemia patient samples, differential cell analysis of normal peripheral and umbilical cord blood; intracellular protein identification and metal-encoded bead arrays. Copyright © 2010 Elsevier B.V. All rights reserved.

  17. Trace amount analysis using spark mass spectrometry

    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

  18. Nuclear analysis techniques and environmental sciences

    1997-10-01

    31 theses are collected in this book. It introduced molecular activation analysis micro-PIXE and micro-probe analysis, x-ray fluorescence analysis and accelerator mass spectrometry. The applications about these nuclear analysis techniques are presented and reviewed for environmental sciences

  19. Mass meta-analysis in Talairach space

    Nielsen, Finn Årup

    2004-01-01

    We provide a method for mass meta-analysis in a neuroinformatics database containing stereotaxic Talairach coordinates from neuroimaging experiments. Database labels are used to group the individual experiments, e.g., according to cognitive function, and the consistent pattern of the experiments...... of experiments, and the distances to the null hypotheses are used to sort the voxels across groups of experiments. This allows for mass meta-analysis, with the construction of a list with the most prominent associations between brain areas and group labels. Furthermore, the method can be used for functional...

  20. D OE top quark mass analysis

    Strovink, M.

    1995-07-01

    Based on (44-48 pb -1 ) of lepton + jets data, we review D0's initial analysis of the top quark mass. The result, M top = 199 ± 19/21 (stat.) ± 22 (syst.) GeV/c 2 , is insensitive to background normalization. The errors are based on ISAJET top Monte Carlo, with its more severe gluon radiation, and allow for ISAJET/HERWIG differences. Good progress is being made in reducing the systematic error. We present a new study based on two-dimensional distributions of reconstructed top quark vs. dijet mass. With 98.7% confidence we observe a peak in the top mass - dijet mass plane. The peak and its projections are similar both in shape and magnitude to expectations based on the decay sequence 1 → bW, W → jj

  1. Mass Spectrometric Analysis for Nuclear Safeguards

    Boulyga, S.

    2013-01-01

    The release of man-made radionuclides into the environment results in contamination that carries specific isotopic signatures according to the release scenarios and the previous usage of materials and facilities. In order to trace the origin of such contamination and/or to assess the potential impact on the public and environmental health, it is necessary to determine the isotopic composition and activity concentrations of radionuclides in environmental samples in an accurate and timely fashion. Mass spectrometric techniques, such as thermal ionization mass spectrometry (TIMS), secondary ion mass spectrometry (SIMS), and inductively coupled plasma mass spectrometry (ICP-MS) belong to the most powerful methods for analysis of nuclear and related samples in nuclear safeguards, forensics, and environmental monitoring. This presentation will address the potential of mass spectrometric analysis of actinides at ultra-trace concentration levels, isotopic analysis of micro-samples, age determination of nuclear materials as well as identification and quantification of elemental and isotopic signatures of nuclear samples in general. (author)

  2. A new scanning proton microprobe with long focus

    Zhu Jieqing; Li Minqian; Mao Yu; Chen Hanmin; Gu Yingmei; Yang Changyi; Sheng Kanglong

    1991-01-01

    A new scanning proton microprobe equipped with a long focus Russian magnetic quadruplet is set up. With excellent performances of ion optics, it can be used to do experiments of PIXE, RBS, RFS, NRA and channelling simultaneously within a micron-region. The power supplies for quadruplet and scanning coils are controlled by an IBM-PC computer and a scanning graphical monitor based on an Apple IIe microcomputer provides convenience of searching for an interesting area to scan. The advanced modes of the fast random scan and the event-by-event data collection make it possible to treat the multi-parameter and multi-detector data by means of the strategy of TQSA (Total quantitative scanning analysis). There are three types of graphical display including the innovation of three dimensional contour mapping

  3. Nuclear microprobe imaging of gallium nitrate in cancer cells

    Ortega, Richard; Suda, Asami; Devès, Guillaume

    2003-09-01

    Gallium nitrate is used in clinical oncology as treatment for hypercalcemia and for cancer that has spread to the bone. Its mechanism of antitumor action has not been fully elucidated yet. The knowledge of the intracellular distribution of anticancer drugs is of particular interest in oncology to better understand their cellular pharmacology. In addition, most metal-based anticancer compounds interact with endogenous trace elements in cells, altering their metabolism. The purpose of this experiment was to examine, by use of nuclear microprobe analysis, the cellular distribution of gallium and endogenous trace elements within cancer cells exposed to gallium nitrate. In a majority of cellular analyses, gallium was found homogeneously distributed in cells following the distribution of carbon. In a smaller number of cells, however, gallium appeared concentrated together with P, Ca and Fe within round structures of about 2-5 μm diameter located in the perinuclear region. These intracellular structures are typical of lysosomial material.

  4. Nuclear microprobe imaging of gallium nitrate in cancer cells

    Ortega, Richard; Suda, Asami; Deves, Guillaume

    2003-01-01

    Gallium nitrate is used in clinical oncology as treatment for hypercalcemia and for cancer that has spread to the bone. Its mechanism of antitumor action has not been fully elucidated yet. The knowledge of the intracellular distribution of anticancer drugs is of particular interest in oncology to better understand their cellular pharmacology. In addition, most metal-based anticancer compounds interact with endogenous trace elements in cells, altering their metabolism. The purpose of this experiment was to examine, by use of nuclear microprobe analysis, the cellular distribution of gallium and endogenous trace elements within cancer cells exposed to gallium nitrate. In a majority of cellular analyses, gallium was found homogeneously distributed in cells following the distribution of carbon. In a smaller number of cells, however, gallium appeared concentrated together with P, Ca and Fe within round structures of about 2-5 μm diameter located in the perinuclear region. These intracellular structures are typical of lysosomial material

  5. Principles of isotopic analysis by mass spectrometry

    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)

  6. Proton microprobe study of tin-polymetallic deposits

    Murao, S. [Geological Survey of Japan, Tsukuba, Ibaraki (Japan); Sie, S.H.; Suter, G.F. [Commonwealth Scientific and Industrial Research Organisation (CSIRO), North Ryde, NSW (Australia). Div. of Exploration Geoscience

    1996-12-31

    Tin-polymetallic vein type deposits are a complex mixture of cassiterite and sulfides and they are the main source of technologically important rare metals such as indium and bismuth. Constituent minerals are usually fine grained having wide range of chemical composition and often the elements of interest occur as trace elements not amenable to electron microprobe analysis. PIXE with a proton microprobe can be an effective tool to study such deposits by delineating the distribution of trace elements among carrier minerals. Two representative indium-bearing deposits of tin- polymetallic type, Tosham of India (Cu-ln-Bi-Sn-W-Ag), and Mount Pleasant of Canada (Zn-Cu-In-Bi-Sn-W), were studied to delineate the distribution of medical/high-tech rare metals and to examine the effectiveness of the proton probe analysis of such ore. One of the results of the study indicated that indium and bismuth are present in chalcopyrite in the deposits. In addition to these important rare metals, zinc, copper, arsenic, antimony, selenium, and tin are common in chalcopyrite and pyrite. Arsenopyrite contains nickel, copper, zinc, silver, tin, antimony and bismuth. In chalcopyrite and pyrite, zinc, arsenic, indium, bismuth and lead are richer in Mount Pleasant ore, but silver is higher at Tosham. Also thallium and gold were found only in Tosham pyrite. The Tosham deposit is related to S-type granite, while Mount Pleasant to A-type. It appears that petrographic character of the source magma is one of the factors to determine the trace element distribution in tin-polymetallic deposit. 6 refs., 2 figs.

  7. Proton microprobe study of tin-polymetallic deposits

    Murao, S [Geological Survey of Japan, Tsukuba, Ibaraki (Japan); Sie, S H; Suter, G F [Commonwealth Scientific and Industrial Research Organisation (CSIRO), North Ryde, NSW (Australia). Div. of Exploration Geoscience

    1997-12-31

    Tin-polymetallic vein type deposits are a complex mixture of cassiterite and sulfides and they are the main source of technologically important rare metals such as indium and bismuth. Constituent minerals are usually fine grained having wide range of chemical composition and often the elements of interest occur as trace elements not amenable to electron microprobe analysis. PIXE with a proton microprobe can be an effective tool to study such deposits by delineating the distribution of trace elements among carrier minerals. Two representative indium-bearing deposits of tin- polymetallic type, Tosham of India (Cu-ln-Bi-Sn-W-Ag), and Mount Pleasant of Canada (Zn-Cu-In-Bi-Sn-W), were studied to delineate the distribution of medical/high-tech rare metals and to examine the effectiveness of the proton probe analysis of such ore. One of the results of the study indicated that indium and bismuth are present in chalcopyrite in the deposits. In addition to these important rare metals, zinc, copper, arsenic, antimony, selenium, and tin are common in chalcopyrite and pyrite. Arsenopyrite contains nickel, copper, zinc, silver, tin, antimony and bismuth. In chalcopyrite and pyrite, zinc, arsenic, indium, bismuth and lead are richer in Mount Pleasant ore, but silver is higher at Tosham. Also thallium and gold were found only in Tosham pyrite. The Tosham deposit is related to S-type granite, while Mount Pleasant to A-type. It appears that petrographic character of the source magma is one of the factors to determine the trace element distribution in tin-polymetallic deposit. 6 refs., 2 figs.

  8. Proton microprobe study of tin-polymetallic deposits

    Murao, S.; Sie, S.H.; Suter, G.F.

    1996-01-01

    Tin-polymetallic vein type deposits are a complex mixture of cassiterite and sulfides and they are the main source of technologically important rare metals such as indium and bismuth. Constituent minerals are usually fine grained having wide range of chemical composition and often the elements of interest occur as trace elements not amenable to electron microprobe analysis. PIXE with a proton microprobe can be an effective tool to study such deposits by delineating the distribution of trace elements among carrier minerals. Two representative indium-bearing deposits of tin- polymetallic type, Tosham of India (Cu-ln-Bi-Sn-W-Ag), and Mount Pleasant of Canada (Zn-Cu-In-Bi-Sn-W), were studied to delineate the distribution of medical/high-tech rare metals and to examine the effectiveness of the proton probe analysis of such ore. One of the results of the study indicated that indium and bismuth are present in chalcopyrite in the deposits. In addition to these important rare metals, zinc, copper, arsenic, antimony, selenium, and tin are common in chalcopyrite and pyrite. Arsenopyrite contains nickel, copper, zinc, silver, tin, antimony and bismuth. In chalcopyrite and pyrite, zinc, arsenic, indium, bismuth and lead are richer in Mount Pleasant ore, but silver is higher at Tosham. Also thallium and gold were found only in Tosham pyrite. The Tosham deposit is related to S-type granite, while Mount Pleasant to A-type. It appears that petrographic character of the source magma is one of the factors to determine the trace element distribution in tin-polymetallic deposit. 6 refs., 2 figs

  9. Combination of synchrotron radiation X-ray microprobe and nuclear microprobe for chromium and chromium oxidation states quantitative mapping in single cells

    Ortega, Richard; Deves, Guillaume; Fayard, Barbara; Salome, Murielle; Susini, Jean

    2003-01-01

    Hexavalent chromium compounds are established carcinogens but their mechanism of cell transformation has not been elucidated yet. In this study, chromium oxidation state distribution maps in cells exposed to soluble (Na 2 CrO 4 ), or insoluble (PbCrO 4 ), Cr(VI) compounds have been obtained by use of the ESRF ID-21 X-ray microscope. In addition, the quantitative maps of element distributions in cells have been determined using the nuclear microprobe of Bordeaux-Gradignan. Nuclear microprobe quantitative analysis revealed interesting features on chromium, and lead, cellular uptake. It is suggested that cells can enhance PbCrO 4 solubility, resulting in chromium, but not lead uptake. The differential carcinogenic potential of soluble and insoluble Cr(VI) compounds is discussed with regard to chromium intracellular quantitative distribution

  10. The new scanning nuclear microprobe in Uppsala

    Sunde, T.; Nystroem, J.; Lindh, U.

    1991-01-01

    During 1989/90 a scanning microprobe, developed for 2-4 MeV protons and submicron resolution, is being installed at the EN-tandem accelerator at the The Svedberg Laboratory, Uppsala University, Sweden. The probe-forming units (object diaphragm, aperture diaphragm and triplet of spark-eroded quadrupoles), the scanning unit of current-controlled ferrite cores and a current digitizer are of Oxford design. The other parts are commercial products or are constructed by ourselves. The latter includes the equipment for optical alignment by interference, a feedback-controlled magnetic beam steerer and stabiliser, a fast beam deflector, specially designed mechanical vibration reducers and dedicated AT expansion cards for scanning control and data acquisition. (orig.)

  11. [Imaging Mass Spectrometry in Histopathologic Analysis].

    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.

  12. Mass Spectrometric Analysis of Synthetic Organic Pigments.

    Sugaya, Naeko; Takahashi, Mitsuko; Sakurai, Katsumi; Tanaka, Nobuko; Okubo, Ichiro; Kawakami, Tsuyoshi

    2018-04-18

    Though synthetic organic colorants are used in various applications nowadays, there is the concern that impurities by-produced during the manufacturing and degradation products in some of these colorants are persistent organic pollutants and carcinogens. Thus, it is important to identify the synthetic organic colorants in various products, such as commercial paints, ink, cosmetics, food, textile, and plastics. Dyes, which are soluble in water and other solvents, could be analyzed by chromatographic methods. In contrast, it is difficult to analyze synthetic organic pigments by these methods because of their insolubility. This review is an overview of mass spectrometric analysis of synthetic organic pigments by various ionization methods. We highlight a recent study of textile samples by atmospheric pressure solid analysis probe MS. Furthermore, the mass spectral features of synthetic organic pigments and their separation from other components such as paint media and plasticizers are discussed.

  13. Applications of nuclear microprobes in the semiconductor industry

    Takai, M.

    1996-01-01

    Possible nuclear microprobe applications in semiconductor industries are discussed. A unique technique using soft-error mapping and ion beam induced current measurements for reliability testing of dynamic random access memories such as soft-error immunity and noise carrier suppression has been developed for obtaining design parameters of future memory devices. Nano-probes and small installation areas are required for the use of microprobes in the semiconductor industry. Issues arising from microprobe applications such as damage induced by the probe beam are clarified. (orig.)

  14. Total quantitative recording of elemental maps and spectra with a scanning microprobe

    Legge, G.J.F.; Hammond, I.

    1979-01-01

    A system of data recording and analysis has been developed by means of which simultaneously all data from a scanning instrument such as a microprobe can be quantitatively recorded and permanently stored, including spectral outputs from several detectors. Only one scanning operation is required on the specimen. Analysis is then performed on the stored data, which contain quantitative information on distributions of all elements and spectra of all regions

  15. Hydrogen isotope analysis by quadrupole mass spectrometry

    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

  16. Mass and emission spectrometry in the Analytical Chemistry Division of Oak Ridge National Laboratory

    Smith, D.H. (ed.)

    1978-11-01

    The capabilities of the Mass and Emission Spectrometry Section of the Analytical Chemistry Division of Oak Ridge National Laboratory are described. Many different areas of mass spectrometric expertise are represented in the section: gas analysis, high abundance sensitivity measurements, high- and low-resolution organic analyses, spark source trace constituent analysis, and ion microprobe analysis of surfaces. These capabilities are complemented by emission spectrometry. The instruments are described along with a few applications, some of which are unique.

  17. Mass and emission spectrometry in the Analytical Chemistry Division of Oak Ridge National Laboratory

    Smith, D.H.

    1978-11-01

    The capabilities of the Mass and Emission Spectrometry Section of the Analytical Chemistry Division of Oak Ridge National Laboratory are described. Many different areas of mass spectrometric expertise are represented in the section: gas analysis, high abundance sensitivity measurements, high- and low-resolution organic analyses, spark source trace constituent analysis, and ion microprobe analysis of surfaces. These capabilities are complemented by emission spectrometry. The instruments are described along with a few applications, some of which are unique

  18. Determination of trace element mineral/liquid partition coefficients in melilite and diopside by ion and electron microprobe techniques

    Kuehner, S. M.; Laughlin, J. R.; Grossman, L.; Johnson, M. L.; Burnett, D. S.

    1989-01-01

    The applicability of ion microprobe (IMP) for quantitative analysis of minor elements (Sr, Y, Zr, La, Sm, and Yb) in the major phases present in natural Ca-, Al-rich inclusions (CAIs) was investigated by comparing IMP results with those of an electron microprobe (EMP). Results on three trace-element-doped glasses indicated that it is not possible to obtain precise quantitative analysis by using IMP if there are large differences in SiO2 content between the standards used to derive the ion yields and the unknowns.

  19. Elemental microanalysis of botanical specimens using the Melbourne Proton Microprobe

    Mazzolini, A.P.J.; Legge, G.J.F.

    1978-01-01

    A proton microprobe has been used to obtain the distribution of elements of various botanical specimens. This paper presents preliminary results obtained by the irradiation of certain organs of the wheat plant

  20. Optimization of the electrostatic structure of the ion microprobe

    I. G. Ignat'ev

    2012-03-01

    Full Text Available The paper presents optimization data obtained for an immersion probe-forming system of the ion microprobe to be used in 3 MeV H+ ion accelerator generating 0,4 μm beam spot for normalized acceptance of 7 μm2 · mrad2 · MeV. To achieve higher microprobe resolution it is intended to place an electrostatic lens between the collimators and the accelerating tube.

  1. Subgroup report on hard x-ray microprobes

    Ice, G.E.; Barbee, T.; Bionta, R.; Howells, M.; Thompson, A.C.; Yun, W.

    1994-01-01

    The increasing availability of synchrotron x-ray sources has stimulated the development of advanced hard x-ray (E≥5 keV) microprobes. New x-ray optics have been demonstrated which show promise for achieving intense submicron hard x-ray probes. These probes will be used for extraordinary elemental detection by x-ray fluorescence/absorption and for microdiffraction to identify phase and strain. The inherent elemental and crystallographic sensitivity of an x-ray microprobe and its inherently nondestructive and penetrating nature makes the development of an advanced hard x-ray microprobe an important national goal. In this workshop state-of-the-art hard x-ray microprobe optics were described and future directions were discussed. Gene Ice, Oak Ridge National Laboratory (ORNL), presented an overview of the current status of hard x-ray microprobe optics and described the use of crystal spectrometers to improve minimum detectable limits in fluorescent microprobe experiments. Al Thompson, Lawrence Berkeley Laboratory (LBL), described work at the Center for X-ray Optics to develop a hard x-ray microprobe based on Kirkpatrick-Baez (KB) optics. Al Thompson also showed the results of some experimental measurements with their KB optics. Malcolm Howells presented a method for bending elliptical mirrors and Troy Barbee commented on the use of graded d spacings to achieve highest efficiency in KB multilayer microfocusing. Richard Bionta, Lawrence Livermore National Laboratory (LLNL), described the development of the first hard x-ray zone plates and future promise of so called open-quotes jelly rollclose quotes or sputter slice zone plates. Wenbing Yun, Argonne National Laboratory (ANL), described characterization of jelly roll and lithographically produced zone plates and described the application of zone plates to focus extremely narrow bandwidths by nuclear resonance. This report summarizes the presentations of the workshop subgroup on hard x-ray microprobes

  2. The new nuclear microprobe at Livermore

    Roberts, M.L.; Bench, G.S.; Heikkinen, D.W.; Morse, D.H.; Bach, P.R.; Pontau, A.E.

    1994-10-01

    Lawrence Livermore National Laboratory (LLNL) and Sandia National Laboratories/California have jointly constructed a new nuclear microprobe beamline. This beamline is located on the LLNL 10 MV tandem accelerator and can be used for multidisciplinary research using PIXE, PIGE, energy loss tomography, or IBS techniques. Distinctive features of the beamline include incorporation of magnet power supplies into the accelerator control system, computer controlled object and image slits, automated target positioning to sub-micron resolution, and video optics for beam positioning and observation. Mitigation of vibrations was accomplished with vibration isolators and a rigid beamline design while integral beamline shielding was used to shield from stray magnetic fields. Available detectors include a wavelength dispersive X-ray spectrometer, a High-Purity Germanium detector (HPGe), a Lithium-Drifted Silicon X-Ray detector (SiLi), and solid state surface barrier detectors. Along with beamline performance, results from recent measurements on determination of trace impurities in an International Thermonuclear Experimental Reactor (ITER) super conducting wire strand, determination of Ca/Sr ratios in seashells, and determination of minor and trace element concentrations in sperm cells are presented

  3. The INS nuclear microprobe and its application

    Coote, G.E.

    1986-01-01

    The nuclear microprobe directs a well-focused beam of high-energy protons or deuterons at a solid specimen inside a vacuum chamber. Atomic and nuclear reactions are induced in those elements in a layer about 20 micro m thick, leading to the emission of characteristic x-rays, gamma rays, and charged particles as well as Rutherford scattering of the incident beam. These radiations impinge on several detectors near the specimen (NaI, Ge(Li), Si(Li) and Si surface barrier). Using proton-excited x-rays all elements above Na may be detected with sensitivities 10 or 100 times that of the electron probe, while elements which can be estimated from their gamma rays include C, N, O, F, Na and Al. In most of our projects the distribution of a trace or minor element (e.g. F, N) is compared to that of a major element (e.g. Ca or Fe). Recent areas of application include archaeometry (diffusion profiles of F in bones and teeth; depth profiles of sodium in obsidian), geology (F concentrations in mineral grains; studies of the Cretaceous-Tertiary boundary), metallurgy (C, O, N in steel and in welds; S, O, C in corrosion layers), fisheries management (Zn, Sr in otoliths; F in dogfish fin spines and vertebrae), biology (Fe, Sr, N in egg shells; trace elements in human hair), and dental research

  4. Deep Space 2: The Mars Microprobe Mission

    Smrekar, Suzanne; Catling, David; Lorenz, Ralph; Magalhães, Julio; Moersch, Jeffrey; Morgan, Paul; Murray, Bruce; Presley-Holloway, Marsha; Yen, Albert; Zent, Aaron; Blaney, Diana

    The Mars Microprobe Mission will be the second of the New Millennium Program's technology development missions to planetary bodies. The mission consists of two penetrators that weigh 2.4 kg each and are being carried as a piggyback payload on the Mars Polar Lander cruise ring. The spacecraft arrive at Mars on December 3, 1999. The two identical penetrators will impact the surface at ~190 m/s and penetrate up to 0.6 m. They will land within 1 to 10 km of each other and ~50 km from the Polar Lander on the south polar layered terrain. The primary objective of the mission is to demonstrate technologies that will enable future science missions and, in particular, network science missions. A secondary goal is to acquire science data. A subsurface evolved water experiment and a thermal conductivity experiment will estimate the water content and thermal properties of the regolith. The atmospheric density, pressure, and temperature will be derived using descent deceleration data. Impact accelerometer data will be used to determine the depth of penetration, the hardness of the regolith, and the presence or absence of 10 cm scale layers.

  5. Study of ion tracks by micro-probe ion energy loss spectroscopy

    Vacík, Jiří; Havránek, Vladimír; Hnatowicz, Vladimír; Horák, Pavel; Fink, Dietmar; Apel, P. Yu.

    2014-01-01

    Roč. 332, AUG (2014), s. 308-311 ISSN 0168-583X. [21st International Conference on Ion Beam Analysis (IBA). Seattle, 23.06.2013-28.06.2013] R&D Projects: GA ČR(CZ) GBP108/12/G108; GA MŠk(XE) LM2011019 Institutional support: RVO:61389005 Keywords : ion energy loss spectrometry * single ion track * microprobe * tomography Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.124, year: 2014

  6. Calcium Isotope Analysis by Mass Spectrometry

    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. Quantitative elemental imaging of octopus stylets using PIXE and the nuclear microprobe

    Doubleday, Zoe [Marine Research Laboratories, Tasmanian Aquaculture and Fisheries Institute, University of Tasmania, Private Bag 49, Tasmania 7001 (Australia)], E-mail: zoeanned@utas.edu.au; Belton, David [CSIRO Exploration and Mining, University of Melbourne (School of Physics), Melbourne 3010 (Australia); Pecl, Gretta; Semmens, Jayson [Marine Research Laboratories, Tasmanian Aquaculture and Fisheries Institute, University of Tasmania, Private Bag 49, Tasmania 7001 (Australia)

    2008-01-15

    By utilising targeted microprobe technology, the analysis of elements incorporated within the hard bio-mineralised structures of marine organisms has provided unique insights into the population biology of many species. As hard structures grow, elements from surrounding waters are incorporated effectively providing a natural 'tag' that is often unique to the animal's particular location or habitat. The spatial distribution of elements within octopus stylets was investigated, using the nuclear microprobe, to assess their potential for determining dispersal and population structure in octopus populations. Proton Induced X-ray Emission (PIXE) was conducted using the Dynamic Analysis method and GeoPIXE software package, which produced high resolution, quantitative elemental maps of whole stylet cross-sections. Ten elements were detected within the stylets which were heterogeneously distributed throughout the microstructure. Although Ca decreased towards the section edge, this trend was consistent between individuals and remained homogeneous in the inner region of the stylet, and thus appears a suitable internal standard for future microprobe analyses. Additional analyses used to investigate the general composition of the stylet structure suggested that they are amorphous and largely organic, however, there was some evidence of phosphatic mineralisation. In conclusion, this study indicates that stylets are suitable for targeted elemental analysis, although this is currently limited to the inner hatch region of the microstructure.

  8. Quantitative elemental imaging of octopus stylets using PIXE and the nuclear microprobe

    Doubleday, Zoe; Belton, David; Pecl, Gretta; Semmens, Jayson

    2008-01-01

    By utilising targeted microprobe technology, the analysis of elements incorporated within the hard bio-mineralised structures of marine organisms has provided unique insights into the population biology of many species. As hard structures grow, elements from surrounding waters are incorporated effectively providing a natural 'tag' that is often unique to the animal's particular location or habitat. The spatial distribution of elements within octopus stylets was investigated, using the nuclear microprobe, to assess their potential for determining dispersal and population structure in octopus populations. Proton Induced X-ray Emission (PIXE) was conducted using the Dynamic Analysis method and GeoPIXE software package, which produced high resolution, quantitative elemental maps of whole stylet cross-sections. Ten elements were detected within the stylets which were heterogeneously distributed throughout the microstructure. Although Ca decreased towards the section edge, this trend was consistent between individuals and remained homogeneous in the inner region of the stylet, and thus appears a suitable internal standard for future microprobe analyses. Additional analyses used to investigate the general composition of the stylet structure suggested that they are amorphous and largely organic, however, there was some evidence of phosphatic mineralisation. In conclusion, this study indicates that stylets are suitable for targeted elemental analysis, although this is currently limited to the inner hatch region of the microstructure

  9. Microprobe measurements to determine phase boundaries and diffusion paths in ternary phase diagrams taking a Cu-Ni-Al system as an example

    Rudolph, G.

    1983-01-01

    With the aid of quantitative microprobe tests, diffusion phenomena and phase formation in the ternary CuNiAl system at 600 - 900 0 C were investigated taking as an example the diffusion couple CuNi5Al5-nickel. The diffusion paths in the ternary system are dependent on temperature and assume an S-form in the copper corner of the phase diagram. In the copper corner, the curves swing away from the more rapid component aluminium towards the copper. Due to this non-linear course of the curves, the intermetallic theta-phase of the type (Ni,Cu) 3 Al can be observed as a layer at all temperatures in the boundary zone. At 800 0 C and to a lesser extend at 900 0 C the solubility of α-CuNi40 for aluminium, at around 5 mass-%, is higher than the value given by W.O. Alexander (1938). As far as it is possible with the diffusion couple under analysis, the microprobe measurements taken otherwise conform at 700 and 600 0 C the position of the phase boundary α-(Cu,Ni)/(α+theta)-miscibility gap indicated in W.O. Alexander (1938). (Author)

  10. Environmental applications of the LANL nuclear microprobe

    Hickmott, D.D.; Herrin, J.M.; Abell, R.; George, M.; Gauerke, E.R.; Denniston, R.F.

    1997-01-01

    The LANL nuclear microprobe has been used to study the distributions of trace elements (TE) of environmental interest including: (1) metals in coal and fly ash, (2) Pb in the Bandelier Tuff (BT), (3) Ba in tree rings, (4) Mn, Fe, Sr and Y in Yucca Mountain calcites. Micro-PIXE (MP) analyses with 5-10 micrometer spatial resolution provide constraints on processes that redistribute contaminants in the environment, and hence may help answer environmental problems where fine-scale chemical records are important. MP analyses of particulates in coal and ash show that pyrite contains As, Se, Hg and Pb; macerals contain Cr, halogens and S; cenospheres contain As, Se and Ni; and hematite ash contains Ni and As. Understanding these elemental modes of occurrence allows prediction of metal behavior in boilers and may enhance compliance with the Clean Air Act Amendments. Fine-grained high-Pb minerals were identified using SEM and MP analyses of BT minerals. These minerals were from samples associated with deep-groundwater wells containing Pb at levels greater than regulatory limits. Pb is concentrated in Pb minerals (e.g. cerussite), smectite, and hematite formed during low-T alteration of tuff. Understanding mineralogic speciation of metals may provide insights into sources of groundwater pollution. Tree rings from ponderosa pines that grew in a Ba-contaminated drainage were analyzed using MP. Ba concentrations are typically higher in rings that formed after operations discharging Ba to the environment began. Such tree-ring analyses may ultimately provide information on rates of contaminant migration in the environment. TE in zoned calcites from Yucca Mountain were analyzed by MP. Calcites from the saturated zone (SZ) have distinct chemical signatures (high Fe, Mn and low Y). No calcites in the unsaturated zone with SZ chemical signatures were found using MP

  11. Scanning transmission ion microscopy mass measurements for quantitative trace element analysis within biological samples and validation using atomic force microscopy thickness measurements

    Deves, Guillaume [Laboratoire de chimie nucleaire analytique et bioenvironnementale, UMR 5084, CNRS-Universite de Bordeaux 1, BP 120 Chemin du solarium, F33175 Gradignan cedex (France)]. E-mail: deves@cenbg.in2p3.fr; Cohen-Bouhacina, Touria [Centre de Physique Moleculaire Optique et Hertzienne, Universite de Bordeaux 1, 351, cours de la Liberation, F33405 Talence cedex (France); Ortega, Richard [Laboratoire de chimie nucleaire analytique et bioenvironnementale, UMR 5084, CNRS-Universite de Bordeaux 1, BP 120 Chemin du solarium, F33175 Gradignan cedex (France)

    2004-10-08

    We used the nuclear microprobe techniques, micro-PIXE (particle-induced X-ray emission), micro-RBS (Rutherford backscattering spectrometry) and scanning transmission ion microscopy (STIM) in order to perform the characterization of trace element content and spatial distribution within biological samples (dehydrated cultured cells, tissues). The normalization of PIXE results was usually expressed in terms of sample dry mass as determined by micro-RBS recorded simultaneously to micro-PIXE. However, the main limit of RBS mass measurement is the sample mass loss occurring during irradiation and which could be up to 30% of the initial sample mass. We present here a new methodology for PIXE normalization and quantitative analysis of trace element within biological samples based on dry mass measurement performed by mean of STIM. The validation of STIM cell mass measurements was obtained in comparison with AFM sample thickness measurements. Results indicated the reliability of STIM mass measurement performed on biological samples and suggested that STIM should be performed for PIXE normalization. Further information deriving from direct confrontation of AFM and STIM analysis could as well be obtained, like in situ measurements of cell specific gravity within cells compartment (nucleolus and cytoplasm)

  12. Mass composition analysis using elongation rate

    Ochilo, Livingstone; Risse, Markus; Yushkov, Alexey [University of Siegen, Siegen (Germany)

    2015-07-01

    The all-particle cosmic ray energy spectrum has been observed to flatten at around 5.2 x 10{sup 18} eV where the spectral index changes from γ = 3.2 to γ = 2.6, a feature called the ''ankle'' of the spectrum. Cosmic rays with energy around the ankle and beyond, known as ultra-high energy cosmic rays (UHECR), have a very low flux and reconstruction of their properties from extensive air shower measurements is subject to uncertainties for instance from hadronic interaction models. Since the year 2004, the Pierre Auger Observatory has recorded a considerable number of UHECR events beyond the ankle. With the greatly improved statistics, the mass composition of the extreme end of the cosmic ray energy spectrum is now being investigated with improved accuracy. The measured composition of UHECR is an important parameter in validating the models used to explain their sources and acceleration mechanisms. In this study, we perform a mass composition analysis using elongation rate (the rate of change of the depth of shower maximum with energy), measured by the fluorescence detector of the Pierre Auger Observatory. The advantage of this approach is a weak dependence of the results on the choice of the hadronic interaction models.

  13. Scaling analysis of meteorite shower mass distributions

    Oddershede, Lene; Meibom, A.; Bohr, Jakob

    1998-01-01

    Meteorite showers are the remains of extraterrestrial objects which are captivated by the gravitational field of the Earth. We have analyzed the mass distribution of fragments from 16 meteorite showers for scaling. The distributions exhibit distinct scaling behavior over several orders of magnetude......; the observed scaling exponents vary from shower to shower. Half of the analyzed showers show a single scaling region while the orther half show multiple scaling regimes. Such an analysis can provide knowledge about the fragmentation process and about the original meteoroid. We also suggest to compare...... the observed scaling exponents to exponents observed in laboratory experiments and discuss the possibility that one can derive insight into the original shapes of the meteoroids....

  14. Analysis of barium by isotope mass spectrometry

    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

  15. A photomultiplier-based secondary electron imaging system for a nuclear microprobe

    Alves, L.C.; Breese, M.B.H.; Silva, M.F. da; Soares, J.C.

    2002-01-01

    The ability to define, or recognise particular regions of interest or surface features is vital to the analysis and interpretation of spatially-resolved images collected with a nuclear microprobe. However, good topographic image contrast is difficult to accomplish using PIXE or RBS images due to their inherent insensitivity to topography, lack of elemental variation or poor statistics. Topographic image contrast is commonly obtained in scanning electron microscopy (SEM) by detecting a large flux of secondary electrons produced by the focused keV electron beam. Similar systems have not been widely used on nuclear microprobes due to ion beam intensity fluctuations, which limit the minimum resolvable contrast and present a major limitation for this technique. This paper describes a secondary electron imaging system which has been developed on the Lisbon microprobe. It is based on a scintillator, a photomultiplier operated in a pulsed mode, a pulse shaping electronic chain and ADC, and requires no changes to the existing data acquisition system. Examples of the images obtained from materials such as patterned SiGe wafers and hydrogen-implanted silicon are given, and compared with SEM or optical images

  16. Deep PIXE: finding diamonds with the proton microprobe

    Griffin, W.L.; Ryan, C.G.

    1991-01-01

    Since 1987 the CSIRO Div. of Exploration Geoscience has carried out a program of proton-microprobe (PIXE) analysis aimed at using trace-element data on indicator minerals to discriminate between those from diamondiferous and barren source rocks. The results have provided both important new tools for the exploration industry, and significant new information on the conditions and processes of diamond growth. Cr-pyrope garnet has been used as Ni thermometer while chromites, in partcular their Zn content, has allowed correlation of chromite composition with temperature. The two techniques described provide a significant increase in exploration efficiency, through early recognition and rejection of barren targets and concentration of resources on more promising targets. They also provide direct cost savings in evaluation of ore bodies once they are found. It is estimated that evaluation of a prospect by conventional bulk testing is expensive ($100-500K) and time-consuming; an evaluation by PIXE methods is done quickly for a tiny fraction of that cost. 1 refs., 4 figs

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

    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...

  18. Accelerator mass spectrometry at the Rossendorf 5 MV tandem accelerator

    Friedrich, M.; Buerger, W.; Curian, H.; Hartmann, B.; Hentschel, E.; Matthes, H.; Probst, W.; Seidel, M.; Turuc, S.; Hebert, D.; Rothe, T.; Stolz, W.

    1992-01-01

    The Rossendorf electrostatic accelerators (5 MV tandem accelerator and single ended 2 MV van de Graaff accelerator) are already used for ion beam analysis. The existing methods (RBS, PIXE, ERDA, NRA, nuclear microprobe and external beam) will be completed by introduction of Accelerator Mass Spectrometry (AMS). A short description of the Rossendorf AMS system is given and first experimental results are presented. (R.P.) 4 refs.; 6 figs

  19. The remote control of nuclear microprobes over the Internet

    Churms, C.L.; Prozesky, V.M.; Springhorn, K.A.

    1999-01-01

    Whereas the concept of remote control is not new, the required equipment and data link have typically been costly and specialized. With the growing availability of reliable Internet connection, it has however become possible and increasingly attractive to be able to control complex equipment remotely over the Internet. Some methods of Internet Remote control are discussed, bearing in mind the specific needs of nuclear microprobe control. One such system has been implemented at the NAC nuclear microprobe, and even though improvements are envisaged, it is already functioning satisfactorily

  20. Extraterrestrial materials examined by mean of nuclear microprobe

    Khodja, H.; Smith, T.; Engrand, C.; Herzog, G.; Raepsaet, C.

    2013-07-01

    Comet fragments, micrometeorites, and Interplanetary Dust Particles (IDPs) are small objects (purpose, we need instruments and methods that provide both microanalysis and detailed imaging. In these respects, the nuclear microprobe offers many potential advantages: (i) the spatial resolution, ∼1 μm is well-matched to the typical object dimensions, (ii) with some reservations, it is non-destructive when carefully conducted, (iii) it is quantitative, and especially sensitive for light elements. At the Saclay nuclear microprobe, we have been performing analyses of extraterrestrial objects for many years. We review some of these studies, emphasizing the specific requirements for successful analyses. We also discuss the potential pitfalls that may be encountered.

  1. Tandem mass spectrometry: analysis of complex mixtures

    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

  2. Surface analysis by imaging mass spectrometry

    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

  3. An SU-8-based microprobe with a nanostructured surface enhances neuronal cell attachment and growth

    Kim, Eunhee; Kim, Jin-Young; Choi, Hongsoo

    2017-12-01

    Microprobes are used to repair neuronal injury by recording electrical signals from neuronal cells around the surface of the device. Following implantation into the brain, the immune response results in formation of scar tissue around the microprobe. However, neurons must be in close proximity to the microprobe to enable signal recording. A common reason for failure of microprobes is impaired signal recording due to scar tissue, which is not related to the microprobe itself. Therefore, the device-cell interface must be improved to increase the number of neurons in contact with the surface. In this study, we developed nanostructured SU-8 microprobes to support neuronal growth. Nanostructures of 200 nm diameter and depth were applied to the surface of microprobes, and the attachment and neurite outgrowth of PC12 cells on the microprobes were evaluated. Neuronal attachment and neurite outgrowth on the nanostructured microprobes were significantly greater than those on non-nanostructured microprobes. The enhanced neuronal attachment and neurite outgrowth on the nanostructured microprobes occurred in the absence of an adhesive coating, such as poly- l-lysine, and so may be useful for implantable devices for long-term use. Therefore, nanostructured microprobes can be implanted without adhesive coating, which can cause problems in vivo over the long term.

  4. High resolution techniques using scanning proton microprobe (SPM)

    Cholewa, M.; Saint, A.; Prawer, S.; Laird, J.S.; Legge, G.J.F.; Bardos, R.A.; Moorhead, G.F.; Taylor, G.N.; Stuart, S.A.; Howard, J.

    1994-01-01

    The very high resolution (down to 50 nm) achieved with low beam currents (fA) in a scanning ion microprobe have lead to many nondestructive techniques of microanalysis. This paper discusses recent developments and applications in the use of 3-D STIM (scanning transmission ion microscopy) Tomography, channeling STIM and IBIC (ion beam induced charge). (orig.)

  5. The French AEC nuclear microprobe: description and first application examples

    Engelmann, C.; Bardy, J.

    1983-05-01

    The major components of the microprobe are briefly described. The performances and the varying possibilities authorized by the instrument are given. Some application examples concerning especially the determination of concentration profiles in an aqueous leached glass and the distribution of deuterium in a graphite sample exposed to plasma in a Tokamak device are presented

  6. [Clinical analysis of vocal fold firbrous mass].

    Chen, Hao; Sun, Jing Wu; Wan, Guang Lun; Hu, Yan Ming

    2018-03-01

    To explore the character of laryngoscopy finding, voice, and therapy of vocal fold fibrous mass. Clinical data, morphology, voice character, surgery and pathology of 15 cases with vocal fold fibrous mass were analyzed. The morbidity of vocal fold fibrous mass might be related to overuse of voice and laryngopharyngeal reflex. Laryngoscopy revealed shuttle line appearance, smoothness and decreased mucosal wave of vocal fold. These patients were invalid for voice training and might be improved by surgery, but recovery is slow. The morbidity of vocal fold fibrous mass might be related to overuse of voice and laryngopharyngeal reflex. Conservative treatment is ineffective for this disease, and surgery might improve. Copyright© by the Editorial Department of Journal of Clinical Otorhinolaryngology Head and Neck Surgery.

  7. Spatial and temporal analysis of mass movement using dendrochronology

    Braam, R.R.; Weiss, E.E.J.; Burrough, P.A.

    1987-01-01

    Tree growth and inclination on sloping land is affected by mass movement. Suitable analysis of tree growth and tree form can therefore provide considerable information on mass movement activity. This paper reports a new, automated method for studying the temporal and spatial aspects of mass

  8. Mass spectrometric analysis for nuclear safeguards

    BOULYGA S.; KONEGGER-KAPPEL S.; RICHTER Stephan; SANGELY L.

    2014-01-01

    Mass spectrometry is currently being implemented in a wide spectrum of research and industrial areas, such as material sciences, cosmo- and geochemistry, biology and medicine, to name just a few. Research and development in nuclear safeguards is closely related to the general field of “Peace Research”; representing a specific application area for analytical sciences in general and for mass spectrometry in particular. According to Albert Einstein “peace cannot be kept by force. It only can be ...

  9. Health worries: analysis of mass media influence

    Beléndez, Marina; Martín Llaguno, Marta; Suriá Martínez, Raquel; Hernández-Ruiz, Alejandra

    2004-01-01

    Póster presentado en 18th Annual Conference of the European Health Psychology Society, 21-24 June 2004, Helsinki, Finland. During the last years, mass media have centred on health and illness information more than ever before and stories about health risks fill up newspapers, magazines, TV programmes and internet sites. Recently, much of these informations are focused on emergent health risks, such as genetically modified food. In western countries, mass media appear as one of the main ...

  10. Analysis of irradiated materials

    Bellamy, B.A.

    1988-01-01

    Papers presented at the UKAEA Conference on Materials Analysis by Physical Techniques (1987) covered a wide range of techniques as applied to the analysis of irradiated materials. These varied from reactor component materials, materials associated with the Authority's radwaste disposal programme, fission products and products associated with the decommissioning of nuclear reactors. An invited paper giving a very comprehensive review of Laser Ablation Microprobe Mass Spectroscopy (LAMMS) was included in the programme. (author)

  11. D-Zero top quark mass analysis

    Strovink, M.

    1996-10-01

    I report on D null's preliminary analyses of the top quark mass m t based on an exposure at √s = 1.8 TeV with integrated luminosity ∼100 pb -1 at the Fermilab Tevatron p anti p collider. From three e + μ + ≥ 2 jet events (with background 0.36 ± 0.09), using partly original methods, we obtain m t = 158 ± 24(stat) ± 10(syst) GeV/c 2 . From 30 e or μ + ±4 jets events (with background 17.4 ±2.2), we find m t = 170 ± 15(stat) ± 10(syst) GeV/c 2 . Recently, using multivariate methods based on particular kinematic variables, we have learned how to improve the background suppression in the latter sample without unduly distorting the reconstructed top mass spectra. Applying these methods should improve considerably the accuracy of our top quark mass determination

  12. Chiral analysis of quenched baryon masses

    Young, R.D.; Leinweber, D.B.; Thomas, A.W.; Wright, S. V.

    2002-01-01

    We extend to quenched QCD an earlier investigation of the chiral structure of the masses of the nucleon and the delta in lattice simulations of full QCD. Even after including the meson-loop self-energies which give rise to the leading and next-to-leading nonanalytic behavior (and hence the most rapid variation in the region of light quark mass), we find surprisingly little curvature in the quenched case. Replacing these meson-loop self-energies by the corresponding terms in full QCD yields a remarkable level of agreement with the results of the full QCD simulations. This comparison leads to a very good understanding of the origins of the mass splitting between these baryons

  13. New 2-stage ion microprobes and a move to higher energies

    Legge, G.J.F.; Dymnikov, A.; Moloney, G.; Saint, A. [Melbourne Univ., Parkville, VIC (Australia). School of Physics; Cohen, D. [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia)

    1996-12-31

    Recent moves in Ion Beam Microanalysis towards the use of a rapidly growing number of very high resolution, low current and single ion techniques has led to the need for high demagnification and greatly improved beam quality. There is also a move to apply Microbeams at higher energies and with heavier ions. This also puts demands on the focusing system and beam control. This paper describes the recent development of 2-stage lens systems to be applied here and overseas, both at very high resolution and at high energies with heavy ions. It looks at new ion beam analysis applications of such ion microprobes. 8 refs., 1 tab., 1 fig.

  14. A new Krakow scanning nuclear microprobe performance tests and early application experienc

    Lebed, S; Polak, W; Potempa, A W; Stachura, Z; Paszkowski, M

    2001-01-01

    A new scanning nuclear microprobe (MP) with a short-length probe forming system was designed,installed and tested at the 3MV Van de Graaff accelerator in Krakow.The MP resolution of 3.3 mu m was reached for 2.4 MeV proton beam in the high-current mode (>= 100pA).The MP facility provides a local,non-destructive,quantitative elemental microanalysis using a Proton Induced X-ray Emission (PIXE) technique.As example of possible application an analysis of a geological sample containing monazite crystals investigated by PIXE method is presented.

  15. New 2-stage ion microprobes and a move to higher energies

    Legge, G J.F.; Dymnikov, A; Moloney, G; Saint, A [Melbourne Univ., Parkville, VIC (Australia). School of Physics; Cohen, D [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia)

    1997-12-31

    Recent moves in Ion Beam Microanalysis towards the use of a rapidly growing number of very high resolution, low current and single ion techniques has led to the need for high demagnification and greatly improved beam quality. There is also a move to apply Microbeams at higher energies and with heavier ions. This also puts demands on the focusing system and beam control. This paper describes the recent development of 2-stage lens systems to be applied here and overseas, both at very high resolution and at high energies with heavy ions. It looks at new ion beam analysis applications of such ion microprobes. 8 refs., 1 tab., 1 fig.

  16. CMB v. 1.1 Data Acquisition and Evaluation System of the Cracow Nuclear Microprobe

    Lekki, J.; Hajduk, R.; Potempa, A.; Pieprzyca, T.; Stachura, Z.; Zieblinski, M.; Styczen, J.; Lebed, S.

    2000-11-01

    An overview of the Cracow nuclear microprobe together with its data acquisition and control system is presented. Magnetic deflection was applied for beam scanning, while detector signals acquisition is performed by the NIM/CAMAC modules under supervision of a Windows operating system running on a PC equipped with the GPIB controller card. Total spectra from every detector are accessible on-line during the measurement, while full information about detected energy and beam position is stored to a disk file in the list mode to allow off-line data analysis. System hardware and software setups together with software operations and data formats used for information storing are described. (author)

  17. X-ray microprobe measurements of the chemical compositions of ALH84001 carbonate globules

    Flynn, G.J.; Sutton, S.R.; Keller, L.P.

    2004-01-01

    We measured minor element contents of carbonate from ALH84001 and report trends in tbe Ca, V, Mn and Sr in carbonate and the associated magnetite bands. McKay et al. suggested that carbonate globules in the ALH84001 meteorite from Mars contained evidence consistent with the development of bacterial life early in the history of Mars. This result provoked an extensive study of the ALH84001 meteorite. More recently Thomas-Keprta et al. have published a study showing that the magnetite associated with carbonate rims are of the size and shape produced by terrestrial bacteria. This paper has revived interest in ALH84001. The typical ALH84001 carbonate globule consists of four regions: a core of Fe-rich carbonate, a thin magnetite-rich band, a rim of Mn-rich carbonate, and another thin magnetite-rich band. Trace element analysis of each of these phases may allow us to address several important questions about these carbonates: (1) The origin of the magnetite-rich bands in the ALH84001 carbonate globules. If the magnetites are derived from the underlying carbonate through thermal decomposition (as proposed by Golden et al.), then we expect to see 'inherited' trace elements in these magnetite bands. (2) The origin of the rim carbonate, by determining whether the carbonate in the core has the same trace elements as the rim carbonates. (3) The age of the rim carbonate. Borg et al. dated the formation of the rim carbonate using the Rb/Sr chronometer. Borg et al. performed their measurements on an aliquot of what they called a high-Rb, low-Sr carbonate separate from the rim. We previously measured the trace element contents of chips from core and rim carbonates from an ALH84001 carbonate globule using an X-Ray Microprobe on Beamline X26A at the National Synchrotron Light Source. These measurements showed the rim carbonate had a very low Rb content, with Sr>>Rb, inconsistent with the ∼5 ppm Rb reported by Borg et al. in the sample they dated by the Rb/Sr chronometer. The large

  18. Individual precipitates in Al alloys probed by the Bonn positron microprobe

    Balarisi, Osman; Eich, Patrick; Haaks, Matz; Klobes, Benedikt; Korff, Bjoern; Maier, Karl; Sottong, Reinhard [Helmholtz-Institut fuer Strahlen- und Kernphysik, Nussallee 14-16, 53115 Bonn (Germany); Huehne, Sven-Martin; Mader, Werner [Institut fuer Anorganische Chemie, Roemerstrasse 164, 53117 Bonn (Germany); Staab, Torsten [Fraunhofer ISC, Neunerplatz 2, 97082 Wuerzburg (Germany)

    2010-07-01

    Positron annihilation spectroscopy (PAS) is a unique tool for the characterization of open-volume defects such as vacancies. Therefore, age hardenable Al alloys, whose decomposition is mainly driven by the vacancy mechanism of diffusion, are often characterized by PAS techniques. Nevertheless, probing the defect state of individual precipitates grown in Al alloys requires a focused positron beam and has not been carried out up to now. In this respect we present the first investigations of the defect state of individual precipitates utilizing the Bonn Positron Microprobe (BPM). Furthermore, the analysis of the experimental data has to be facilitated by theoretical calculations of the observables of positron annihilation spectroscopy.

  19. Effect of magnetic quadrupole lens alignment on a nuclear microprobe resolution

    Kolinko, S.V.; Ponomarev, A.G.

    2016-01-01

    The paper reports the research trends in developing probe-forming systems with high demagnification and analysis factors that limit a nuclear microprobe resolution. Parasitic aberrations caused by tilts and offsets of magnetic quadrupoles are studied in terms of their effect on probe parameters on a target. The most common arrangements of probe-forming systems such as a triplet and “Russian quadruplet” with separated geometry are considered. The accuracy prerequisites for the positioning of the quadrupoles are defined, and practical guidelines for alignment of probe-forming systems with high demagnification factors are suggested.

  20. Forensic analysis of explosions: Inverse calculation of the charge mass

    Voort, M.M. van der; Wees, R.M.M. van; Brouwer, S.D.; Jagt-Deutekom, M.J. van der; Verreault, J.

    2015-01-01

    Forensic analysis of explosions consists of determining the point of origin, the explosive substance involved, and the charge mass. Within the EU fP7 project Hyperion, TNO developed the Inverse Explosion Analysis (TNO-IEA) tool to estïmate the charge mass and point of origin based on observed damage

  1. ;Study of secondary hydriding at high temperature in zirconium based nuclear fuel cladding tubes by coupling information from neutron radiography/tomography, electron probe micro analysis, micro elastic recoil detection analysis and laser induced breakdown spectroscopy microprobe

    Brachet, Jean-Christophe; Hamon, Didier; Le Saux, Matthieu; Vandenberghe, Valérie; Toffolon-Masclet, Caroline; Rouesne, Elodie; Urvoy, Stéphane; Béchade, Jean-Luc; Raepsaet, Caroline; Lacour, Jean-Luc; Bayon, Guy; Ott, Frédéric

    2017-05-01

    This paper gives an overview of a multi-scale experimental study of the secondary hydriding phenomena that can occur in nuclear fuel cladding materials exposed to steam at high temperature (HT) after having burst (loss-of-coolant accident conditions). By coupling information from several facilities, including neutron radiography/tomography, electron probe micro analysis, micro elastic recoil detection analysis and micro laser induced breakdown spectroscopy, it was possible to map quantitatively, at different scales, the distribution of oxygen and hydrogen within M5™ clad segments having experienced ballooning and burst at HT followed by steam oxidation at 1100 and 1200 °C and final direct water quenching down to room temperature. The results were very reproducible and it was confirmed that internal oxidation and secondary hydriding at HT of a cladding after burst can lead to strong axial and azimuthal gradients of hydrogen and oxygen concentrations, reaching 3000-4000 wt ppm and 1.0-1.2 wt% respectively within the β phase layer for the investigated conditions. Consistent with thermodynamic and kinetics considerations, oxygen diffusion into the prior-β layer was enhanced in the regions highly enriched in hydrogen, where the α(O) phase layer is thinner and the prior-β layer thicker. Finally the induced post-quenching hardening of the prior-β layer was mainly related to the local oxygen enrichment. Hardening directly induced by hydrogen was much less significant.

  2. Determination of the chemical properties of residues retained in individual cloud droplets by XRF microprobe at SPring-8

    Ma, C.-J.; Tohno, S.; Kasahara, M.; Hayakawa, S.

    2004-01-01

    To determine the chemical properties of residue retained in individual cloud droplets is primarily important for the understanding of rainout mechanism and aerosol modification in droplet. The sampling of individual cloud droplets were carried out on the summit of Mt. Taiko located in Tango peninsula, Kyoto prefecture, during Asian dust storm event in March of 2002. XRF microprobe system equipped at SPring-8, BL-37XU was applied to the subsequent quantification analysis of ultra trace elements in residues of individual cloud droplets. It was possible to form the replicas of separated individual cloud droplets on the thin collodion film. The two dimensional XRF maps for the residues in individual cloud droplets were clearly drawn by scanning of micro-beam. Also, XRF spectra of trace elements in residues were well resolved. From the XRF spectra for individual residues, the chemical mixed state of residues could be assumed. The chemical forms of Fe (Fe +++ ) and Zn (Zn + ) could be clearly characterized by their K-edge micro-XANES spectra. By comparison of Z/Si mass ratios of residues in cloud droplets and those of the original sands collected in desert areas in China, the aging of ambient dust particles and their in cloud modification were indirectly assumed

  3. “Study of secondary hydriding at high temperature in zirconium based nuclear fuel cladding tubes by coupling information from neutron radiography/tomography, electron probe micro analysis, micro elastic recoil detection analysis and laser induced breakdown spectroscopy microprobe

    Brachet, Jean-Christophe, E-mail: jean-christophe.brachet@cea.fr [DEN-Service de Recherches Métallurgiques Appliquées (SRMA), CEA, Université Paris-Saclay, 91191 Gif-sur-Yvette (France); Hamon, Didier; Le Saux, Matthieu [DEN-Service de Recherches Métallurgiques Appliquées (SRMA), CEA, Université Paris-Saclay, 91191 Gif-sur-Yvette (France); Vandenberghe, Valérie [DEN-Service de Recherches Métallurgiques Appliquées (SRMA), CEA, Université Paris-Saclay, 91191 Gif-sur-Yvette (France); DEN-Service d’Etudes Mécaniques et Thermiques (SEMT), CEA, Université Paris-Saclay, 91191 Gif-sur-Yvette (France); Toffolon-Masclet, Caroline; Rouesne, Elodie; Urvoy, Stéphane [DEN-Service de Recherches Métallurgiques Appliquées (SRMA), CEA, Université Paris-Saclay, 91191 Gif-sur-Yvette (France); Béchade, Jean-Luc [DEN-Service de Recherches Métallurgiques Appliquées (SRMA), CEA, Université Paris-Saclay, 91191 Gif-sur-Yvette (France); DEN-Service de Recherches de Métallurgie Physique (SRMP), CEA, Université Paris-Saclay, 91191 Gif-sur-Yvette (France); Raepsaet, Caroline [LEEL, CEA, Université Paris-Saclay, 91191 Gif-sur-Yvette (France); NIMBE, CEA, CNRS, Université Paris-Saclay, 91191 Gif-sur-Yvette Cedex (France); and others

    2017-05-15

    This paper gives an overview of a multi-scale experimental study of the secondary hydriding phenomena that can occur in nuclear fuel cladding materials exposed to steam at high temperature (HT) after having burst (loss-of-coolant accident conditions). By coupling information from several facilities, including neutron radiography/tomography, electron probe micro analysis, micro elastic recoil detection analysis and micro laser induced breakdown spectroscopy, it was possible to map quantitatively, at different scales, the distribution of oxygen and hydrogen within M5™ clad segments having experienced ballooning and burst at HT followed by steam oxidation at 1100 and 1200 °C and final direct water quenching down to room temperature. The results were very reproducible and it was confirmed that internal oxidation and secondary hydriding at HT of a cladding after burst can lead to strong axial and azimuthal gradients of hydrogen and oxygen concentrations, reaching 3000–4000 wt ppm and 1.0–1.2 wt% respectively within the β phase layer for the investigated conditions. Consistent with thermodynamic and kinetics considerations, oxygen diffusion into the prior-β layer was enhanced in the regions highly enriched in hydrogen, where the α(O) phase layer is thinner and the prior-β layer thicker. Finally the induced post-quenching hardening of the prior-β layer was mainly related to the local oxygen enrichment. Hardening directly induced by hydrogen was much less significant. - Highlights: •More than 50% of the gaseous hydrogen produced by the inner clad oxidation absorbed and trapped into prior-β layer. •High hydrogen and oxygen local concentrations, up to 3000–4000 wt. ppm and 1.0–1.2 wt.% respectively, within the β phase. •Enhanced oxygen diffusion into hydrogen enriched prior-β layer, with locally thinner α(O) and thicker prior-β layers. •Post-quenching hardening of the prior-β structure mainly related to the (local) oxygen concentration.

  4. Development of a scanning proton microprobe - computer-control, elemental mapping and applications

    Loevestam, Goeran.

    1989-08-01

    A scanning proton microprobe set-up has been developed at the Pelletron accelerator in Lund. A magnetic beam scanning system and a computer-control system for beam scanning and data aquisition is described. The computer system consists of a VMEbus front-end computer and a μVax-II host-computer, interfaced by means of a high-speed data link. The VMEbus computer controls data acquisition, beam charge monitoring and beam scanning while the more sophisticated work of elemental mapping and spectrum evaluations is left to the μVax-II. The calibration of the set-up is described as well as several applications. Elemental micro patterns in tree rings and bark has been investigated by means of elemental mapping and quantitative analysis. Large variations of elemental concentrations have been found for several elements within a single tree ring. An external beam set-up has been developed in addition to the proton microprobe set-up. The external beam has been used for the analysis of antique papyrus documents. Using a scanning sample procedure and particle induced X-ray emission (PIXE) analysis, damaged and missing characters of the text could be made visible by means of multivariate statistical data evaluation and elemental mapping. Also aspects of elemental mapping by means of scanning μPIXE analysis are discussed. Spectrum background, target thickness variations and pile-up are shown to influence the structure of elemental maps considerably. In addition, a semi-quantification procedure has been developed. (author)

  5. Mass spectrometry a versatile aid to inorganic analysis

    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

  6. Thermogravimetric-quadrupole mass-spectrometric analysis of geochemical samples.

    Gibson, E. K., Jr.; Johnson, S. M.

    1972-01-01

    Thermogravimetric-quadrupole mass-spectrometric-analysis techniques can be used to study a wide variety of problems involving decomposition processes and identification of released volatile components. A recording vacuum thermoanalyzer has been coupled with a quadrupole mass spectrometer. The rapid scan capabilities of the quadrupole mass spectrometer are used to identify the gaseous components released. The capability of the thermogravimetric-quadrupole mass spectrometer to provide analytical data for identification of the released volatile components, for determination of their sequence of release and for correlation of thermal-decomposition studies is illustrated by an analysis of the Orgueil carbonaceous chondrite.

  7. Characterization of semiconductor and frontier materials by nuclear microprobe technology

    Zhu Jieqing; Li Xiaolin; Yang Changyi; Lu Rongrong; Wang Jiqing; Guo Panlin

    2002-01-01

    The nuclear microprobe technology is used to characterize the properties of semiconductor and other frontier materials at the stages of their synthesis, modification, integration and application. On the basis of the beam current being used, the analytical nuclear microprobe techniques being used in this project can be divided into two categories: high beam current (PIXE, RBS, PEB) or low beam current (IBIC, STIM) techniques. The material properties measured are the thickness and composition of a composite surface on a SiC ceramic, the sputtering-induced surface segregation and depth profile change in a Ag-Cu binary alloy, the irradiation effects on the CCE of CVD diamond, the CCE profile at a polycrystalline CVD diamond film and a GaAs diode at different voltage biases and finally, the characterization of individual sample on an integrated material chip. (author)

  8. Installation and performance of the Budapest-Hamburg proton microprobe

    Kovacs, I.; Kocsonya, A.; Kostka, P.; Szokefalvi-Nagy, Z.; Schrang, K.; Krueger, A.; Niecke, M.

    2005-01-01

    A new scanning proton microprobe has been installed at the 5 MV Van de Graaff accelerator of the KFKI Research Institute for Particle and Nuclear Physics. It is the energy-upgraded version of the Hamburg proton microprobe dismantled in 2001. The probe forming system includes a pair of focusing quadrupoles and an additional quadrupole pair in front of it, which is applied to increase the proton beam divergence. The average probe size at 2.5 MeV proton energy is 2.2 μm x 1.1 μm. The test results on stability and the preliminary experiments on cement corrosion and fish otoliths are also presented

  9. Wavelength dispersive μPIXE setup for the ion microprobe

    Fazinić, S., E-mail: stjepko.fazinic@irb.hr [Laboratory for Ion Beam Interactions, Division of Experimental Physics, Rudjer Bošković Institute, Bijenicka cesta 54, 10000 Zagreb (Croatia); Božičević Mihalić, I.; Tadić, T.; Cosic, D.; Jakšić, M. [Laboratory for Ion Beam Interactions, Division of Experimental Physics, Rudjer Bošković Institute, Bijenicka cesta 54, 10000 Zagreb (Croatia); Mudronja, D. [Croatian Conservation Institute, Grškovićeva 23, 10000 Zagreb (Croatia)

    2015-11-15

    We have developed a small wavelength dispersive X-ray spectrometer to explore the possibility of performing chemical speciation on microscopic samples utilizing focused ion beams available at the Rudjer Boskovic Institute ion microprobe. Although PIXE spectra are in principle chemically invariant, small influence of chemical effects could be observed even with Si(Li) or SDD detectors. Such chemical effects can be clearly seen with high resolution crystal X-ray spectrometers having energy resolution of several eV. A dedicated vacuum chamber, housing the diffraction crystal, sample holder and CCD X-ray detector, was constructed and positioned behind the main ion microprobe vacuum chamber. Here we will briefly describe the spectrometer, and illustrate its capabilities on measured K X-ray spectra of selected sulfur compounds. We will also demonstrate its abilities to resolve K and M X-ray lines irresolvable by solid state ED detectors usually used in PIXE.

  10. Raman microprobe study of heat-treated pitches

    Cottinet, D.; Couderc, P.; Saint Romain, J.L.; Dhamelincourt, P.

    1988-01-01

    A series of heat-treated pitches from the same coal-tar precursor is investigated by means of a Raman microprobe. Separated Raman spectra are obtained for the isotropic phase and the mesophase. The evolutions observed are characteristic of the structural rearrangement change in the two phases. They correlate well with the observations reported in literature and obtained by using different methods of structural investigations.

  11. Design considerations for an x-ray microprobe

    Howells, M.R.; Hastings, J.B.

    1982-01-01

    The optical design of a fluorescent microprobe covering the x-ray region from 2 to 16 keV is considered for the NSLS x-ray ring. The limit on detectability is from total flux (photons/μm 2 ) and several design choices are considered to match the optical system to the storage ring to maximize throughput. The tradeoffs in image quality and energy resolution of these designs have been considered and within these constraints two firm proposals are presented

  12. The nuclear microprobe of the CENBG: the choices

    Llabador, Y.

    1987-04-01

    A microbeam line with a spatial resolution of the micrometer order has been set on the Van de Graaf of the Bordeaux-Gradignan nuclear center. This report presents the different stages of the microprobe design: the experimental device which has been chosen, the reason of the different choices, the traps to keep out of during the construction (for instance, the accuracy of the mechanical standards) [fr

  13. Use of X-ray microprobe to diagnose bone tissue demineralization after caffeine administration Use of X-ray microprobe to diagnose bone tissue demineralization after caffeine administration

    Marek Tomaszewski

    2012-10-01

    Full Text Available Caffeine is a methylxanthine which permeates the placenta. In studies on animals, it has been
    shown to produce teratogenic and embryotoxic effects in large doses. The objective of this study was to
    assess the influence of caffeine on the development of bone tissue, with particular reference to elemental
    bone composition using an X-ray microprobe. The research was conducted on rats. The fertilized females
    were randomly divided into an experimental and a control group. The experimental group was
    given caffeine orally in 30 mg/day doses from the 8th to the 21st day of pregnancy, while the control group
    was given water. The fetuses were used to assess the growth and mineralization of the skeleton. On the
    basis of double dyeing, a qualitative analysis of the bone morphology and mineralization was conducted.
    For calcium and potassium analysis, an X-ray microprobe was used. In 67 fetuses from the experimental
    group, changes in skeleton staining with the alcian-alizarin method were noticed. The frequency of the
    development of variants in the experimental group was statistically higher. In the experimental group,
    a significant decrease in the calcium level, as well as an increase in the potassium level, was observed.
    The X-ray microprobe’s undoubted advantage is that is offers a quick qualitative and quantitative analysis
    of the elemental composition of the examined samples. Employing this new technique may furnish us
    with new capabilities when investigating the essence of the pathology process.Caffeine is a methylxanthine which permeates the placenta. In studies on animals, it has been
    shown to produce teratogenic and embryotoxic effects in large doses. The objective of this study was to
    assess the influence of caffeine on the development of bone tissue, with particular reference to elemental
    bone composition using an X-ray microprobe. The research was conducted on

  14. The Fudan nuclear microprobe set-up and performance

    Zhong, L.; Zhuang, W.; Shen, H.; Mi, Y.; Wu, Y.; Liu, B.; Yang, M.; Cheng, H.

    2007-01-01

    A new scanning nuclear microprobe has been constructed at the Institute of Modern Physics in Fudan University, to replace the old microbeam system which had been running for more than ten years. The key parts were purchased from Oxford Microbeams Ltd., including triplet quadrupole lens (model OM-150), collimator slits, scanning system, target chamber, and data acquisition system. Ion beams are provided from a NEC 9SDH-2 Tandem accelerator. Three CCD cameras and multiple monitors were installed to assist beam adjust. The design of beam line and beam monitors is described. Beam optics calculations were carried out based on the specific Fudan microprobe system geometry, and the results regarding beam line performance and limitations of the spacial resolution are presented and discussed here. A comparison with experimental results is given as well. About 1.5 μm beam spot size could be achieved with a 3 MeV proton beam at a current of around 10 pA. Recently, the new microprobe is applied to obtain information of fly ash particle, algae cell and otoliths

  15. Liquid chromatography - mass spectrometry analysis of pharmaceuticals

    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)

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

    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....

  17. Quantitative mass-spectrometric analysis of hydrogen helium isotope mixtures

    Langer, U.

    1998-12-01

    This work deals with the mass-spectrometric method for the quantitative analysis of hydrogen-helium-isotope mixtures, with special attention to fusion plasma diagnostics. The aim was to use the low-resolution mass spectrometry, a standard measuring method which is well established in science and industry. This task is solved by means of the vector mass spectrometry, where a mass spectrum is repeatedly measured, but with stepwise variation of the parameter settings of a quadruple mass spectrometer. In this way, interfering mass spectra can be decomposed and, moreover, it is possible to analyze underestimated mass spectra of complex hydrogen-helium-isotope mixtures. In this work experimental investigations are presented which show that there are different parameters which are suitable for the UMS-method. With an optimal choice of the parameter settings hydrogen-helium-isotope mixtures can be analyzed with an accuracy of 1-3 %. In practice, a low sensitivity for small helium concentration has to be noted. To cope with this task, a method for selective hydrogen pressure reduction has been developed. Experimental investigations and calculations show that small helium amounts (about 1 %) in a hydrogen atmosphere can be analyzed with an accuracy of 3 - 10 %. Finally, this work deals with the effects of the measuring and calibration error on the resulting error in spectrum decomposition. This aspect has been investigated both in general mass-spectrometric gas analysis and in the analysis of hydrogen-helium-mixtures by means of the vector mass spectrometry. (author)

  18. Nuclear microprobe studies of elemental distribution in the seagrass Thalassodendron ciliatum

    Barnabas, A.D. E-mail: alban@pixie.udw.ac.za; Przybylowicz, W.J.; Mesjasz-Przybylowicz, J.; Pineda, C.A

    1999-09-02

    Elemental levels and distributions in various organs (leaves, upright stems, rhizomes and roots) of the seagrass Thalassodendron ciliatum were determined using the NAC nuclear microprobe. Elemental distributions were obtained using the true elemental imaging system Dynamic Analysis (DA). Cl was the most abundant element present in the organs, occurring in all tissues, but present in relatively low concentrations in epidermal cells of leaves and roots. Na, K, S and Mg were also abundant and occurred in all organ tissues. Ca concentration was highest in the leaves, especially in the epidermis. Low concentrations of P were found and its tissue distribution was limited. Although Fe, Cu, Zn, Mn, Br, Ti and Si were present in relatively small amounts, enrichment of the epidermis with Fe, Ti and Si in all organs, was observed. Fe concentration was the highest in rhizomes while Si concentration was highest in upright stems. The significance of these elemental distribution patterns and the value of the nuclear microprobe in elemental analysis of seagrasses are discussed.

  19. Structural and electrical characterisation of semiconductor materials using a nuclear microprobe

    Jamieson, D.N.

    1998-01-01

    The domain of high-resolution imaging techniques (sub-micron) traditionally belongs to low-energy ion beams (ke V ion microprobe), electrons (transmission or scanning electron microscopy), light (near field microscopy), or all variants of scanning probe microscopies. Now, nuclear techniques of analysis, with a nuclear microprobe, have entered this domain, bringing a range of unique techniques for making images. In addition to-conventional techniques like Rutherford (and non-Rutherford) backscattering spectrometry and particle induced x-ray emission for structural characterisation, new ion beam analysis techniques have been developed for electrical characterisation as well. Foremost of these new techniques is ion beam induced charge (IBIC) which has seen an explosion of applications in the last five years to the study of charge transport properties of a variety of materials including polycrystalline diamond and silicon. An additional novel technique is ionoluminescence, which may be used to image various electronic properties of the material. Presented here are some examples of these imaging techniques in a variety of semiconductor materials. In all these examples, the specimens display structural inhomogeneities on the scale of 10 micrometres, making it essential to employ a focused beam. (author)

  20. Structural and electrical characterisation of semiconductor materials using a nuclear microprobe

    Jamieson, D.N. [Melbourne Univ., Parkville, VIC (Australia). School of Physics, Microanalytical Centre

    1998-06-01

    The domain of high-resolution imaging techniques (sub-micron) traditionally belongs to low-energy ion beams (ke V ion microprobe), electrons (transmission or scanning electron microscopy), light (near field microscopy), or all variants of scanning probe microscopies. Now, nuclear techniques of analysis, with a nuclear microprobe, have entered this domain, bringing a range of unique techniques for making images. In addition to-conventional techniques like Rutherford (and non-Rutherford) backscattering spectrometry and particle induced x-ray emission for structural characterisation, new ion beam analysis techniques have been developed for electrical characterisation as well. Foremost of these new techniques is ion beam induced charge (IBIC) which has seen an explosion of applications in the last five years to the study of charge transport properties of a variety of materials including polycrystalline diamond and silicon. An additional novel technique is ionoluminescence, which may be used to image various electronic properties of the material. Presented here are some examples of these imaging techniques in a variety of semiconductor materials. In all these examples, the specimens display structural inhomogeneities on the scale of 10 micrometres, making it essential to employ a focused beam. (author). Extended abstract. 18 refs. 4 figs.

  1. Mass spectrometry for real-time quantitative breath analysis

    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

  2. The expanding universe of mass analyzer configurations for biological analysis.

    Calvete, Juan J

    2014-01-01

    Mass spectrometry (MS) is an analytical technique that measures the mass-to-charge ratio of electrically charged gas-phase particles. All mass spectrometers combine ion formation, mass analysis, and ion detection. Although mass analyzers can be regarded as sophisticated devices that manipulate ions in space and time, the rich diversity of possible ways to combine ion separation, focusing, and detection in dynamic mass spectrometers accounts for the large number of instrument designs. A historical perspective of the progress in mass spectrometry that since 1965 until today have contributed to position this technique as an indispensable tool for biological research has been recently addressed by a privileged witness of this golden age of MS (Gelpí J. Mass Spectrom 43:419-435, 2008; Gelpí J. Mass Spectrom 44:1137-1161, 2008). The aim of this chapter is to highlight the view that the operational principles of mass spectrometry can be understood by a simple mathematical language, and that an understanding of the basic concepts of mass spectrometry is necessary to take the most out of this versatile technique.

  3. Ion microprobe imaging of 44Ca-labeled mammalian chromosomes

    Levi-Setti, R.; Gavrilov, K.L.; Strissel, P.L.; Strick, R.

    2004-01-01

    In our previous investigation, we showed for the first time high-resolution analytical images of the cation composition of mammalian interphase and mitotic cells as well as of isolated metaphase chromosomes using the University of Chicago scanning ion microprobe (UC-SIM). In order to preserve the ionic integrity of the analyzed cells and prevent the well known occurrence of analytical artifacts due to the high diffusivity of cations in biological samples we used fast cryo-preservation methods (freeze-drying and freeze fracture), without any pre-fixations or washes. We identified the role of the cations in chromosome structure and maintenance using SIMS imaging and immunfluorescence methodologies. Importantly, we determined that the above cations are essential participants in chromosome condensation and maintenance of chromatin higher order structure, through their presumed function in DNA electrostatic neutralization and the direct interaction of Ca 2+ , in particular, with structural proteins. In addition, both Ca 2+ and Mg 2+ showed the same cell cycle regulation where during interphase both cations were enriched in the cytosol, particularly in organelles then at mitosis became specifically bound to chromatin. Our present research interest focuses on a more detailed analysis of the distribution of Ca 2+ throughout the different cell cycle stages, e.g. G1, G2 and mitosis. We have chosen the stable isotope 44 Ca as a tracer to follow Ca 2+ throughout the cell cycle. This nuclide occurs naturally in the ratio 44 Ca/ 40 Ca+ 44 Ca of 2.06%, so that incorporation at higher concentrations into chromatin or other cellular components should be easily detected by SIMS. Such incorporation can be obtained either by growing cells in a medium where ordinary Ca is replaced entirely by 44 Ca, or by replacing the cell culture medium with the 44 Ca medium for a gated time span (pulsing), after appropriate cell cycle stage synchronization. In this paper, we describe our

  4. Classification of mammographic masses using geometric symmetry and fractal analysis

    Guo Qi; Ruiz, V.F. [Cybernetics, School of Systems Engineering, Univ. of Reading (United Kingdom); Shao Jiaqing [Dept. of Electronics, Univ. of Kent (United Kingdom); Guo Falei [WanDe Industrial Engineering Co. (China)

    2007-06-15

    In this paper, we propose a fuzzy symmetry measure based on geometrical operations to characterise shape irregularity of mammographic mass lesion. Group theory, a powerful tool in the investigation of geometric transformation, is employed in our work to define and describe the underlying mathematical relations. We investigate the usefulness of fuzzy symmetry measure in combination with fractal analysis for classification of masses. Comparative studies show that fuzzy symmetry measure is useful for shape characterisation of mass lesions and is a good complementary feature for benign-versus-malignant classification of masses. (orig.)

  5. Gas Chromatography-Mass Spectrometric Analysis and Insecticidal ...

    HP

    Original Research Article. Gas Chromatography-Mass Spectrometric Analysis and ... into a natural fumigant/insecticide for the control of stored product insects. Keywords: Mallotus ..... stability as well as reduce cost. ACKNOWLEDGEMENT.

  6. Gas Chromatography-Mass Spectrometric Analysis of Nematicidal ...

    Gas Chromatography-Mass Spectrometric Analysis of Nematicidal Essential Oil of Valeriana ... Tropical Journal of Pharmaceutical Research ... have a potential to be developed to natural nematicides for the control of cereal cyst nematodes.

  7. SIMS device with quadrupole mass spectrometer

    Szigethy, D.; Riedel, M.

    1980-01-01

    A versatile secondary ion mass spectrometer (SIMS) has been designed and constructed. The device is applicable for dinamic and static SIMS investigations. The sputtering and ionisation can be studied simultaneously. Oil diffusion pumps and an auxiliary ion-getter pump are used. A commercial ion gun is used in the working chamber. The secondary ion optics assures the preliminary filtering of fast ions, and the collection of sputtered ions for a separate microprobe analysis. The performance of the apparatus is illustrated with examples. (R.J.)

  8. Elemental characterization of individual glia and glioma cells in the nuclear microprobe

    Lindh, U.

    1982-01-01

    To investigate whether variations in levels of microelements are reflected at the cellular level, a study of cultured cells was undertaken. For elemental characterization were chosen human glia and glioma cell lines. The cells were freeze-dried and about 1000 cells of each line were analyzed in the nuclear microprobe with a probe diameter of 10 μm. Scanning of the specimens under the beam made possible heat reduction and the X-ray spectrum induced was continuously recorded and subsequently processed in the computer. Elemental maps of the cells were then generated and the information from each member of the cell populations could be considered as well as the population statistics. Mass determination was accomplished by means of the bremsstrahlung continuum intensity. The main feature resulting from the characterization was that the glioma cells in average held appreciably higher contents of copper and zinc than did the glia cells. (orig.)

  9. Color electron microprobe cathodoluminescence of Bishunpur meteorite compared with the traditional optical microscopy method

    Amanda Araujo Tosi

    Full Text Available Abstract Cathodoluminescence (CL imaging is an outstanding method for sub classification of Unequilibrated Ordinary Chondrites (UOC - petrological type 3. CL can be obtained by several electron beam apparatuses. The traditional method uses an electron gun coupled to an optical microscope (OM. Although many scanning electron microscopes (SEM and electron microprobes (EPMA have been equipped with a cathodoluminescence, this technique was not fully explored. Images obtained by the two methods differ due to a different kind of signal acquisition. While in the CL-OM optical photography true colors are obtained, in the CL-EPMA the results are grayscale monochromatic electronic signals. L-RGB filters were used in the CL-EPMA analysis in order to obtain color data. The aim of this work is to compare cathodoluminescence data obtained from both techniques, optical microscope and electron microprobe, on the Bishunpur meteorite classified as LL 3.1 chondrite. The present study allows concluding that 20 KeV and 7 nA is the best analytical condition at EPMA in order to test the equivalence between CL-EPMA and CL-OM colour results. Moreover, the color index revealed to be a method for aiding the study of the thermal metamorphism, but it is not definitive for the meteorite classification.

  10. Optical system optimization of the microprobe beamline of the Ion Implantation Laboratory (IF-UFRGS), Brazil

    Bauer, Deiverti de Vila

    2015-01-01

    The aim of the present work is to optimize the microprobe beamline of the Ion Implantation Laboratory (IF-UFRGS). In short, an ion microprobe consists of charged particles focused to the dimensions of a few micrometers. The focusing system is made of two slits for demagnification, a set of magnetic lenses with scanning capability and a reaction chamber. By changing the parameters related to this system, one can optimize the features of the beam. To that end, samples of poly(tereftalate etylene) were irradiated with 2.2 MeV H+ ions and etched, yielding 2D microstructures with high aspect ratio. The analysis of the structures with Scanning Electron Microscopy proved to be an important tool in order to establish a correlation between the size of the microstructures and the parameters of the focusing system. In this work, the causes leading to a beam enlargement are discussed, as well as the aberrations which affect the system. Finally, the advantages of using ions for lithography purposes is pointed out. (author)

  11. New mass analysis and results for neutron rich nuclei performed with isochronous mass spectrometry

    Diwisch, Marcel [Justus-Liebig-Universitaet Giessen, Giessen (Germany); Knoebel, Ronja; Geissel, Hans; Plass, Wolfgang; Scheidenberger, Christoph [Justus-Liebig-Universitaet Giessen, Giessen (Germany); GSI Helmholtzzentrum fuer Schwerionenforschung, Darmstadt (Germany); Patyk, Zygmunt [Soltan Institute for Nuclear Studies, Warsaw (Poland); Weick, Helmut [GSI Helmholtzzentrum fuer Schwerionenforschung, Darmstadt (Germany)

    2015-07-01

    The Isochronous Mass Spectrometry (IMS) allows to measure masses of rare exotic nuclei in a storage ring in a timescale of tens of μs. The ring is operated in an isochronous mode, i.e. such that particles with different velocities but same mass-to-charge ratio (m/q) travel different paths in the ring arcs (faster ions travel longer paths whereas slower ions travel shorter paths). This means that for each m/q a fix revolution time exists and can be measured by a time-of-flight (TOF) detector which then yields the masses of the nuclei for known charge states. A new analysis approach of IMS data with a correlation matrix method allowed combining data with different quality. The latest production run was using an additional determination of the magnetic rigidity which increased the resolving power of the experiment. Combining this experiment with previous experiments one can increase the statistics and accuracy of the overall mass determination. It was possible to deduce mass values of neutron rich isotopes which have not been measured before. One of those isotopes is {sup 130}Cd which is a very important nuclei involved in the r-process. Those mass values and a comparison to theoretical predictions will be presented in the poster.

  12. Determination of SB2 masses and age: introduction of the mass ratio in the Bayesian analysis

    Giarrusso, M.; Leone, F.; Tognelli, E.; Degl'Innocenti, S.; Prada Moroni, P. G.

    2018-04-01

    Stellar age assignment still represents a difficult task in Astrophysics. This unobservable fundamental parameter can be estimated only through indirect methods, as well as generally the mass. Bayesian analysis is a statistical approach largely used to derive stellar properties by taking into account the available information about the quantities we are looking for. In this paper we propose to apply the method to the double-lined spectroscopic binaries (SB2), for which the only available information about masses is the observed mass ratio of the two components. We validated the method on a synthetic sample of Pre-Main Sequence (PMS) SB2 systems showing the capability of the technique to recover the simulated age and masses. Then, we applied our procedure to the PMS eclipsing binaries Parenago 1802 and RX J0529.4+0041 A, whose masses of both components are known, by treating them as SB2 systems. The estimated masses are in agreement with those dynamically measured. We conclude that the method, if based on high resolution and high signal-to-noise spectroscopy, represents a robust way to infer the masses of the very numerous SB2 systems together with their age, allowing to date the hosting astrophysical environments.

  13. Determination of SB2 masses and age: introduction of the mass ratio in the Bayesian analysis

    Giarrusso, M.; Leone, F.; Tognelli, E.; Degl'Innocenti, S.; Prada Moroni, P. G.

    2018-07-01

    Stellar age assignment still represents a difficult task in Astrophysics. This unobservable fundamental parameter can be estimated only through indirect methods, as well as generally the mass. Bayesian analysis is a statistical approach largely used to derive stellar properties by taking into account the available information about the quantities we are looking for. In this paper, we propose to apply the method to the double-lined spectroscopic binaries (SB2), for which the only available information about masses is the observed mass ratio of the two components. We validated the method on a synthetic sample of pre-main-sequence (PMS) SB2 systems showing the capability of the technique to recover the simulated age and masses. Then, we applied our procedure to the PMS eclipsing binaries Parenago 1802 and RX J0529.4+0041 A, whose masses of both components are known, by treating them as SB2 systems. The estimated masses are in agreement with those dynamically measured. We conclude that the method, if based on high resolution and high signal-to-noise spectroscopy, represents a robust way to infer the masses of the very numerous SB2 systems together with their age, allowing to date the hosting astrophysical environments.

  14. A tunable x-ray microprobe using synchrotron radiation

    Wu, Y.; Thompson, A.C.; Underwood, J.H.; Giauque, R.D.; Chapman, K.; Rivers, M.L.; Jones, K.W.

    1989-08-01

    We describe an x-ray microprobe using multilayer mirrors. Previously, we had demonstrated a Kirkpatrick-Baez type focusing system working at both 8 and 10 keV and successfully applied it to a variety of applications, including the determination of elemental contents in fluid inclusions. In this paper, we show that the usable excitation energy for this microprobe is not restricted to between 8 and 10 keV, and furthermore, it can be simply tuned in operation. A 10-keV x-ray fluorescence microprobe can be used to measure the concentration of the elements form potassium (Z = 19) to zinc (Z = 30) using K x-ray lines, and from cadmium (Z = 48) to erbium (Z = 68) using L x-ray lines. There are a number of geologically important elements in the gap between gallium (Z = 31) and silver(Z = 47) and also with Z > 68. In order to cover this range, a higher excitation energy is required. On the other hand, for samples that contain major elements with absorption edges lower than the excitation energy, it would be hard to detect other mirror elements because of the strong signal from the major elements and the background they produce. In this case, a tunable x-ray source can be used to avoid the excitation of the major elements. We demonstrate that, with the existing setup, it is possible to tune the excitation energy from 6 keV to 14 keV, in this range, the intensity does not decrease by more than one order of magnitude. As an illustration, a geological sample was examined by using two different excitation energy range as well as the possibility of improving the intensity. 11 refs., 5 figs

  15. Analysis of Damped Mass-Spring Systems for Sound Synthesis

    Don Morgan

    2009-01-01

    Full Text Available There are many ways of synthesizing sound on a computer. The method that we consider, called a mass-spring system, synthesizes sound by simulating the vibrations of a network of interconnected masses, springs, and dampers. Numerical methods are required to approximate the differential equation of a mass-spring system. The standard numerical method used in implementing mass-spring systems for use in sound synthesis is the symplectic Euler method. Implementers and users of mass-spring systems should be aware of the limitations of the numerical methods used; in particular we are interested in the stability and accuracy of the numerical methods used. We present an analysis of the symplectic Euler method that shows the conditions under which the method is stable and the accuracy of the decay rates and frequencies of the sounds produced.

  16. X-ray microprobe for the microcharacterization of materials

    Sparks, C.J.; Ice, G.E.

    1988-01-01

    The unique properties of x rays offer many advantages over those of electrons and other charged particles for the microcharacterization of materials. X rays are more efficient in exciting characteristic x-ray fluorescence and produce higher fluorescent signal-to-background ratios than obtained with electrons. Such x-ray microprobes will also produce unprecedentedly low levels of detection in diffraction, EXAFS, Auger, and photoelectron spectroscopies for structural and chemical characterization and elemental identification. These major improvements in microcharacterization capabilities will have wide-ranging ramifications not only in materials science but also in physics, chemistry, geochemistry, biology, and medicine. 24 refs., 6 figs., 2 tabs

  17. Enhancements to the analytical facilities at the GNS proton microprobe

    Barry, B.J.; Markwitz, A.; Kennedy, V.J.; Trompetter, W.J.

    2005-01-01

    In recent years a number of detection systems have been added to the proton microprobe facility at GNS Science. Particular additions have been a large area HPGe detector and a system for scanning transmission imaging microscopy. The HPGe detector has improved detection sensitivity, particularly for higher energy K x-rays where energy resolution is of lesser importance. The scanning microscopy system has enabled mapping of areal densities in biological samples to give accurate elemental maps. Examples are given of these applications. (author). 22 refs., 7 figs

  18. Operation and acquisition automation of a nuclear microprobe

    Simond, Isabelle

    1990-01-01

    The purpose of this work was to design the hardware and the software parts of data acquisition and its graphical analyses of a nuclear microprobe. Our realisation was built from a microprocessor 68020 and specialized co-processors on a VME bus. The more important demand was the amount of time required to collect the data and to perform the graphical analyses during the acquisition. To overcome this problem, we adapted a real time operating system and its kernel to our need, and built special graphical processes. (author) [fr

  19. Integrated analysis of rock mass deformation within shaft protective pillar

    Ewa Warchala

    2016-01-01

    Full Text Available The paper presents an analysis of the rock mass deformation resulting from mining in the vicinity of the shaft protection pillar. A methodology of deformation prediction is based on a deterministic method using Finite Element Method (FEM. The FEM solution is based on the knowledge of the geomechanical properties of the various geological formations, tectonic faults, types of mining systems, and the complexity of the behaviour of the rock mass. The analysis gave the stress and displacement fields in the rock mass. Results of the analysis will allow for design of an optimal mining system. The analysis is illustrated by an example of the shaft R-VIII Rudna Mine KGHM Polish Copper SA.

  20. Trans-Regional technologies and the Lapita problem: characterisation of volcanic glass inclusions by electron microprobe

    Grave, P.; Nockolds, C.; White, P.

    1997-01-01

    Full text: Analysis of pre-modern pottery of the Pacific has long attempted to formulate measures independent of style for constructing archaeologically meaningful groups. However, the variable character of fabrics and the longevity of production (Lapita and post-Lapita wares from 3000 years ago to the present) have tended to obscure differences due to changes in production practices and resources through time and differences relating to the exchange of ceramics between islands or regions. In this poster we outline a preliminary study that employs an economical and robust technique to distinguish both within- and between-region groups. This is achieved with electron microprobe analysis of small volcanic glass fragments present in wares tempered with volcanic sands, and interpretation based on Principal Components Analysis. The method builds on the chemical groupings for glass from different volcanic complexes in the Pacific established through high energy ion beam (PIXE-PIGME) analysis. The purpose of this study is to characterise a selection of samples of pottery from the Duke of York's peninsula using electron microprobe analysis of very small glass fragments in the sections that ranged in size from around 0.05 mm to 1 mm.. The study involved the identification and elemental characterisation of individual fragments of glass in a section. Principal Component Analysis was used to identify structure latent in the dataset. The results of the study show that clear characterisation is possible to enable the wider application of the technique to Lapita and post Lapita ceramics produced originating in volcanic areas of the Pacific

  1. Inorganic trace analysis by laser ionization mass spectrometry

    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.)

  2. Laser ionization mass spectrometry in inorganic trace analysis

    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.)

  3. Ion beam induced luminescence from diamond using an MeV ion microprobe

    Bettiol, A A; Jamieson, D N; Prawer, S; Allen, M G [Melbourne Univ., Parkville, VIC (Australia). School of Physics

    1994-12-31

    Analysis of the luminescence induced by a MeV ion beam offers the potential to provide useful information about the chemical properties of atoms in crystals to complement the information provided by more traditional Ion Beam Analysis (IBA) such as Rutherford Backscattering Spectrometry (RBS), ion channeling and Particle Induced X-ray Emission (PIXE). Furthermore, the large penetration depth of the MeV ion beam offers several advantages over the relatively shallow penetration of keV electrons typically employed in cathodoluminescence. An Ion Beam Induced Luminescence (IBIL) detection system was developed for the Melbourne microprobe that allows the spatial mapping of the luminescence signal along with the signals from RBS and PIXE. Homoepitaxial diamond growth has been studied and remarkable shifts in the characteristic blue luminescence of diamond towards the green were observed in the overgrowth. This has been tentatively identified as being due to transition metal inclusions in the epitaxial layers. 8 refs., 2 refs.

  4. Ion beam induced luminescence from diamond using an MeV ion microprobe

    Bettiol, A.A.; Jamieson, D. N.; Prawer, S.; Allen, M.G. [Melbourne Univ., Parkville, VIC (Australia). School of Physics

    1993-12-31

    Analysis of the luminescence induced by a MeV ion beam offers the potential to provide useful information about the chemical properties of atoms in crystals to complement the information provided by more traditional Ion Beam Analysis (IBA) such as Rutherford Backscattering Spectrometry (RBS), ion channeling and Particle Induced X-ray Emission (PIXE). Furthermore, the large penetration depth of the MeV ion beam offers several advantages over the relatively shallow penetration of keV electrons typically employed in cathodoluminescence. An Ion Beam Induced Luminescence (IBIL) detection system was developed for the Melbourne microprobe that allows the spatial mapping of the luminescence signal along with the signals from RBS and PIXE. Homoepitaxial diamond growth has been studied and remarkable shifts in the characteristic blue luminescence of diamond towards the green were observed in the overgrowth. This has been tentatively identified as being due to transition metal inclusions in the epitaxial layers. 8 refs., 2 refs.

  5. Present status of research and development on X-ray microprobe

    Koike, Masaki; Suzuki, I.H.

    1991-01-01

    X-ray beam micro-analysis has advanced rapidly in these years in conjunction with the development of powerful X-ray sources. Among a variety of methods being attempted, the method using a collimated narrow beam has been important because of high brightness, and of usability in both regions of soft and hard X-rays. In the soft X-ray region, the focused beam is formed by a fresnel zone plate or a Schwaltzschild mirror assembly, and can be used for scanning transmission microscope or scanning photoelectron microscope. In the hard X-ray region, the beam is formed by grazing incidence mirrors, and can be used for X-ray fluorescence micro-analysis for obtaining elemental mapping. In this report, the recent progress on the soft X-ray scanning microscopy and the X-ray microprobe has been surveyed, together with the improvement on the related optical elements. (author) 84 refs

  6. Online Open Neuroimaging Mass Meta-Analysis with a Wiki

    Nielsen, Finn Arup; Kempton, Matthew J.; Williams, Steven C. R.

    2015-01-01

    We describe a system for meta-analysis where a wiki stores numerical data in a simple comma-separated values format and a web service performs the numerical statistical computation. We initially apply the system on multiple meta-analyses of structural neuroimaging data results. The described system...... allows for mass meta-analysis, e.g., meta-analysis across multiple brain regions and multiple mental disorders providing an overview of important relationships and their uncertainties in a collaborative environment....

  7. Realtime control system for microprobe beamline at PLS

    Yoon, J.C.; Lee, J.W.; Kim, K.H.; Ko, I.S. [Pohang Accelerator Laboratory, POSTECH, Pohang (Korea)

    1998-11-01

    The microprobe beamline of the Pohang Light Source (PLS) consists of main and second slits, a microprobe system, two ion chambers, a video-microscope, and a Si(Li) detector. These machine components must be controlled remodely through the computer system to make user's experiments precise and speedy. A real-time computer control system was developed to control and monitor these components. A VMEbus computer with an OS-9 real-time operating system was used for the low-level data acquisition and control. VME I/O modules were used for the step motor control and the scalar control. The software has a modular structure for the maximum performance and the easy maintenance. We developed the database, the I/O driver, and the control software. We used PC/Windows 95 for the data logging and the operator interface. Visual C{sup ++} was used for the graphical user interface programming. RS232C was used for the communication between the VME and the PC. (author)

  8. Characterization of PE-g-HEMA films prepared by gamma irradiation through nuclear microprobe techniques

    Ferreira, L.M.; Rodrigues, P.A.; Falcao, A.N.; Leal, J.P.

    2011-01-01

    Complete text of publication follows. The functional success of a copolymer as biomaterial depends fundamentally on their mechanical properties (stemming from the material matrix) and on the characteristics of its surface. For biomedical applications, among all the other important properties, the biocompatibility of the surface acquires extreme importance and can dictate its rejection. One of the issues regarding biocompatibility is cytotoxicity which strongly depends on the contamination level at surface. Ion beam analysis techniques associated to Nuclear Microprobe (PIXE, RBS and STIM) allows a rigorous and precise analysis of the concentration (ppm) and distribution of elements contamination, and may also provide information on its near-surface structure. In this work PE-g-HEMA films with different grafting yields were prepared by mutual gamma irradiation at a 60 Co source and were analyzed through nuclear microprobe. Data collected allowed the qualitative and quantitative evaluation of contaminants distribution observed in the different samples as well as the clarification of some processes occurred during the copolymerization reaction. Qualitative analysis showed a random and no homogeneous distribution of the contaminant elements, independent of the grafting degree, suggesting the existence of several sources of contamination at different stages of their preparation. Results also suggest that this 'phased' contamination occurs simultaneously with mechanisms of agglomeration/entrapment of impurities during the gamma induced copolymerization reaction. Moreover, quantitative data showed that all contaminants found in the copolymeric films are natural contaminants of their reagents of preparation, although at concentrations without toxicological hazard, which points to a low cytotoxic potential. The combined analysis of these data with data from SEM and AFM allowed a better understanding of the surface structure and other properties already observed in these

  9. Mass

    Quigg, Chris

    2007-01-01

    In the classical physics we inherited from Isaac Newton, mass does not arise, it simply is. The mass of a classical object is the sum of the masses of its parts. Albert Einstein showed that the mass of a body is a measure of its energy content, inviting us to consider the origins of mass. The protons we accelerate at Fermilab are prime examples of Einsteinian matter: nearly all of their mass arises from stored energy. Missing mass led to the discovery of the noble gases, and a new form of missing mass leads us to the notion of dark matter. Starting with a brief guided tour of the meanings of mass, the colloquium will explore the multiple origins of mass. We will see how far we have come toward understanding mass, and survey the issues that guide our research today.

  10. General theory of three-dimensional radiance measurements with optical microprobes RID A-1977-2009

    FukshanskyKazarinova, N.; Fukshansky, L.; Kuhl, M.

    1997-01-01

    Measurements of the radiance distribution and fluence rate within turbid samples with fiber-optic radiance microprobes contain a large variable instrumental error caused by the nonuniform directional sensitivity of the microprobes. A general theory of three-dimensional radiance measurements...

  11. Progress of the new CSIRO-GEMOC nuclear microprobe: first results, performance and recent applications

    Ryan, C.G.; Cripps, G.; Sie, S.H.; Suter, G.F.; Jamieson, D.N.; Griffin, W.L.; Commonwealth Scientific and Industrial Research Organisation

    1999-01-01

    The new CSIRO-GEMOC Nuclear Microprobe (NMP) features a number of technical advances for high resolution, high sensitivity microanalysis. It was designed at the CSIRO and developed as collaboration between the CSlRO, the GEMOC key-centre at Macquarie University and the MARC group of the University of Melbourne. For imaging applications, it also features a software system using a powerful algorithm called Dynamic Analysis, developed at the CSIRO for unmixing elemental signatures in proton induced X-ray emission (PIXE) data, to provide a tool for rapid quantitative imaging of trace and major element spatial distribution in minerals. This paper reports on the performance of the NMP and examples of its application over the past 6 months since completion

  12. Trace element composition and distribution in micron area of dinosaur eggshell fossils determined by proton microprobe

    Chen Youhong; Zhu Jieqing; Wang Xiaohong; Wang Yimin

    1997-01-01

    The scanning proton microprobe and micro-PIXE quantitative analysis technique have been used to determine composition and distribution of the trace elements in micron areas of dinosaur eggshell fossils from the stratum of Upper Cretaceous system at Nanxiong Basin in Guangdong Province, China. The study shows that the trace elements mainly include Ti, V, Cr, Mn, Co, Ni, Cu, Zn, As, Rb, Sr, Y, Zr, Sb, Ba and Pb in the micron area, but they present different distributions. While the element Sr is mainly enriched in the near surface layer, others mainly reside in the near inner layer. A preliminary discussion on the reason of the dinosaur extinction is given based on the above study

  13. Trace element composition and distribution in micron area of dinosaur eggshell fossils determined by proton microprobe

    Chen Youhong; Zhu Jieqing; Wang Xiaohong; Wang Yimin

    1997-01-01

    The scanning proton microprobe and micro-PIXE quantitative analysis technique have been used to determine composition and distribution of the trace elements in micron areas of dinosaur eggshell fossils from the stratum of Upper Cretaceous system at Nanxiong Basin in Guangdong Province, China. The study shows that the trace elements mainly include Ti, V, Cr, Mn, Co, Ni, Cu, Zn, As, Rb, Sr, Y, Zr, Sb, Ba and Pb in the micron area, but they present different distributions. While the elements Sr is mainly enriched in the near surface layer, others mainly reside in the near inner layer. A preliminary discussion on the reason of the dinosaur extinction is given based on the above study

  14. Microprobe study of fission product behavior in high-burnup HTR fuels

    Kleykamp, H.

    Electron microprobe analysis of irradiated coated particles with high burnup (greater than 50 percent fima) gives detailed information on the chemical state and the transport behavior of the fission products in UO 2 and UC 2 kernels and in the coatings. In oxide fuel kernels, metallic inclusions and ceramic precipitations are observed. The solubility behavior of the fission products in the fuel matrix has been investigated. Fission product inclusions could not be detected in carbide fuel kernels; post irradiation annealed UC 2 kernels, however, give information on the element combinations of some fission product phases. Corresponding to the chemical state in the kernel, Cs, Sr, Ba, Pd, Te and the rare earths are released easily and diffuse through the entire pyrocarbon coating. These fission products can be retained by a silicon carbide layer. The initial stage of a corrosive attack of the SiC coating by the fission products is evidenced

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

    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.

  16. On-Line Synthesis and Analysis by Mass Spectrometry

    Bain, Ryan M.; Pulliam, Christopher J.; Raab, Shannon A.; Cooks, R. Graham

    2015-01-01

    In this laboratory experiment, students learn how to use ESI to accelerate chemical synthesis and to couple it with on-line mass spectrometry for structural analysis. The Hantzsch synthesis of symmetric 1,4-dihydropyridines is a classic example of a one-pot reaction in which multiple intermediates can serve to indicate the progress of the reaction…

  17. Gas Chromatographic-Mass Spectrometric Analysis of Essential Oil ...

    Purpose: To analyze the essential oil composition of the flower of Jasminum officinale L. var. grandifloroum L. (Jasminum grandiflorum) by gas chromatography-mass spectrometry (GC-MS). Methods: The optimum GC-MS conditions used for the analysis were 250 oC inlet temperature, 150 oC MSD detector temperature, ...

  18. Fundamentals of Biomolecule Analysis by Electrospray Ionization Mass Spectrometry

    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…

  19. Molecular characterization and expression analysis of fat mass and ...

    Keywords. fat mass and obesity-associated gene (FTO); rabbit; mRNA expression patterns; sequence analysis; Oryctolagus cuniculus. ... In this work, the molecular characterization and expression features of rabbit (Oryctolagus cuniculus) FTO cDNA were analysed. The rabbit FTO cDNA with a size of 2158 bp was cloned, ...

  20. Isotopic analysis of plutonium by computer controlled mass spectrometry

    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

  1. Mercury mass measurement in fluorescent lamps via neutron activation analysis

    Viererbl, L.; Vinš, M.; Lahodová, Z.; Fuksa, A.; Kučera, J.; Koleška, M.; Voljanskij, A.

    2015-01-01

    Mercury is an essential component of fluorescent lamps. Not all fluorescent lamps are recycled, resulting in contamination of the environment with toxic mercury, making measurement of the mercury mass used in fluorescent lamps important. Mercury mass measurement of lamps via instrumental neutron activation analysis (NAA) was tested under various conditions in the LVR-15 research reactor. Fluorescent lamps were irradiated in different positions in vertical irradiation channels and a horizontal channel in neutron fields with total fluence rates from 3×10 8 cm −2 s −1 to 10 14 cm −2 s −1 . The 202 Hg(n,γ) 203 Hg nuclear reaction was used for mercury mass evaluation. Activities of 203 Hg and others induced radionuclides were measured via gamma spectrometry with an HPGe detector at various times after irradiation. Standards containing an Hg 2 Cl 2 compound were used to determine mercury mass. Problems arise from the presence of elements with a large effective cross section in luminescent material (europium, antimony and gadolinium) and glass (boron). The paper describes optimization of the NAA procedure in the LVR-15 research reactor with particular attention to influence of neutron self-absorption in fluorescent lamps. - Highlights: • Mercury is an essential component of fluorescent lamps. • Fluorescent lamps were irradiated in neutron fields in research reactor. • 203 Hg induced radionuclide activity was measured using gamma spectrometry. • Mercury mass in fluorescent lamps can be measured by neutron activation analysis.

  2. Quantification of the distribution of hydrogen by nuclear microprobe at the Laboratory Pierre Sue in the width of zirconium alloy fuel clad of PWR reactors

    Raepsaet, C.; Bossis, Ph.; Hamon, D.; Bechade, J.L.; Brachet, J.C.

    2007-01-01

    Among the analysis techniques by ions beams, the micro ERDA (Elastic Detection Analysis) is an interesting technique which allows the quantitative distribution of the hydrogen in materials. In particular, this analysis has been used for hydride zirconium alloys, with the nuclear microprobe of the Laboratory Pierre Sue. This probe allows the characterization of radioactive materials. The technique principles are recalled and then two examples are provided to illustrate the fuel clad behavior in PWR reactors. (A.L.B.)

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

    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.

  4. Analysis of chirality by femtosecond laser ionization mass spectrometry.

    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.

  5. Implementation of ionoluminescence in the AGLAE scanning external microprobe

    Pichon, L.; Calligaro, T.; Gonzalez, V.; Lemasson, Q.; Moignard, B.; Pacheco, C.

    2015-01-01

    The scope of this work is to present the implementation of an IBIL imaging system in the scanning external microprobe of the AGLAE facility so as to correlate luminescence and composition maps provided by PIXE, RBS and PIGE. The challenging integration of the optical spectrometer, due to incompatibility of acquisition timings and data formats with the other IBA channels has motivated the development of a specific acquisition system. This article details the IBIL setup and explains the technical solutions retained for the coupling of IBIL with IBA techniques in order to produce fast and large IBIL-IBA maps. The IBIL maps stored in the same format as the PIXE, RBS and PIGE ones can be visualised and compared using the dedicated AGLAEmap program or the PyMCA processing package. An example of such a coupled mapping on Mesoamerican jade is presented to emphasise the interest of performing simultaneously IBA and IBIL large mappings

  6. Wireless cardiac action potential transmission with ultrasonically inserted silicon microprobes

    Shen, C J; Ramkumar, A; Lal, A; Gilmour, R F Jr

    2011-01-01

    This paper reports on the integration of ultrasonically inserted horn-shaped cardiac probes with wireless transmission of 3D cardiac action potential measurement for applications in ex vivo preparations such as monitoring the onset of ventricular fibrillation. Ultrasonically inserted silicon horn probes permit reduced penetration force during insertion, allowing silicon, a brittle material, to penetrate cardiac tissue. The probes also allow recording from multiple sites that are lithographically defined. An application-specific integrated circuit has been designed with a 40 dB amplifying stage and a frequency modulating oscillator at 95 MHz to wirelessly transmit the recorded action potentials. This ultrasonically inserted microprobe wireless system demonstrates the initial results in wireless monitoring of 3D action potential propagation, and the extraction of parameters of interest including the action potential duration and diastolic interval

  7. Data acquisition for X ray microprobe. User's manual

    2002-01-01

    A modified data acquisition software for X ray microprobe was developed by the Physics Group, Instrumentation Unit, IAEA Laboratories at Seibersdorf, with assistance from M. Bogovac, Croatia. The software consists of data acquisition (scanning and calibration), automatic positioning and micro-movement of sample, data reduction and evaluation. The acquisition software was designed in order to support different measurement set-ups which are applied in low-energy nuclear physics. The modification was done in 1999-2000 under the projects Nuclear Spectrometry and Utilization of Particle Accelerators. The manual supersedes the first version entitled Microanalysis Data Acquisition and Control Program published under Computer Manual Series, No. 9 in 1996. The software described in this manual is freely available from the IAEA upon request

  8. Isotope analysis of lithium by thermionic mass spectrometry

    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)

  9. Mass spectrometric methods for trace analysis of metals

    Bahr, U.; Schulten, H.R.

    1981-01-01

    A brief outline is given of the principles of mass spectrometry (MS) and the fundamentals of qualitative and quantitative mass spectrometric analysis emphasizing recent developments and results. Classical methods of the analysis of solids, i.e. spark-source MS and thermal ionization MS, as well as recent methods of metal analysis are described. Focal points in this survey of recently developed techniques include secondary ion MS, laser probe MS, plasma ion source MS, gas discharge MS and field desorption MS. Here, a more detailed description is given and the merits of these emerging methods are discussed more explicitly. In particular, the results of the field desorption techniques in elemental analyses are reviewed and critically evaluated

  10. Ion microprobe U-Pb dating of a dinosaur tooth

    Sano, Yuji; Terada, Kentaro; Ly, Chi V.; Park, Eun Ju

    2006-01-01

    Ion microprobe U-Pb dating of apatite is applied to a fossil tooth of a Allosaurid derived from the Hasandong Formation in the Gyeongsang basin, southeastern Korea. Twelve spots on a single fragment of the fossil dentine yield a Tera-Wasserburg concordia intercept age of 115±10 Ma (2σ, MSWD=0.59) on a 238 U/ 206 Pb- 207 Pb/ 206 Pb- 204 Pb/ 206 Pb diagram. The age provides a constraint on the depositional age of the fossil in its host Hassandong Formation as Early Aptian. The success of the ion microprobe dating depends on the heterogeneities of diagenetically incorporated U and Pb at the few hundred μm scale, the consequent variations in Pb isotopic compositions due to radioactive decay and the closed-system behavior of U and Pb. There are at least three end-members to explain the variations of minor chemical components such as FeO, SiO 2 and Al 2 O 3 , and trace elements as Th, U and rare earth elements (REE) in the sample by a simple mixing model. They are (1) very low minor and REE, very high common Pb with variable U abundances, (2) low common Pb, high minor, REE, and U abundances, and (3) low minor, common Pb, and U with intermediate REE abundances, even though groups (2) and (3) may consist of a larger group. Various contributions of the three (and/or two) end-members during diagenetic processes may cause the elemental fractionation of U and Pb in a fossil tooth. (author)

  11. Element analysis with a proton microprobe of early atherosclerotic lesions

    Roijers, R.B.

    2009-01-01

    Atherosclerosis is a progressive inflammatory vascular disease accompanied by a gradual build-up of cholesterol in the artery walls. The associated chronic inflammatory process leads to tissue damage in the vascular wall as a consequence of an excessive inflammatory response. Large calcified

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

    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.

  13. Secondary neutral mass spectrometry depth profile analysis of silicides

    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)

  14. AMIDST: Analysis of MassIve Data STreams

    Masegosa, Andres; Martinez, Ana Maria; Borchani, Hanen

    2015-01-01

    The Analysis of MassIve Data STreams (AMIDST) Java toolbox provides a collection of scalable and parallel algorithms for inference and learning of hybrid Bayesian networks from data streams. The toolbox, available at http://amidst.github.io/toolbox/ under the Apache Software License version 2.......0, also efficiently leverages existing functionalities and algorithms by interfacing to software tools such as HUGIN and MOA....

  15. Ultratrace analysis of uranium and plutonium by mass spectrometry

    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

  16. New Isotope Analysis Method: Atom Trap Mass Spectrometry

    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

  17. Mass spectrometric analysis of helium in stainless steel

    Isagawa, Hiroto; Wada, Yukio; Asakura, Yoshiro; Tsuji, Nobuo; Sato, Hitoshi; Tsutsumi, Kenichi

    1974-01-01

    Vacuum fusion mass-spectrometry was adopted for the analysis of helium in stainless steel. Samples were heated in a vacuum crucible, and helium in the samples was extracted and collected into a reservoir tank. The gas was then introduced through an orifice into a mass spectrometer, where the amount of helium was determined. The maspeq 070 quadrupole type mass spectrometer made by Shimazu Seisakusho, Ltd. was used. The resolving power was 150, and the mass range of the apparatus was 0-150. The determination limit of helium was about 2 x 10 -3 μg when standard helium gas was analyzed, and was about 10 -2 μg when the helium in stainless steel was analyzed. The relative standard deviation of helium intensity in repetitive measurement was about 2% in the amount of helium of 0.05 μg. Helium was injected into stainless steel by means of alpha particle irradiation with a cyclotron. The amount of helium in stainless steel was then determined. The energy of alpha particles was 34 MeV, and the beam area was 10 mm x 10 mm. The experimental data were higher than the expected value in one case, and were lower in the other case. This difference was attributable to the fluctuation of alpha particle beam, misplacement of sample plates, and unevenness of the alpha beam. (Fukutomi, T.)

  18. Mercury mass measurement in fluorescent lamps via neutron activation analysis

    Viererbl, L.; Vinš, M.; Lahodová, Z.; Fuksa, A.; Kučera, J.; Koleška, M.; Voljanskij, A.

    2015-11-01

    Mercury is an essential component of fluorescent lamps. Not all fluorescent lamps are recycled, resulting in contamination of the environment with toxic mercury, making measurement of the mercury mass used in fluorescent lamps important. Mercury mass measurement of lamps via instrumental neutron activation analysis (NAA) was tested under various conditions in the LVR-15 research reactor. Fluorescent lamps were irradiated in different positions in vertical irradiation channels and a horizontal channel in neutron fields with total fluence rates from 3×108 cm-2 s-1 to 1014 cm-2 s-1. The 202Hg(n,γ)203Hg nuclear reaction was used for mercury mass evaluation. Activities of 203Hg and others induced radionuclides were measured via gamma spectrometry with an HPGe detector at various times after irradiation. Standards containing an Hg2Cl2 compound were used to determine mercury mass. Problems arise from the presence of elements with a large effective cross section in luminescent material (europium, antimony and gadolinium) and glass (boron). The paper describes optimization of the NAA procedure in the LVR-15 research reactor with particular attention to influence of neutron self-absorption in fluorescent lamps.

  19. Transition of Iodine Analysis to Accelerator Mass Spectrometry

    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

  20. Transition of Iodine Analysis to Accelerator Mass Spectrometry

    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

  1. MPAI (mass probes aided ionization) method for total analysis of biomolecules by mass spectrometry.

    Honda, Aki; Hayashi, Shinichiro; Hifumi, Hiroki; Honma, Yuya; Tanji, Noriyuki; Iwasawa, Naoko; Suzuki, Yoshio; Suzuki, Koji

    2007-01-01

    We have designed and synthesized various mass probes, which enable us to effectively ionize various molecules to be detected with mass spectrometry. We call the ionization method using mass probes the "MPAI (mass probes aided ionization)" method. We aim at the sensitive detection of various biological molecules, and also the detection of bio-molecules by a single mass spectrometry serially without changing the mechanical settings. Here, we review mass probes for small molecules with various functional groups and mass probes for proteins. Further, we introduce newly developed mass probes for proteins for highly sensitive detection.

  2. Surface acoustic wave nebulization facilitating lipid mass spectrometric analysis.

    Yoon, Sung Hwan; Huang, Yue; Edgar, J Scott; Ting, Ying S; Heron, Scott R; Kao, Yuchieh; Li, Yanyan; Masselon, Christophe D; Ernst, Robert K; Goodlett, David R

    2012-08-07

    Surface acoustic wave nebulization (SAWN) is a novel method to transfer nonvolatile analytes directly from the aqueous phase to the gas phase for mass spectrometric analysis. The lower ion energetics of SAWN and its planar nature make it appealing for analytically challenging lipid samples. This challenge is a result of their amphipathic nature, labile nature, and tendency to form aggregates, which readily precipitate clogging capillaries used for electrospray ionization (ESI). Here, we report the use of SAWN to characterize the complex glycolipid, lipid A, which serves as the membrane anchor component of lipopolysaccharide (LPS) and has a pronounced tendency to clog nano-ESI capillaries. We also show that unlike ESI SAWN is capable of ionizing labile phospholipids without fragmentation. Lastly, we compare the ease of use of SAWN to the more conventional infusion-based ESI methods and demonstrate the ability to generate higher order tandem mass spectral data of lipid A for automated structure assignment using our previously reported hierarchical tandem mass spectrometry (HiTMS) algorithm. The ease of generating SAWN-MS(n) data combined with HiTMS interpretation offers the potential for high throughput lipid A structure analysis.

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

    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

  4. Laser microprobe for the study of noble gases and nitrogen in single ...

    R. Narasimhan (Krishtel eMaging) 1461 1996 Oct 15 13:05:22

    Planetary and Geosciences Division, Physical Research Laboratory, Ahmedabad 380 009, India. ∗e-mail: murty@prl.ernet.in. A laser microprobe capable of analysing nitrogen and noble gases in .... tion properties for light radiation, with some.

  5. Contribution to the application of nuclear microprobe in geochemistry. Carbon and nitrogen microanalysis in glasses and minerals

    Mosbah, M.

    1988-01-01

    The morphological complexity of geological materials implies the use of microanalysis techniques utilization. Nuclear microprobe allows selective and no destructive light elements determination, through nuclear reactions. Nuclear microanalysis has been used to characterize carbon and nitrogen in volatile phase dissolved in magmatic samples. The application of some microanalysis techniques in geochemistry are discussed, nuclear microprobe theory and techniques are developed. Minerals, glasses and glassy inclusions are described, and more particularly, the interest of these investigations. Optimal conditions of carbon and nitrogen analysis ( 12 C(d.p) 13 C and 14 N(d,p) 15 N reaction respectively), as deuteron energy and observation angle are studied. A methodology has been established for this purpose. Several results are exposed: Punctual analysis, carbon concentration profile in depth surface scanning, surficial mapping in glassy inclusions. The carbon content interpretation in glassy inclusions measured conveniently for the first time agrees with data obtained through other techniques. In conclusion, degazing schedule improvements require more analysis. Perspective research axis are evocated [fr

  6. Ion Mobility Mass Spectrometry Direct Isotope Abundance Analysis

    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

  7. The role of mass spectrometry in hydrocarbon analysis

    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)

  8. Raman microprobe measurements of stress in ion implanted materials

    Nugent, K W; Prawer, S; Weiser, P S; Dooley, S P [Melbourne Univ., Parkville, VIC (Australia). School of Physics

    1994-12-31

    Raman microprobe measurements of ion implanted diamond and silicon have shown significant shifts in the Raman line due to stresses in the materials. The Raman line shifts to higher energy if the stress is compressive and to lower energy for tensile stress{sup 1}. The silicon sample was implanted in a 60 {mu}m square with 2.56 x 10{sup 17} ions per square centimeter of 2 MeV Helium. This led to the formation of raised squares with the top 370mm above the original surface. In Raman studies of silicon using visible light, the depth of penetration of the laser beam into the sample is much less than one micron. It was found that the Raman line is due to the silicon overlying the damage region. The diamond sample was implanted with 2 x 10{sup 15} ions per square centimeter of 2.8 MeV carbon. It was concluded that the Raman spectrum could provide information concerning both the magnitude and the direction of stress in an ion implanted sample. It was possible in some cases to determine whether the stress direction is parallel or perpendicular to the sample surface. 1 refs., 2 figs.

  9. Raman microprobe measurements of stress in ion implanted materials

    Nugent, K.W.; Prawer, S.; Weiser, P.S.; Dooley, S.P. [Melbourne Univ., Parkville, VIC (Australia). School of Physics

    1993-12-31

    Raman microprobe measurements of ion implanted diamond and silicon have shown significant shifts in the Raman line due to stresses in the materials. The Raman line shifts to higher energy if the stress is compressive and to lower energy for tensile stress{sup 1}. The silicon sample was implanted in a 60 {mu}m square with 2.56 x 10{sup 17} ions per square centimeter of 2 MeV Helium. This led to the formation of raised squares with the top 370mm above the original surface. In Raman studies of silicon using visible light, the depth of penetration of the laser beam into the sample is much less than one micron. It was found that the Raman line is due to the silicon overlying the damage region. The diamond sample was implanted with 2 x 10{sup 15} ions per square centimeter of 2.8 MeV carbon. It was concluded that the Raman spectrum could provide information concerning both the magnitude and the direction of stress in an ion implanted sample. It was possible in some cases to determine whether the stress direction is parallel or perpendicular to the sample surface. 1 refs., 2 figs.

  10. Characterisation of Inorganic Pigments Used by Selected Painters by Using Ion Microprobe and Other Complementary Techniques

    Fazinic, S.; Pastuovic, Z.; Jaksic, M.; Kusijanovic, K.; Mudronja, D.; Braun, M.; Desnica, V.

    2011-01-01

    The aim of the presentation is to show results of the collaboration between the Croatian Conservation Institute (CCI) and the Laboratory for Ion Beam Interactions of the Rudjer Boskovic Institute (RBI) established within the present CRP. CCI is the central Croatian institution for conservation and restoration of cultural heritage objects. Prior to restoration/conservation CCI performs scientific analysis of an object, primarily to enable selection of the best strategy for its restoration/conservation. In many occasions such analysis is also helpful to resolve issues such as clarification of authenticity and/or authorship of an object. CCI has its analytical laboratory which is fully dedicated to the analysis of cultural heritage and art objects. CCI analytical laboratory is equipped with various microscopy techniques, photography methods, portable X-ray Fluorescence Spectrometer (XRF) and X-ray radiography instrumentation. Access to complementary microanalytical techniques like Raman Spectroscopy or Ion Beam Analytical (IBA) techniques is provided through already long and successful collaboration with RBI. The RBI Laboratory for Ion Beam Interactions provides complementary analysis of layered microsamples by using IBA techniques, such as Particle Induced X-ray Emission (PIXE) and Rutherford Back-scattering (RBS), and for the miniature samples by using ion microprobe. (author)

  11. Quantitative mass spectrometric analysis of glycoproteins combined with enrichment methods.

    Ahn, Yeong Hee; Kim, Jin Young; Yoo, Jong Shin

    2015-01-01

    Mass spectrometry (MS) has been a core technology for high sensitive and high-throughput analysis of the enriched glycoproteome in aspects of quantitative assays as well as qualitative profiling of glycoproteins. Because it has been widely recognized that aberrant glycosylation in a glycoprotein may involve in progression of a certain disease, the development of efficient analysis tool for the aberrant glycoproteins is very important for deep understanding about pathological function of the glycoprotein and new biomarker development. This review first describes the protein glycosylation-targeting enrichment technologies mainly employing solid-phase extraction methods such as hydrizide-capturing, lectin-specific capturing, and affinity separation techniques based on porous graphitized carbon, hydrophilic interaction chromatography, or immobilized boronic acid. Second, MS-based quantitative analysis strategies coupled with the protein glycosylation-targeting enrichment technologies, by using a label-free MS, stable isotope-labeling, or targeted multiple reaction monitoring (MRM) MS, are summarized with recent published studies. © 2014 The Authors. Mass Spectrometry Reviews Published by Wiley Periodicals, Inc.

  12. Analysis of soils by glow discharge mass spectrometry

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

    1993-01-01

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

  13. 7th international conference on Nuclear microprobe technology and applications; 7. conference internationale sur la technologie et les applications des microsondes nucleaires

    NONE

    2000-07-01

    This colloquium gives an up-to-date report on the continuously advancing applications and development of microbeam technology. It presents abstracts and oral contributions in the following domains: microprobes facilities, analysis techniques, imaging techniques, micro-ion beam modification of materials, microelectronics, applications in Material Sciences in Biology in Medicine in earth and planetary Sciences in environment in art in archaeology, alternative techniques. (A.L.B.)

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

    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.)

  15. A mass spectrometer for the rapid analysis of gaseous mixtures

    Cassignol, C.; Ortel, Y.; Taieb, J.

    1950-01-01

    A mass spectrometer for leak detection and rapid gas analysis were constructed, having the characteristics and several structural features of a simple instrument described by Siry in Rev. Sri. Instruments. 540 (1947). Although exhibiting a good resolving power, the apparatus, which has no ion lenses and whose electrodes can be regulated during the performance, has not been sufficiently tested. Since several design defects have been discovered, it will probably be rebuilt with various improvements (ion source outside the magnetic field, modified circuits, etc.). (author)

  16. Recent Advances in Water Analysis with Gas Chromatograph Mass Spectrometers

    MacAskill, John A.; Tsikata, Edem

    2014-01-01

    We report on progress made in developing a water sampling system for detection and analysis of volatile organic compounds in water with a gas chromatograph mass spectrometer (GCMS). Two approaches are described herein. The first approach uses a custom water pre-concentrator for performing trap and purge of VOCs from water. The second approach uses a custom micro-volume, split-splitless injector that is compatible with air and water. These water sampling systems will enable a single GC-based instrument to analyze air and water samples for VOC content. As reduced mass, volume, and power is crucial for long-duration, manned space-exploration, these water sampling systems will demonstrate the ability of a GCMS to monitor both air and water quality of the astronaut environment, thereby reducing the amount of required instrumentation for long duration habitation. Laboratory prototypes of these water sampling systems have been constructed and tested with a quadrupole ion trap mass spectrometer as well as a thermal conductivity detector. Presented herein are details of these water sampling system with preliminary test results.

  17. Laser desorption mass spectrometry for fast DNA analysis

    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.

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

    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.

  19. A study of aluminium-exposed fish using a scanning proton microprobe

    Cholewa, M; Legge, G L.F. [Melbourne Univ., Parkville, VIC (Australia). School of Physics; Eeckhaoudt, S; Van Grieken, R [Universitaire Instelling Antwerpen, Antwerp (Belgium)

    1994-12-31

    A major problem has arisen in Europe with the depopulation of fresh water fish in lakes and streams collecting acid rain. The sensitivity to acidification is species specific and appears to be associated with metal levels. The Scanning Proton Microprobe (SPMP) at the Micro Analytical Research Centre of the University of Melbourne was used to study the subcellular distribution of aluminium and other elements in the gills of fish exposed to acidified water with elevated Al-levels. Experiments were performed on thin sections taken from fish exposed to media with different pH and aluminium concentration. Aluminium was found on the surface of the gill lamellae, but also inside the tissue. Bulk analysis of the gills showed much higher concentrations in the aluminium-exposed fish, compared to the control ones, but no information regarding the actual accumulation sites can be inferred. Extensive study of damage done to the sample by intense proton beams during elemental analysis was performed with scanning transmission ion microscopy. 3 refs., 3 figs.

  20. A study of aluminium-exposed fish using a scanning proton microprobe

    Cholewa, M.; Legge, G.L.F. [Melbourne Univ., Parkville, VIC (Australia). School of Physics; Eeckhaoudt, S.; Van Grieken, R. [Universitaire Instelling Antwerpen, Antwerp (Belgium)

    1993-12-31

    A major problem has arisen in Europe with the depopulation of fresh water fish in lakes and streams collecting acid rain. The sensitivity to acidification is species specific and appears to be associated with metal levels. The Scanning Proton Microprobe (SPMP) at the Micro Analytical Research Centre of the University of Melbourne was used to study the subcellular distribution of aluminium and other elements in the gills of fish exposed to acidified water with elevated Al-levels. Experiments were performed on thin sections taken from fish exposed to media with different pH and aluminium concentration. Aluminium was found on the surface of the gill lamellae, but also inside the tissue. Bulk analysis of the gills showed much higher concentrations in the aluminium-exposed fish, compared to the control ones, but no information regarding the actual accumulation sites can be inferred. Extensive study of damage done to the sample by intense proton beams during elemental analysis was performed with scanning transmission ion microscopy. 3 refs., 3 figs.

  1. Practical aspects of quantitative laser Raman microprobe spectroscopy for the study of fluid inclusions

    Pasteris, J.D.; Wopenka, B.; Seitz, J.C.

    1988-01-01

    This paper is addressed to both geologists who use laser Raman microprobe (LRM) spectroscopy to analyze fluid inclusions and to those who want to evaluate analyses done by this technique. Emphasis is on how to obtain quantitative analyses of fluid inclusions. The authors discuss the basic method of fluid inclusion analysis by LRM spectroscopy and the levels of accuracy and precision attainable with this technique. They evaluate which kinds of fluid inclusions and host mineral matrices will yield the most reliable compositional data. Necessary sample preparations, detection limits, problems with fluorescence, dependence of Raman scattering efficiencies on density, and many other questions asked at the workshop on Raman spectroscopy during the 1987 ACROFI meeting also are addressed. The complementary nature, advantages, and disadvantages of both LRM spectroscopy and microthermometry, the two techniques most frequently used for the analysis of individual fluid inclusions, are emphasized. Some discussions are intended to held LRM users calibrate, and evaluate the optical characteristics of, their particular instruments. It is hoped that this paper will further LRM users in finding a common ground on which to discuss the differences and similarities among different LRM instruments, and that it will encourage a future consensus on efficient means of calibration and on interlaboratory standards

  2. A study of aluminium-exposed fish using a scanning proton microprobe

    Cholewa, M.; Legge, G.L.F.

    1993-01-01

    A major problem has arisen in Europe with the depopulation of fresh water fish in lakes and streams collecting acid rain. The sensitivity to acidification is species specific and appears to be associated with metal levels. The Scanning Proton Microprobe (SPMP) at the Micro Analytical Research Centre of the University of Melbourne was used to study the subcellular distribution of aluminium and other elements in the gills of fish exposed to acidified water with elevated Al-levels. Experiments were performed on thin sections taken from fish exposed to media with different pH and aluminium concentration. Aluminium was found on the surface of the gill lamellae, but also inside the tissue. Bulk analysis of the gills showed much higher concentrations in the aluminium-exposed fish, compared to the control ones, but no information regarding the actual accumulation sites can be inferred. Extensive study of damage done to the sample by intense proton beams during elemental analysis was performed with scanning transmission ion microscopy. 3 refs., 3 figs

  3. Analysis of hazardous biological material by MALDI mass spectrometry

    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.

  4. Isotopic analysis of boron by thermal ionization mass spectrometry

    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)

  5. Preliminary Mass Spectrometric Analysis of Uranium on Environmental Swipe Materials

    Cheong, Chang-Sik; Jeong, Youn-Joong; Ryu, Jong-Sik; Shin, Hyung-Seon; Cha, Hyun-Ju; Ahn, Gil-Hoon; Park, Il-Jin; Min, Gyung-Sik

    2006-01-01

    It is well-known that uranium and plutonium isotopic compositions of safeguards samples are very useful to investigate the history of nuclear activities. To strengthen the capabilities of environmental sampling analysis in the ROK through MOST/DOE collaboration, round robin test for uranium and plutonium was designed in 2003. As the first round robin test, a set of dried uranium-containing solutions (∼35ng and (∼300ng) was distributed to the participating laboratories in November of 2003, with results reported in April of 2004. The KBSI (Korea Basic Science Institute) and ORNL (Oak Ridge National Laboratory) are currently in the process of analyzing uranium on cotton swipes for the second round robin test. As a preliminary test for the second round, KBSI intends to analyze home-made swipe samples into which international uranium standards are added. Here we describe technical steps of sample preparation and mass spectrometry at KBSI, and report some results of the preliminary test

  6. Tissue preservation with mass spectroscopic analysis: Implications for cancer diagnostics.

    Hall, O Morgan; Peer, Cody J; Figg, William D

    2018-05-17

    Surgical intervention is a common treatment modality for localized cancer. Post-operative analysis involves evaluation of surgical margins to assess whether all malignant tissue has been resected because positive surgical margins lead to a greater likelihood of recurrence. Secondary treatments are utilized to minimize the negative effects of positive surgical margins. Recently, in Science Translational Medicine, Zhang et al describe a new mass spectroscopic technique that could potentially decrease the likelihood of positive surgical margins. Their nondestructive in vivo tissue sampling leads to a highly accurate and rapid cancer diagnosis with great precision between healthy and malignant tissue. This new tool has the potential to improve surgical margins and accelerate cancer diagnostics by analyzing biomolecular signatures of various tissues and diseases.

  7. Isotopic analysis of uranium by thermoionic mass spectrometry

    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

  8. Selective laser ionization for mass-spectral isotopic analysis

    Miller, C.M.; Nogar, N.S.; Downey, S.W.

    1983-01-01

    Resonant enhancement of the ionization process can provide a high degree of elemental selectivity, thus eliminating or drastically reducing the interference problem. In addition, extension of this method to isotopically selective ionization has the potential for greatly increasing the range of isotope ratios that can be determined experimentally. This gain can be realized by reducing or eliminating the tailing of the signal from the high-abundance isotope into that of the low-abundance isotope, augmenting the dispersion of the mass spectrometer. We briefly discuss the hardware and techniques used in both our pulsed and cw RIMS experiments. Results are presented for both cw ionization experiments on Lu/Yb mixtures, and spectroscopic studies of multicolor RIMS of Tc. Lastly, we discuss practical limits of cw RIMS analysis in terms of detection limits and measurable isotope ratios

  9. Raman and luminescence spectroscopy of zirconium oxide with the use of the MOLE microprobe

    Doyle, T.E.; Alvarez, J.L.

    1984-01-01

    Raman and luminescence spectroscopy with the use of the MOLE microprobe has been used to characterize ZrO 2 originating from oxidized fuel-rod cladding in nuclear accidents. Micro-Raman analysis of samples from Three Mile Island Unit 2 and the Power Burst Facility identified tetragonal and cubic ZrO 2 . The tetragonal and cubic phases are high-temperature polymorphs of ZrO 2 and provide information about temperatures and hydrogen formation in the TMI-2 core. The data suggest that the tetragonal ZrO 2 in TMI-2 samples was stabilized by a crystallite size effect, whereas cubic ZrO 2 in PBF debris samples was stabilized by impurities. Luminescence was used to differentiate yttria-stabilized ZrO 2 ceramics and oxidized fuel-rod cladding in PBF debris samples. The ZrO 2 ceramics produced strong, sharp luminescence peaks which indicated the presence of titanium and yttria in the ZrO 2 . Oxidized fuel-rod cladding displayed no luminescence

  10. Treatment of dentin with stannous fluoride - SEM and electron microprobe study

    Ellingsen, J.E.; Roella, G.

    1987-01-01

    The effect of SnF 2 -treatment of dentin surfaces was investigated by means of scanning electron microscopy (SEM) and electron microprobe analysis. Human dentin was treated with aqueous SnF 2 solutions of concentrations varying from 1 to 10%. The treatment periods lasted for 1, 5, 10 or 60 min. Both tin and fluoride were identified on the surfaces. The concentration varied depending on the extensiveness of the treatment. Immersion in 1 M KOH for 15 h removed both tin and fluoride from the surfaces. This reaction was not observed after immersion in H 2 O for the same time period. Examination of the SnF 2 -treated dentin surfaces showed a dense layer of globular particles and in addition some larger particles. The dentinal tubules were totally covered even after the treatment with the lowest concentration of SnF 2 . Deposition of tin- and fluoride-containing globules on dentin surfaces may be of clinical interest. This layer may have importance both for the caries resistance of dentin and for hypersensitivity reactions. (author)

  11. Nuclear microprobe studies of elemental distributions in dormant seeds of Burkea africana

    Witkowski, E. T. F.; Weiersbye-Witkowski, I. M.; Przybyłowicz, W. J.; Mesjasz-Przybyłowicz, J.

    1997-07-01

    Seed nutrient stores are vital post-germination for the establishment of seedlings in harsh and unpredictable environments. Plants of nutrient-poor environments allocate a substantial proportion of total acquired nutrients to reproduction (i.e. seeds). We propose that differential allocation of mineral resources to specific seed tissues is an indication of a species germination and establishment strategy. Burkea africana Hook is a leguminous tree typical of broad-leaved nutrient-poor savannas in southern Africa. Elemental distributions in dormant B. africana seed structures were obtained using the true elemental imaging system (Dynamic Analysis) of the NAC Van de Graaff nuclear microprobe. Raster scans of 3.0 MeV protons were complemented by simultaneous BS and PIXE point analyses. Mineral nutrient concentrations varied greatly between seed tissues. Elevated levels of metals known to play an important role as plant enzyme co-factors were found in the seed lens and embryonic axis. Distributions of most of these metals (Ca, Mn, Fe and Zn, but not K or Cu) were positively correlated with embryonic P distribution, and probably represent phytin deposits. The distribution of metals within seed structures is 'patchy' due to their complexation with P as electron-dense globoid phytin crystals, which constrains the interpretation of PIXE point analyses.

  12. Using Synchrotron X-ray Fluorescence Microprobes in the Study of Metal Homeostasis in Plants

    Punshon, T.; Guerinot, M.; Lanzirotti, A.

    2009-01-01

    Background and Aims: This Botanical Briefing reviews the application of synchrotron X-ray fluorescence (SXRF) microprobes to the plant sciences; how the technique has expanded our knowledge of metal(loid) homeostasis, and how it can be used in the future. Scope: The use of SXRF microspectroscopy and microtomography in research on metal homeostasis in plants is reviewed. The potential use of SXRF as part of the ionomics toolbox, where it is able to provide fundamental information on the way that plants control metal homeostasis, is recommended. Conclusions: SXRF is one of the few techniques capable of providing spatially resolved in-vivo metal abundance data on a sub-micrometre scale, without the need for chemical fixation, coating, drying or even sectioning of samples. This gives researchers the ability to uncover mechanisms of plant metal homeostasis that can potentially be obscured by the artefacts of sample preparation. Further, new generation synchrotrons with smaller beam sizes and more sensitive detection systems will allow for the imaging of metal distribution within single living plant cells. Even greater advances in our understanding of metal homeostasis in plants can be gained by overcoming some of the practical boundaries that exist in the use of SXRF analysis.

  13. Development of an external beam nuclear microprobe on the Aglae facility of the Louvre museum

    Calligaro, T.; Dran, J.-C. E-mail: dran@culture.fr; Ioannidou, E.; Moignard, B.; Pichon, L.; Salomon, J

    2000-03-01

    The external beam line of our facility has been recently equipped with the focusing system previously mounted on a classical nuclear microprobe. When using a 0.1 {mu}m thick Si{sub 3}N{sub 4} foil for the exit window and flowing helium on the sample under analysis, a beam spot as small as 10 {mu}m is attainable at a distance of 3 mm from the window. Elemental micromapping is performed by mechanical scanning. An electronic device has been designed which allows XY scanning by moving the sample under the beam by steps down to 0.1 {mu}m. Beam monitoring is carried out by means of the weak X-ray signal emitted by the exit foil and detected by a specially designed Si(Li) detector cooled by Peltier effect. The characteristics of external beams of protons and alpha particles are evaluated by means of resonance scanning and elemental mapping of a grid. An example of application is presented, dealing with elemental micro-mapping of inclusions in gemstones.

  14. Microprobe PIXE study of Ni–Ge interactions in lateral diffusion couples

    Chilukusha, D. [Department of Physics, University of Zambia, P.O. Box 32379, Lusaka 10101 (Zambia); Pineda-Vargas, C.A. [iThemba LABS, National Research Foundation, P.O. Box 722, Somerset West 7129 (South Africa); Faculty of Health & Wellness Sciences, CPUT, Bellville (South Africa); Nemutudi, R. [iThemba LABS, National Research Foundation, P.O. Box 722, Somerset West 7129 (South Africa); Habanyama, A. [Department of Physics, Copperbelt University, P.O. Box 21692, Jambo Drive, Riverside, Kitwe 10101 (Zambia); Comrie, C.M. [iThemba LABS, National Research Foundation, P.O. Box 722, Somerset West 7129 (South Africa)

    2015-11-15

    Rutherford backscattering spectrometry on the nuclear microprobe (μRBS) is often used in studies of lateral diffusion couples. RBS requires that the positions of the interacting species on the periodic table are not too close in terms of atomic number and therefore do not produce excessive RBS peak overlap. In order to satisfactorily characterize systems that have atomic numbers which are close, it is necessary to find techniques which can complement μRBS. The aim of this study was to determine the extent to which particle induced X-ray emission (PIXE) could be applied in the lateral diffusion couple study of a system with relatively close atomic numbers. This was with a view that it may eventually be adopted to study systems where the atomic numbers are too close for RBS analysis. The system studied here was the Ni–Ge binary system. Since RBS is an established technique for studying lateral diffusion couples, we used it as a standard for comparison. The PIXE results showed a maximum error of 12% with reference to the RBS standard. In order to achieve the most effective use of PIXE in lateral diffusion couple studies we recommend the use of the technique in such a way as to obtain depth information and the use of relatively thick sample layers.

  15. Evaluation of errors for mass-spectrometric analysis with surface-ionization type mass-spectrometer (statistical evaluation of mass-discrimination effect)

    Wada, Y.

    1981-01-01

    The surface-ionization type mass-spectrometer is widely used as an apparatus for quality assurance, accountability and safeguarding of nuclear materials, and for this analysis it has become an important factor to statistically evaluate an analytical error which consists of a random error and a systematic error. The major factor of this systematic error was the mass-discrimination effect. In this paper, various assays for evaluating the factor of variation on the mass-discrimination effect were studied and the data obtained were statistically evaluated. As a result of these analyses, it was proved that the factor of variation on the mass-discrimination effect was not attributed to the acid concentration of sample, sample size on the filament and supplied voltage for a multiplier, but mainly to the filament temperature during the mass-spectrometric analysis. The mass-discrimination effect values β which were usually calculated from the measured data of uranium, plutonium or boron isotopic standard sample were not so significant dependently of the difference of U-235, Pu-239 or B-10 isotopic abundance. Furthermore, in the case of U and Pu, measurement conditions and the mass range of these isotopes were almost similar, and these values β were not statistically significant between U and Pu. On the other hand, the value β for boron was about a third of the value β for U or Pu, but compared with the coefficient of the correction on the mass-discrimination effect for the difference of mass-number, ΔM, these coefficient values were almost the same among U, Pu, and B.As for the isotopic analysis error of U, Pu, Nd and B, it was proved that the isotopic abundance of these elements and the isotopic analysis error were in a relationship of quadratic curves on a logarithmic-logarithmic scale

  16. Quantitative analysis of LISA pathfinder test-mass noise

    Ferraioli, Luigi; Congedo, Giuseppe; Hueller, Mauro; Vitale, Stefano; Hewitson, Martin; Nofrarias, Miquel; Armano, Michele

    2011-01-01

    LISA Pathfinder (LPF) is a mission aiming to test the critical technology for the forthcoming space-based gravitational-wave detectors. The main scientific objective of the LPF mission is to demonstrate test masses free falling with residual accelerations below 3x10 -14 m s -2 /√(Hz) at 1 mHz. Reaching such an ambitious target will require a significant amount of system optimization and characterization, which will in turn require accurate and quantitative noise analysis procedures. In this paper, we discuss two main problems associated with the analysis of the data from LPF: i) excess noise detection and ii) noise parameter identification. The mission is focused on the low-frequency region ([0.1, 10] mHz) of the available signal spectrum. In such a region, the signal is dominated by the force noise acting on test masses. At the same time, the mission duration is limited to 90 days and typical data segments will be 24 hours in length. Considering those constraints, noise analysis is expected to deal with a limited amount of non-Gaussian data, since the spectrum statistics will be far from Gaussian and the lowest available frequency is limited by the data length. In this paper, we analyze the details of the expected statistics for spectral data and develop two suitable excess noise estimators. One is based on the statistical properties of the integrated spectrum, the other is based on the Kolmogorov-Smirnov test. The sensitivity of the estimators is discussed theoretically for independent data, then the algorithms are tested on LPF synthetic data. The test on realistic LPF data allows the effect of spectral data correlations on the efficiency of the different noise excess estimators to be highlighted. It also reveals the versatility of the Kolmogorov-Smirnov approach, which can be adapted to provide reasonable results on correlated data from a modified version of the standard equations for the inversion of the test statistic. Closely related to excess noise

  17. Continuous-flow accelerator mass spectrometry for radiocarbon analysis

    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)

  18. Continuous-flow accelerator mass spectrometry for radiocarbon analysis

    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)

  19. Mass spectrometric analysis of simple hydrogen compounds; Analyse de composes hydrogenes simples au spectrometre de masse

    Nief, C; Botter, R [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires

    1960-07-01

    A uranium furnace is inserted in the gas inlet line of a mass spectrometer between the leak and the source. The line is fed with simple hydrogen compounds (H{sub 2}O, NH{sub 3}, H{sub 2}S) which are in this way reduced to hydrogen gas. Memory effects are largely avoided by heating the sample line to 90 deg. C. The speed of the isotopic analysis is only slightly less than that of hydrogen gas itself; the accuracy is better due to the reduction of fractionating effects in the leak. For the absolute measurements of deuterium in water, the presence of H{sub 3}{sup +} is a problem. Water samples, prepared by mixing an unknown light water sample with different amounts of heavy water, are equilibrated with hydrogen sulphide and analysis of the two phases of each sample enables the zero of the concentration scale to be determined from the point of intersection of the two curves obtained by plotting mixture composition against the observed isotope ratio in the two phases. The whole experiment can be carried out in the apparatus described which analyses hydrogen in H{sub 2}S and H{sub 2}O in the same way. (author) [French] Un four a uranium est insere dans la ligne d'introduction de gaz d'un spectrometre de masse entre la fuite et la source. La ligne est alimentee par des composes hydrogenes simples (H{sub 2}O, NH{sub 3}, H{sub 2}S) qui sont de cette facon transformes en hydrogene gazeux. On evite dans une large mesure les effets de memoire en chauffant la ligne de l'echantillon jusqu'a 90 deg. C. La vitesse de l'analyse isotopique est seulement legerement inferieure a celle de l'hydrogene gazeux lui-meme; la precision est meilleure du fait de la reduction des effets de fractionnement dans la fuite. Pour les mesures absolues du deuterium dans l'eau, la presence de H{sub 3}{sup +} pose un probleme. Les echantillons d'eau, prepares en melangeant un echantillon inconnu d'eau legere a differentes quantites d'eau lourde, sont equilibres par de l'hydrogene sulfure et l'analyse de

  20. Iron distribution in cancer cells following doxorubicin exposure using proton and X-ray synchrotron radiation microprobes

    Ortega, R.; Deves, G.; Bohic, S.; Simionovici, A.; Menez, B.; Bonnin-Mosbah, M.

    2001-01-01

    Chemical studies have shown that doxorubicin, a well-established anticancer agent, is a powerful iron chelator and the resultant iron-drug complex is an efficient catalyst of the conversion of hydrogen peroxide to the highly reactive hydroxyl radical. However, the intracellular complexation of doxorubicin with iron is still debated. Using nuclear microprobe analysis (NMPA), we previously observed in human ovarian cancer cells exposed to 20 μM iodo-doxorubicin (IDX) that iodine and iron cellular distributions were spatially correlated, suggesting a mechanism of intracellular iron chelation by the anthracycline compound. Because maximal plasma drug concentrations in patients are expected to be around 5 μM, NMPA and X-ray absorption near edge spectroscopy (XANES) experiments for iron speciation analysis were performed on cultured cells exposed to pharmacological doses of 2 μM IDX or doxorubicin

  1. Cs+ ion source for secondary ion mass spectrometry

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

    1981-12-01

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

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

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

    2009-01-01

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

  3. Assessment of dye distribution in sensitized solar cells by microprobe techniques

    Barreiros, M.A., E-mail: alexandra.barreiros@lneg.pt [Laboratório Nacional de Energia e Geologia, LEN/UES, Estrada do Paço do Lumiar, 22, 1649-038 Lisboa (Portugal); Corregidor, V. [IPFN, Instituto Superior Técnico, Universidade de Lisboa, E.N. 10, 2686-953 Sacavém (Portugal); Alves, L.C. [C2TN, Campus Tecnológico e Nuclear, Instituto Superior Técnico, Universidade de Lisboa, E.N. 10, 2686-953 Sacavém (Portugal); Guimarães, F. [Laboratório Nacional de Energia e Geologia, LGM/UCTM, Rua da Amieira, Apartado 1089, 4466-901 S. Mamede de Infesta (Portugal); Mascarenhas, J.; Torres, E.; Brites, M.J. [Laboratório Nacional de Energia e Geologia, LEN/UES, Estrada do Paço do Lumiar, 22, 1649-038 Lisboa (Portugal)

    2015-04-01

    Dye sensitized solar cells (DSCs) have received considerable attention once this technology offers economic and environmental advantages over conventional photovoltaic (PV) devices. The PV performance of a DSC relies on the characteristics of its photoanode, which typically consists of a nanocrystalline porous TiO{sub 2} film, enabled with a large adsorptive surface area. Dye molecules that capture photons from light during device operation are attached to the film nanoparticles. The effective loading of the dye in the TiO{sub 2} electrode is of paramount relevance for controlling and optimizing solar cell parameters. Relatively few methods are known today for quantitative evaluation of the total dye adsorbed on the film. In this context, microprobe techniques come out as suitable tools to evaluate the dye surface distribution and depth profile in sensitized films. Electron Probe Microanalysis (EPMA) and Ion Beam Analytical (IBA) techniques using a micro-ion beam were used to quantify and to study the distribution of the Ru organometallic dye in TiO{sub 2} films, making use of the different penetration depth and beam sizes of each technique. Different 1D nanostructured TiO{sub 2} films were prepared, morphologically characterized by SEM, sensitized and analyzed by the referred techniques. Dye load evaluation in different TiO{sub 2} films by three different techniques (PIXE, RBS and EPMA/WDS) provided similar results of Ru/Ti mass fraction ratio. Moreover, it was possible to assess dye surface distribution and its depth profile, by means of Ru signal, and to visualize the dye distribution in sample cross-section through X-ray mapping by EPMA/EDS. PIXE maps of Ru and Ti indicated an homogeneous surface distribution. The assessment of Ru depth profile by RBS showed that some films have homogeneous Ru depth distribution while others present different Ru concentration in the top layer (2 μm thickness). These results are consistent with the EPMA/EDS maps obtained.

  4. Core Community Specifications for Electron Microprobe Operating Systems: Software, Quality Control, and Data Management Issues

    Fournelle, John; Carpenter, Paul

    2006-01-01

    Modem electron microprobe systems have become increasingly sophisticated. These systems utilize either UNIX or PC computer systems for measurement, automation, and data reduction. These systems have undergone major improvements in processing, storage, display, and communications, due to increased capabilities of hardware and software. Instrument specifications are typically utilized at the time of purchase and concentrate on hardware performance. The microanalysis community includes analysts, researchers, software developers, and manufacturers, who could benefit from exchange of ideas and the ultimate development of core community specifications (CCS) for hardware and software components of microprobe instrumentation and operating systems.

  5. Mapping of trace elements with photon microprobes: x-ray fluorescence with focussed synchrotron radiation

    Hanson, A.L.; Jones, K.W.; Gordon, B.M.; Pounds, J.G.; Rivers, M.L.; Schidlovsky, G.

    1985-04-01

    High energy electron synchrotron storage rings provide copious quantities of polarized photons that make possible the mapping of many trace elements with sensitivities at the parts per billion (ppB) level with spatial resolutions in the micrometer range. The brightness of the x-ray ring of the National Synchrotron Light Source (NSLS), presently being commissioned, will be five orders of magnitude larger than that of the bremsstrahlung spectrum of state-of-the-art rotating anode tubes. We will discuss mapping trace elements with a photon microprobe presently being constructed for use at the NSLS. This microprobe will have micrometer spatial resolution

  6. An x-ray microprobe using focussing optics with a synchrotron radiation source

    Thompson, A.C.; Underwood, J.H.; Wu, Y.; Giauque, R.D.

    1989-01-01

    An x-ray microprobe can be used to produce maps of the concentration of elements in a sample. Synchrotron radiation provides x-ray beams with enough intensity and collimation to make possible elemental images with femtogram sensitivity. The use of focussing x-ray mirrors made from synthetic multilayers with a synchrotron x-ray beam allows beam spot sizes of less than 10 μm /times/ 10 μm to be produced. Since minimal sample preparation is required and a vacuum environment is not necessary, there will be a wide variety of applications for such microprobes. 8 refs., 6 figs

  7. The PNC/XOR x-ray microprobe station at APS sector 20

    Heald, S. M.; Cross, J. O.; Brewe, D. L.; Gordon, R. A.

    2007-01-01

    The X-ray microprobe is the most popular experimental setup at the PNC/XOR insertion device beamline located at sector 20 at the Advanced Photon Source. To satisfy user demand and to simplify the setup, we have developed a dedicated station with multiple detection options. This paper will describe the setup in detail and demonstrate the capabilities with some example imaging, micro-XAS and microdiffraction data. In the future, an improved version of the microprobe will be installed on a dedicated undulator. The improvements planned for this station are based on our operational experience and will also be discussed

  8. Polymer SU-8 Based Microprobes for Neural Recording and Drug Delivery

    Altuna, Ane; Fernandez, Luis; Berganzo, Javier

    2015-06-01

    This manuscript makes a reflection about SU-8 based microprobes for neural activity recording and drug delivery. By taking advantage of improvements in microfabrication technologies and using polymer SU-8 as the only structural material, we developed several microprobe prototypes aimed to: a) minimize injury in neural tissue, b) obtain high-quality electrical signals and c) deliver drugs at a micrometer precision scale. Dedicated packaging tools have been developed in parallel to fulfill requirements concerning electric and fluidic connections, size and handling. After these advances have been experimentally proven in brain using in vivo preparation, the technological concepts developed during consecutive prototypes are discussed in depth now.

  9. POLYMER SU-8 BASED MICROPROBES FOR NEURAL RECORDING AND DRUG DELIVERY

    Ane eAltuna

    2015-06-01

    Full Text Available This manuscript makes a reflection about SU-8 based microprobes for neural activity recording and drug delivery. By taking advantage of improvements in microfabrication technologies and using polymer SU-8 as the only structural material, we developed several microprobe prototypes aimed to: a minimize injury in neural tissue, b obtain high-quality electrical signals and c deliver drugs at a micrometer precision scale. Dedicated packaging tools have been developed in parallel to fulfill requirements concerning electric and fluidic connections, size and handling. After these advances have been experimentally proven in brain using in vivo preparation, the technological concepts developed during consecutive prototypes are discussed in depth now.

  10. Theory of equidistant three-dimensional radiance measurements with optical microprobes RID A-1977-2009

    FukshanskyKazarinova, N.; Fukshansky, L.; Kuhl, Morten

    1996-01-01

    Fiber-optic radiance microprobes, increasingly applied for measurements of internal light fields in living tissues, provide three-dimensional radiance distribution solids and radiant energy fluence rates at different depths of turbid samples. These data are, however, distorted because of an inher...... of application is presented. The limitations of this theory and the prospects for this approach are discussed....... of an inherent feature of optical fibers: nonuniform angular sensitivity. Because of this property a radiance microprobe during a single measurement partly underestimates light from the envisaged direction and partly senses light from other directions. A theory of three-dimensional equidistant radiance...

  11. Analysis on one underground nuclear waste repository rock mass in USA

    Ha Qiuling; Zhang Tiantian

    2012-01-01

    When analyzing the rock mass of a underground nuclear waste repository, the current studies are all based on the loading mechanical condition, and the unloading damage of rock mass is unconsidered. According to the different mechanical condition of actual engineering rock mass of loading and unloading, this paper implements a comprehensive analysis on the rock mass deformation of underground nuclear waste repository through the combination of present loading and unloading rock mass mechanics. It is found that the results of comprehensive analysis and actual measured data on the rock mass deformation of underground nuclear waste repository are basically the same, which provide supporting data for the underground nuclear waste repository. (authors)

  12. Australian Mass Shootings: An Analysis of Incidents and Offenders.

    McPhedran, Samara

    2017-06-01

    Mass shooting events are relatively underresearched, and most study comes from the United States. Despite significant international interest, little is known about other countries' experiences of these events. The current study examines Australian mass shooting incidents and offenders, with emphasis on mental illness, life strains, and offenders' life histories. Australia had 14 mass shootings between 1964 and 2014. Most offenders experienced acute life stressors and/or chronic strains leading up to the event; however, diagnosed mental illness was less commonly documented. These observations provide new information about mass shooting incidents and offenders, and can help to inform international policy development.

  13. Second Law Analysis in Convective Heat and Mass Transfer

    A. Ben Brahim

    2006-02-01

    Full Text Available This paper reports the numerical determination of the entropy generation due to heat transfer, mass transfer and fluid friction in steady state for laminar double diffusive convection, in an inclined enclosure with heat and mass diffusive walls, by solving numerically the mass, momentum, species conservation and energy balance equations, using a Control Volume Finite-Element Method. The influences of the inclination angle, the thermal Grashof number and the buoyancy ratio on total entropy generation were investigated. The irreversibilities localization due to heat transfer, mass transfer and fluid friction is discussed for three inclination angles at a fixed thermal Grashof number.

  14. Vehicle Lightweighting: Mass Reduction Spectrum Analysis and Process Cost Modeling

    Mascarin, Anthony [IBIS Associates, Inc., Waltham, MA (United States); Hannibal, Ted [IBIS Associates, Inc., Waltham, MA (United States); Raghunathan, Anand [Energetics Inc., Columbia, MD (United States); Ivanic, Ziga [Energetics Inc., Columbia, MD (United States); Clark, Michael [Idaho National Lab. (INL), Idaho Falls, ID (United States)

    2016-03-01

    The U.S. Department of Energy’s Vehicle Technologies Office, Materials area commissioned a study to model and assess manufacturing economics of alternative design and production strategies for a series of lightweight vehicle concepts. In the first two phases of this effort examined combinations of strategies aimed at achieving strategic targets of 40% and a 45% mass reduction relative to a standard North American midsize passenger sedan at an effective cost of $3.42 per pound (lb) saved. These results have been reported in the Idaho National Laboratory report INL/EXT-14-33863 entitled Vehicle Lightweighting: 40% and 45% Weight Savings Analysis: Technical Cost Modeling for Vehicle Lightweighting published in March 2015. The data for these strategies were drawn from many sources, including Lotus Engineering Limited and FEV, Inc. lightweighting studies, U.S. Department of Energy-funded Vehma International of America, Inc./Ford Motor Company Multi-Material Lightweight Prototype Vehicle Demonstration Project, the Aluminum Association Transportation Group, many United States Council for Automotive Research’s/United States Automotive Materials Partnership LLC lightweight materials programs, and IBIS Associates, Inc.’s decades of experience in automotive lightweighting and materials substitution analyses.

  15. Vehicle Lightweighting: Mass Reduction Spectrum Analysis and Process Cost Modeling

    Mascarin, Anthony; Hannibal, Ted; Raghunathan, Anand; Ivanic, Ziga; Clark, Michael

    2016-01-01

    The U.S. Department of Energy's Vehicle Technologies Office, Materials area commissioned a study to model and assess manufacturing economics of alternative design and production strategies for a series of lightweight vehicle concepts. In the first two phases of this effort examined combinations of strategies aimed at achieving strategic targets of 40% and a 45% mass reduction relative to a standard North American midsize passenger sedan at an effective cost of $3.42 per pound (lb) saved. These results have been reported in the Idaho National Laboratory report INL/EXT-14-33863 entitled Vehicle Lightweighting: 40% and 45% Weight Savings Analysis: Technical Cost Modeling for Vehicle Lightweighting published in March 2015. The data for these strategies were drawn from many sources, including Lotus Engineering Limited and FEV, Inc. lightweighting studies, U.S. Department of Energy-funded Vehma International of America, Inc./Ford Motor Company Multi-Material Lightweight Prototype Vehicle Demonstration Project, the Aluminum Association Transportation Group, many United States Council for Automotive Research's/United States Automotive Materials Partnership LLC lightweight materials programs, and IBIS Associates, Inc.'s decades of experience in automotive lightweighting and materials substitution analyses.

  16. Atmospheric pressure plasma analysis by modulated molecular beam mass spectrometry

    Aranda Gonzalvo, Y.; Whitmore, T.D.; Rees, J.A.; Seymour, D.L.; Stoffels - Adamowicz, E.

    2006-01-01

    Fractional no. d. measurements for a radiofrequency plasma needle operating at atm. pressure were obtained using a mol. beam mass spectrometer (MBMS) system designed for diagnostics of atm. plasmas. The MBMS system comprises three differentially pumped stages and a mass/energy analyzer and includes

  17. Quantifying trace elements in individual aquatic protist cells with a synchrotron x-ray fluorescence microprobe

    Twining, B.S.; Baines, S.B.; Fisher, N.S.; Maser, J.; Vogt, S.; Jacobsen, C.; Tovar-Sanchez, A.; Sanudo-Wihelmy, S.A.

    2003-01-01

    The study of trace metal cycling by aquatic protists is limited by current analytical techniques. Standard 'bulk' element analysis techniques that rely on physical separations to concentrate cells for analysis cannot separate cells from co-occurring detrital material or other cells of differing taxonomy or trophic function. Here we demonstrate the ability of a synchrotron-based X-ray fluorescence (SXRF) microprobe to quantify the elements Si, Mn, Fe, Ni, and Zn in individual aquatic protist cells. This technique distinguishes between different types of cells in an assemblage and between cells and other particulate matter. Under typical operating conditions, the minimum detection limits are 7.0 x 10 -16 mol μm -2 for Si and between 5.0 x 10 -20 and 3.9 x 10 -19 mol μm -2 for Mn, Fe, Ni, and Zn; this sensitivity is sufficient to detect these elements in cells from even the most pristine waters as demonstrated in phytoplankton cells collected from remote areas of the Southern Ocean. Replicate analyses of single cells produced variations of <5% for Si, Mn, Fe, and Zn and <10% for Ni. Comparative analyses of cultured phytoplankton cells generally show no significant differences in cellular metal concentrations measured with SXRF and standard bulk techniques (spectrophotometry and graphite furnace atomic absorption spectrometry). SXRF also produces two-dimensional maps of element distributions in cells, thereby providing information not available with other analytical approaches. This technique enables the accurate and precise measurement of trace metals in individual aquatic protists collected from natural environments.

  18. Analysis of fall injuries by body mass index.

    Ren, Jun; Waclawczyk, Amanda; Hartfield, Doug; Yu, Shicheng; Kuang, Xiangyu; Zhang, Hongrui; Alamgir, Hasanat

    2014-05-01

    To examine the association of body mass index (BMI) and fall injuries. Data were derived from the 2010 Behavioral Risk Factor Surveillance System and included subjects aged 45 years and older from Texas. The outcome was self-reported falls that resulted in injury to the respondents. Analysis of fall injuries by BMI was conducted and standard errors, 95% confidence intervals (CIs), and coefficients of variation were reported. Complex sample multivariate Poisson regression was used to examine the association of BMI and fall injuries. A total of 18,077 subjects were surveyed in 2010, and 13,235 subjects were aged 45 years old and older. The mean BMI was higher (29.94 vs 28.32 kg/m(2)) among those who reported fall injuries compared with those who did not. The fall injuries reported by obese respondents (relative risk [RR] 1.67) were found to be significantly (P = 0.031) higher compared with normal-weight respondents in the multivariate regression. Other risk factors that had significant association with fall injuries (when adjusted for BMI) were activity limitations (RR 5.00, 95% CI 3.36-7.46) compared with no limitations, and not having formal employment (homemaker: RR 2.68, 95% CI 1.33-5.37; unable to work: RR 5.01, 95% CI 1.87-13.29; out of work and students: RR 3.21, 95% CI 1.41-7.29) compared with the employed population. There is a significant association between obesity and fall injuries in adults aged 45 years old and older in Texas. Interventions in fall prevention, although generally targeted at present to older adults, also should take into account the weight status of the subjects.

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

    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.

  20. Round robin: Quantitative lateral resolution of PHI XPS microprobes Quantum 2000/Quantera SXM

    Scheithauer, Uwe; Kolb, Max; Kip, Gerard A.M.; Naburgh, Emile; Snijders, J.H.M.

    2016-01-01

    Highlights: • The quantitative lateral resolution of 7 PHI XPS microprobes has been estimated in a round robin. • An ellipsoidally shaped quartz crystal monochromatizes the Alkα radiation and refocuses it from the Al anode to the sample surface. • The long tail contributions of the X-ray beam intensity distribution were measured using a new and innovative approach. • This quantitative lateral resolution has a significantly larger value than the nominal X-ray beam diameter. • The quantitative lateral resolution follows a trend in time: The newer the monochromator so much the better the quantitative lateral resolution. - Abstract: The quantitative lateral resolution is a reliable measure for the quality of an XPS microprobe equipped with a focused X-ray beam. It describes the long tail contributions of the X-ray beam intensity distribution. The knowledge of these long tail contributions is essential when judging on the origin of signals of XPS spectra recorded on small-sized features. In this round robin test the quantitative lateral resolution of 7 PHI XPS microprobes has been estimated. As expected, the quantitative lateral resolution has significantly larger values than the nominal X-ray beam diameter. The estimated values of the quantitative lateral resolution follow a trend in time: the newer the monochromator of an XPS microprobe so much the better the quantitative lateral resolution.

  1. Round robin: Quantitative lateral resolution of PHI XPS microprobes Quantum 2000/Quantera SXM

    Scheithauer, Uwe, E-mail: scht.uhg@googlemail.com [82008 Unterhaching (Germany); Kolb, Max, E-mail: max.kolb@airbus.com [Airbus Group Innovations, TX2, 81663 Munich (Germany); Kip, Gerard A.M., E-mail: G.A.M.Kip@utwente.nl [Universiteit Twente, MESA+ Nanolab, Postbus 217, 7500AE Enschede (Netherlands); Naburgh, Emile, E-mail: e.p.naburgh@philips.com [Materials Analysis, Philips Innovation Services, High Tech Campus 11, 5656 AE Eindhoven (Netherlands); Snijders, J.H.M., E-mail: j.h.m.snijders@philips.com [Materials Analysis, Philips Innovation Services, High Tech Campus 11, 5656 AE Eindhoven (Netherlands)

    2016-07-15

    Highlights: • The quantitative lateral resolution of 7 PHI XPS microprobes has been estimated in a round robin. • An ellipsoidally shaped quartz crystal monochromatizes the Alkα radiation and refocuses it from the Al anode to the sample surface. • The long tail contributions of the X-ray beam intensity distribution were measured using a new and innovative approach. • This quantitative lateral resolution has a significantly larger value than the nominal X-ray beam diameter. • The quantitative lateral resolution follows a trend in time: The newer the monochromator so much the better the quantitative lateral resolution. - Abstract: The quantitative lateral resolution is a reliable measure for the quality of an XPS microprobe equipped with a focused X-ray beam. It describes the long tail contributions of the X-ray beam intensity distribution. The knowledge of these long tail contributions is essential when judging on the origin of signals of XPS spectra recorded on small-sized features. In this round robin test the quantitative lateral resolution of 7 PHI XPS microprobes has been estimated. As expected, the quantitative lateral resolution has significantly larger values than the nominal X-ray beam diameter. The estimated values of the quantitative lateral resolution follow a trend in time: the newer the monochromator of an XPS microprobe so much the better the quantitative lateral resolution.

  2. Characterization of Alq3 thin films by a near-field microwave microprobe.

    Hovsepyan, Artur; Lee, Huneung; Sargsyan, Tigran; Melikyan, Harutyun; Yoon, Youngwoon; Babajanyan, Arsen; Friedman, Barry; Lee, Kiejin

    2008-09-01

    We observed tris-8-hydroxyquinoline aluminum (Alq3) thin films dependence on substrate heating temperatures by using a near-field microwave microprobe (NFMM) and by optical absorption at wavelengths between 200 and 900 nm. The changes of absorption intensity at different substrate heating temperatures are correlated to the changes in the sheet resistance of Alq3 thin films.

  3. Scanning deep level transient spectroscopy using an MeV ion microprobe

    Laird, J S; Bardos, R A; Saint, A; Moloney, G M; Legge, G F.J. [Melbourne Univ., Parkville, VIC (Australia)

    1994-12-31

    Traditionally the scanning ion microprobe has given little or no information regarding the electronic structure of materials in particular semiconductors. A new imaging technique called Scanning Ion Deep Level Transient Spectroscopy (SIDLTS) is presented which is able to spatially map alterations in the band gap structure of materials by lattice defects or impurities. 3 refs., 2 figs.

  4. Scanning deep level transient spectroscopy using an MeV ion microprobe

    Laird, J.S.; Bardos, R.A.; Saint, A.; Moloney, G.M.; Legge, G.F.J. [Melbourne Univ., Parkville, VIC (Australia)

    1993-12-31

    Traditionally the scanning ion microprobe has given little or no information regarding the electronic structure of materials in particular semiconductors. A new imaging technique called Scanning Ion Deep Level Transient Spectroscopy (SIDLTS) is presented which is able to spatially map alterations in the band gap structure of materials by lattice defects or impurities. 3 refs., 2 figs.

  5. Developments of new generation nuclear microprobe systems at the University of Melbourne

    Rout, B.; Jamieson, D.N.; Hopt, R.; Hearne, S.; Szymaski, R.

    2002-01-01

    Full text: A review of the recent developments in fabricating a new generation nuclear microprobe systems at University of Melbourne, Melbourne, will be presented. These new generation systems present high spatial resolution (less than 1 micrometer) with increasing current density (in excess of 100 pA/micrometer 2 ) of the probing ion beam. Detectors with large solid angles and high brightness of the ion source of the accelerator increase the capabilities of these microprobes many fold. Some of the key ingredients of these microprobes are (i) novel magnetic quadrupole lens quintuplet probe forming system (ii) integrated fast data acquisition system to handle high count rates (excess of 100 KHz) due to increasing current density as well as large detector solid angles up to 4 detector stations. Full dead time corrected and charge normalised maps are also implemented to counter the problems normally associated with such high count rate systems. First version of these systems is presently under operation at CSIRO, Sydney. Another similar system is currently being installed at Dutch Institute for Nuclear and High Energy Physics, Amsterdam, Netherlands. A further optimised version of the CSIRO/MARC quintuplet probe forming systems is currently being fabricated at University of Melbourne. Some of the applications involve microelectronic materials, superconductors and geological samples. We will be presenting exciting results arising out of investigations into these materials. We will be demonstrating ultimate spatial resolution of the new microprobe being fabricated at Melbourne

  6. Gas Chromatography-Mass Spectrometric Analysis and Insecticidal ...

    Tropical Journal of Pharmaceutical Research ... apelta aerial parts was analyzed by gas chromatography/mass spectrometric (GC/MS) to determine its composition. ... into a natural fumigant/insecticide for the control of stored product insects.

  7. Genome-wide association analysis identifies three new susceptibility loci for childhood body mass index

    J.F. Felix (Janine); J.P. Bradfield (Jonathan); C. Monnereau; R.J.P. van der Valk (Ralf); E. Stergiakouli (Evie); A. Chesi (Alessandra); R. Gaillard (Romy); B. Feenstra (Bjarke); E. Thiering (Elisabeth); E. Kreiner-Møller (Eskil); A. Mahajan (Anubha); Niina Pitkänen; R. Joro (Raimo); A. Cavadino (Alana); V. Huikari (Ville); S. Franks (Steve); M. Groen-Blokhuis (Maria); D.L. Cousminer (Diana); J.A. Marsh (Julie); T. Lehtimäki (Terho); J.A. Curtin (John); J. Vioque (Jesus); T.S. Ahluwalia (Tarunveer Singh); R. Myhre (Ronny); T.S. Price (Thomas); Natalia Vilor-Tejedor; L. Yengo (Loic); N. Grarup (Niels); I. Ntalla (Ioanna); W.Q. Ang (Wei); M. Atalay (Mustafa); H. Bisgaard (Hans); A.I.F. Blakemore (Alexandra); A. Bonnefond (Amélie); L. Carstensen (Lisbeth); J.G. Eriksson (Johan G.); C. Flexeder (Claudia); L. Franke (Lude); F. Geller (Frank); M. Geserick (Mandy); A.L. Hartikainen; C.M.A. Haworth (Claire M.); J.N. Hirschhorn (Joel N.); A. Hofman (Albert); J.-C. Holm (Jens-Christian); M. Horikoshi (Momoko); J.J. Hottenga (Jouke Jan); J. Huang (Jian); H.N. Kadarmideen (Haja N.); M. Kähönen (Mika); W. Kiess (Wieland); T.A. Lakka (Timo); T.A. Lakka (Timo); A. Lewin (Alex); L. Liang (Liming); L.-P. Lyytikäinen (Leo-Pekka); B. Ma (Baoshan); P. Magnus (Per); S.E. McCormack (Shana E.); G. Mcmahon (George); F.D. Mentch (Frank); C.M. Middeldorp (Christel); C.S. Murray (Clare S.); K. Pahkala (Katja); T.H. Pers (Tune); R. Pfäffle (Roland); D.S. Postma (Dirkje); C. Power (Christine); A. Simpson (Angela); V. Sengpiel (Verena); C. Tiesler (Carla); M. Torrent (Maties); A.G. Uitterlinden (André); J.B.J. van Meurs (Joyce); R. Vinding (Rebecca); J. Waage (Johannes); J. Wardle (Jane); E. Zeggini (Eleftheria); B.S. Zemel (Babette S.); G.V. Dedoussis (George); O. Pedersen (Oluf); P. Froguel (Philippe); J. Sunyer (Jordi); R. Plomin (Robert); B. Jacobsson (Bo); T. Hansen (Torben); J.R. Gonzalez (Juan R.); A. Custovic; O.T. Raitakari (Olli T.); C.E. Pennell (Craig); Elisabeth Widén; D.I. Boomsma (Dorret); G.H. Koppelman (Gerard); S. Sebert (Sylvain); M.-R. Jarvelin (Marjo-Riitta); E. Hypponen (Elina); M.I. McCarthy (Mark); V. Lindi (Virpi); N. Harri (Niinikoski); A. Körner (Antje); K. Bønnelykke (Klaus); J. Heinrich (Joachim); M. Melbye (Mads); F. Rivadeneira Ramirez (Fernando); H. Hakonarson (Hakon); S.M. Ring (Susan); G.D. Smith; T.I.A. Sørensen (Thorkild I.A.); N.J. Timpson (Nicholas); S.F.A. Grant (Struan); V.W.V. Jaddoe (Vincent); H.J. Kalkwarf (Heidi J.); J.M. Lappe (Joan M.); V. Gilsanz (Vicente); S.E. Oberfield (Sharon E.); J.A. Shepherd (John A.); A. Kelly (Andrea)

    2016-01-01

    textabstractA large number of genetic loci are associated with adult body mass index. However, the genetics of childhood body mass index are largely unknown.We performed a meta-analysis of genome-wide association studies of childhood body mass index, using sex- and age-adjusted standard deviation

  8. Electrospray Ionization Mass Spectrometric Analysis of Highly Reactive Glycosyl Halides

    Lajos Kovács

    2012-07-01

    Full Text Available Highly reactive glycosyl chlorides and bromides have been analysed by a routine mass spectrometric method using electrospray ionization and lithium salt adduct-forming agents in anhydrous acetonitrile solution, providing salient lithiated molecular ions [M+Li]+, [2M+Li]+ etc. The role of other adduct-forming salts has also been evaluated. The lithium salt method is useful for accurate mass determination of these highly sensitive compounds.

  9. Subcellular analysis by laser ablation electrospray ionization mass spectrometry

    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.

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

    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

  11. Laser ionization time of flight mass spectrometer for isotope mass detection and elemental analysis of materials

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

    2017-08-01

    In this paper we present the construction and modification of a linear time-of-flight mass spectrometer to improve its mass resolution. This system consists of a laser ablation/ionization section based on a Q-switched Nd:YAG laser (532 nm, 500 mJ, 5 ns pulse duration) integrated with a one meter linear time-of-flight mass spectrometer coupled with an electric sector and a magnetic lens and outfitted with a channeltron electron multiplier for ion detection. The resolution of the system has been improved by optimizing the accelerating potential and inserting a magnetic lens after the extraction region. The isotopes of lithium, lead and cadmium samples have been resolved and detected in accordance with their natural abundance. The capability of the system has been further exploited to determine the elemental composition of a brass alloy, having a certified composition of zinc and copper. Our results are in excellent agreement with its certified composition. This setup is found to be extremely efficient and convenient for fast analyses of any solid sample.

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

    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 ...

  13. CALCMIN - an EXCEL™ Visual Basic application for calculating mineral structural formulae from electron microprobe analyses

    Brandelik, Andreas

    2009-07-01

    CALCMIN, an open source Visual Basic program, was implemented in EXCEL™. The program was primarily developed to support geoscientists in their routine task of calculating structural formulae of minerals on the basis of chemical analysis mainly obtained by electron microprobe (EMP) techniques. Calculation programs for various minerals are already included in the form of sub-routines. These routines are arranged in separate modules containing a minimum of code. The architecture of CALCMIN allows the user to easily develop new calculation routines or modify existing routines with little knowledge of programming techniques. By means of a simple mouse-click, the program automatically generates a rudimentary framework of code using the object model of the Visual Basic Editor (VBE). Within this framework simple commands and functions, which are provided by the program, can be used, for example, to perform various normalization procedures or to output the results of the computations. For the clarity of the code, element symbols are used as variables initialized by the program automatically. CALCMIN does not set any boundaries in complexity of the code used, resulting in a wide range of possible applications. Thus, matrix and optimization methods can be included, for instance, to determine end member contents for subsequent thermodynamic calculations. Diverse input procedures are provided, such as the automated read-in of output files created by the EMP. Furthermore, a subsequent filter routine enables the user to extract specific analyses in order to use them for a corresponding calculation routine. An event-driven, interactive operating mode was selected for easy application of the program. CALCMIN leads the user from the beginning to the end of the calculation process.

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

    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

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

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

    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....

  17. A novel technique for producing antibody-coated microprobes using a thiol-terminal silane and a heterobifunctional crosslinker.

    Routh, V H; Helke, C J

    1997-02-01

    Antibody-coated microprobes are used to measure neuropeptide release in the central nervous system. Although they are not quantitative, they provide the most precise spatial resolution of the location of in vivo release of any currently available method. Previous methods of coating antibody microprobes are difficult and time-consuming. Moreover, using these methods we were unable to produce evenly coated antibody microprobes. This paper describes a novel method for the production of antibody microprobes using thiol-terminal silanes and the heterobifunctional crosslinker, 4-(4-N-maleimidophenyl)butyric acid hydrazide HCl 1/2 dioxane (MPBH). Following silation, glass micropipettes are incubated with antibody to substance P (SP) that has been conjugated to MPBH. This method results in a dense, even coating of antibody without decreasing the biological activity of the antibody. Additionally, this method takes considerably less time than previously described methods without sacrificing the use of antibody microprobes as micropipettes. The sensitivity of the microprobes for SP is in the picomolar range, and there is a linear correlation between the log of SP concentration (M) and B/B0 (r2 = 0.98). The microprobes are stable for up to 3 weeks when stored in 0.1 M sodium phosphate buffer with 50 mM NaCl (pH 7.4) at 5 degrees C. Finally, insertion into the exposed spinal cord of an anesthetized rat for 15 min produces no damage to the antibody coating.

  18. Mass analysis of charged aerosol particles in NLC and PMSE during the ECOMA/MASS campaign

    S. Robertson

    2009-03-01

    Full Text Available MASS (Mesospheric Aerosol Sampling Spectrometer is a multichannel mass spectrometer for charged aerosol particles, which was flown from the Andøya Rocket Range, Norway, through NLC and PMSE on 3 August 2007 and through PMSE on 6 August 2007. The eight-channel analyzers provided for the first time simultaneous measurements of the charge density residing on aerosol particles in four mass ranges, corresponding to ice particles with radii <0.5 nm (including ions, 0.5–1 nm, 1–2 nm, and >3 nm (approximately. Positive and negative particles were recorded on separate channels. Faraday rotation measurements provided electron density and a means of checking charge density measurements made by the spectrometer. Additional complementary measurements were made by rocket-borne dust impact detectors, electric field booms, a photometer and ground-based radar and lidar. The MASS data from the first flight showed negative charge number densities of 1500–3000 cm−3 for particles with radii >3 nm from 83–88 km approximately coincident with PMSE observed by the ALWIN radar and NLC observed by the ALOMAR lidar. For particles in the 1–2 nm range, number densities of positive and negative charge were similar in magnitude (~2000 cm−3 and for smaller particles, 0.5–1 nm in radius, positive charge was dominant. The occurrence of positive charge on the aerosol particles of the smallest size and predominately negative charge on the particles of largest size suggests that nucleation occurs on positive condensation nuclei and is followed by collection of negative charge during subsequent growth to larger size. Faraday rotation measurements show a bite-out in electron density that increases the time for positive aerosol particles to be neutralized and charged negatively. The larger particles (>3 nm are observed throughout the NLC region, 83–88 km, and the smaller particles are observed primarily at the high end of the range, 86–88 km

  19. Mass analysis of charged aerosol particles in NLC and PMSE during the ECOMA/MASS campaign

    S. Robertson

    2009-03-01

    Full Text Available MASS (Mesospheric Aerosol Sampling Spectrometer is a multichannel mass spectrometer for charged aerosol particles, which was flown from the Andøya Rocket Range, Norway, through NLC and PMSE on 3 August 2007 and through PMSE on 6 August 2007. The eight-channel analyzers provided for the first time simultaneous measurements of the charge density residing on aerosol particles in four mass ranges, corresponding to ice particles with radii <0.5 nm (including ions, 0.5–1 nm, 1–2 nm, and >3 nm (approximately. Positive and negative particles were recorded on separate channels. Faraday rotation measurements provided electron density and a means of checking charge density measurements made by the spectrometer. Additional complementary measurements were made by rocket-borne dust impact detectors, electric field booms, a photometer and ground-based radar and lidar. The MASS data from the first flight showed negative charge number densities of 1500–3000 cm−3 for particles with radii >3 nm from 83–88 km approximately coincident with PMSE observed by the ALWIN radar and NLC observed by the ALOMAR lidar. For particles in the 1–2 nm range, number densities of positive and negative charge were similar in magnitude (~2000 cm−3 and for smaller particles, 0.5–1 nm in radius, positive charge was dominant. The occurrence of positive charge on the aerosol particles of the smallest size and predominately negative charge on the particles of largest size suggests that nucleation occurs on positive condensation nuclei and is followed by collection of negative charge during subsequent growth to larger size. Faraday rotation measurements show a bite-out in electron density that increases the time for positive aerosol particles to be neutralized and charged negatively. The larger particles (>3 nm are observed throughout the NLC region, 83–88 km, and the smaller particles are observed primarily at the high end of the range, 86–88 km. The second flight into

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

    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

  1. Mass spectral analysis of cationic and neutral technetium complexes

    Unger, S.E.; McCormick, T.J.; Nunn, A.N.; Treher, E.N.

    1986-01-01

    Cationic and neutral technetium compounds have been characterized by mass spectrometry using a variety of ionization methods. These compounds include octahedral cationic complexes containing phosphorous and arsenic ligands such as DIPHOS and DIARS and neutral complexes containing PnAO and dimethylglyoxime, DMG, or cyclohexanedione dioxime, CDO, ligands. Boronate esters incorporating methyl and butyl derivatives of the DMG and CDO dioximes represent a new class of seven-coordinate Tc radiopharmaceuticals whose characterization by mass spectrometry has not previously been described. These complexes show promise as myocardial imaging agents. (author)

  2. Comparative Analysis of Mass Spectral Similarity Measures on Peak Alignment for Comprehensive Two-Dimensional Gas Chromatography Mass Spectrometry

    2013-01-01

    Peak alignment is a critical procedure in mass spectrometry-based biomarker discovery in metabolomics. One of peak alignment approaches to comprehensive two-dimensional gas chromatography mass spectrometry (GC×GC-MS) data is peak matching-based alignment. A key to the peak matching-based alignment is the calculation of mass spectral similarity scores. Various mass spectral similarity measures have been developed mainly for compound identification, but the effect of these spectral similarity measures on the performance of peak matching-based alignment still remains unknown. Therefore, we selected five mass spectral similarity measures, cosine correlation, Pearson's correlation, Spearman's correlation, partial correlation, and part correlation, and examined their effects on peak alignment using two sets of experimental GC×GC-MS data. The results show that the spectral similarity measure does not affect the alignment accuracy significantly in analysis of data from less complex samples, while the partial correlation performs much better than other spectral similarity measures when analyzing experimental data acquired from complex biological samples. PMID:24151524

  3. Risk Analysis of Loblolly Pine Controlled Mass Pollination Program

    T.D. Byram; F.E. Bridgwater

    1999-01-01

    The economic success of controlled mass pollination (CMP) depends both upon the value of the genetic gain obtained and the cost per seed. Crossing the best six loblolly pine (Pinus taeda) parents currently available in each deployment region of the Western Gulf Forest Tree Improvement Program will produce seed with an average additional gain in mean...

  4. Mass transfer analysis for terephthalic acid biodegradation by ...

    Biodegradation of terephthalic acid (TA) by polyvinyl alcohol (PVA)-alginate immobilized Pseudomonas sp. was carried out in a packed-bed reactor. The effect of inlet TA concentration on biodegradation was investigated at 30°C, pH 7 and flow rate of 20 ml/min. The effects of flow rate on mass transfer and biodegradation ...

  5. Objective Bayesian analysis of neutrino masses and hierarchy

    Heavens, Alan F.; Sellentin, Elena

    2018-04-01

    Given the precision of current neutrino data, priors still impact noticeably the constraints on neutrino masses and their hierarchy. To avoid our understanding of neutrinos being driven by prior assumptions, we construct a prior that is mathematically minimally informative. Using the constructed uninformative prior, we find that the normal hierarchy is favoured but with inconclusive posterior odds of 5.1:1. Better data is hence needed before the neutrino masses and their hierarchy can be well constrained. We find that the next decade of cosmological data should provide conclusive evidence if the normal hierarchy with negligible minimum mass is correct, and if the uncertainty in the sum of neutrino masses drops below 0.025 eV. On the other hand, if neutrinos obey the inverted hierarchy, achieving strong evidence will be difficult with the same uncertainties. Our uninformative prior was constructed from principles of the Objective Bayesian approach. The prior is called a reference prior and is minimally informative in the specific sense that the information gain after collection of data is maximised. The prior is computed for the combination of neutrino oscillation data and cosmological data and still applies if the data improve.

  6. Tandem mass spectrometric analysis of cyclophosphamide, ifosfamide and their metabolites.

    Liu, Zhongfa; Chan, Kenneth K; Wang, Jeffrey J

    2005-01-01

    A detailed multi-stage (MSn) fragmentation study of cyclophosphamide (CP), ifosfamide (IF) and their major metabolites, using an ion-trap mass spectrometer and a Q-TOF mass spectrometer, was performed with the aid of specifically deuterium-labeled analogs. The analytes showed good responses in positive-ion electrospray mass spectrometry as [MH]+ ions. Tandem mass spectra revealed a wealth of structurally specific ions, allowing characterization of the fragmentation pathways of these analytes. The major fragmentation pathways of the protonated CP and IF are elimination of ethylene from C5 and C6 of 1,3,2-oxazaphosphorine-2-oxide via a McLafferty rearrangement, and cleavage of the P-N bond. However, their activated 4-OOH and 4-OH metabolites primarily underwent hydrogen peroxide elimination and dehydration, respectively, followed by fragmentation pathways similar to those of CP and IF. These results should prove useful in structural elucidation of future analogs of CP and IF, and/or of their metabolites. Copyright (c) 2005 John Wiley & Sons, Ltd.

  7. Quantile regression analysis of body mass and wages.

    Johar, Meliyanni; Katayama, Hajime

    2012-05-01

    Using the National Longitudinal Survey of Youth 1979, we explore the relationship between body mass and wages. We use quantile regression to provide a broad description of the relationship across the wage distribution. We also allow the relationship to vary by the degree of social skills involved in different jobs. Our results find that for female workers body mass and wages are negatively correlated at all points in their wage distribution. The strength of the relationship is larger at higher-wage levels. For male workers, the relationship is relatively constant across wage distribution but heterogeneous across ethnic groups. When controlling for the endogeneity of body mass, we find that additional body mass has a negative causal impact on the wages of white females earning more than the median wages and of white males around the median wages. Among these workers, the wage penalties are larger for those employed in jobs that require extensive social skills. These findings may suggest that labor markets reward white workers for good physical shape differently, depending on the level of wages and the type of job a worker has. Copyright © 2011 John Wiley & Sons, Ltd.

  8. 15N sample preparation for mass spectroscopy analysis

    Trivelin, P.C.O.; Salati, E.; Matsui, E.

    1973-01-01

    Technics for preparing 15 N samples to be analised is presented. Dumas method and oxidation by sodium hypobromite method are described in order to get the appropriate sample. Method to calculate 15 N ratio from mass spectrometry dates is also discussed [pt

  9. Mass Spectrometric Analysis of Eight Common Chemical Explosives Using Ion Trap Mass Spectrometer

    Park, Sehwan; Lee, Jihyeon; KIm, Jeongkwon [Chungnam National Univ., Daejeon (Korea, Republic of); Cho, Soo Gyeong; Goh, Eun Mee [Agency for Defense Development, Daejeon (Korea, Republic of); Lee, Sungman; Koh, Sungsuk [Sensor Tech Inc., Seoul (Korea, Republic of)

    2013-12-15

    Eight representative explosives (ammonium perchlorate (AP), ammonium nitrate (AN), trinitrotoluene (TNT), 2,4-dinitrotoluene (DNT), cyclonite (RDX), cyclotetramethylenetetranitramine (HMX), pentaerythritol tetranitrate (PETN), and hexanitrostilbene (HNS)) were comprehensively analyzed with an ion trap mass spectrometer in negative ion mode using direct infusion electrospray ionization. MS/MS experiments were performed to generate fragment ions from the major parent ion of each explosive. Explosives in salt forms such as AP or AN provided cluster parent ions with their own anions. Explosives with an aromatic ring were observed as either [M.H]{sup -} for TNT and DNT or [M]{sup ·-}. for HNS, while explosives without an aromatic ring such as RDX, HMX, and PETN were detected as an adduct ion with a formate anion, i. e., [M+HCOO]{sup -}. These findings provide a guideline for the rapid and accurate detection of explosives once portable MS instruments become more readily available.

  10. Mass Spectrometric Analysis of Eight Common Chemical Explosives Using Ion Trap Mass Spectrometer

    Park, Sehwan; Lee, Jihyeon; KIm, Jeongkwon; Cho, Soo Gyeong; Goh, Eun Mee; Lee, Sungman; Koh, Sungsuk

    2013-01-01

    Eight representative explosives (ammonium perchlorate (AP), ammonium nitrate (AN), trinitrotoluene (TNT), 2,4-dinitrotoluene (DNT), cyclonite (RDX), cyclotetramethylenetetranitramine (HMX), pentaerythritol tetranitrate (PETN), and hexanitrostilbene (HNS)) were comprehensively analyzed with an ion trap mass spectrometer in negative ion mode using direct infusion electrospray ionization. MS/MS experiments were performed to generate fragment ions from the major parent ion of each explosive. Explosives in salt forms such as AP or AN provided cluster parent ions with their own anions. Explosives with an aromatic ring were observed as either [M.H] - for TNT and DNT or [M] ·- . for HNS, while explosives without an aromatic ring such as RDX, HMX, and PETN were detected as an adduct ion with a formate anion, i. e., [M+HCOO] - . These findings provide a guideline for the rapid and accurate detection of explosives once portable MS instruments become more readily available

  11. Mass and Heat Transfer Analysis of Membrane Humidifier with a Simple Lumped Mass Model

    Lee, Young Duk; Bae, Ho June; Ahn, Kook Young; Yu, Sang Seok; Hwang, Joon Young

    2009-01-01

    The performance of proton exchange membrane fuel cell (PEMFC) is seriously changed by the humidification condition which is intrinsic characteristics of the PEMFC. Typically, the humidification of fuel cell is carried out with internal or external humidifier. A membrane humidifier is applied to the external humidification of residential power generation fuel cell due to its convenience and high performance. In this study, a simple static model is constructed to understand the physical phenomena of the membrane humidifier in terms of geometric parameters and operating parameters. The model utilizes the concept of shell and tube heat exchanger but the model is also able to estimate the mass transport through the membrane. Model is constructed with FORTRAN under Matlab/Simulink □ environment to keep consistency with other components model which we already developed. Results shows that the humidity of wet gas and membrane thickness are critical parameters to improve the performance of the humidifier

  12. Fluid-Structure Interaction Analysis of Parachute Finite Mass Inflation

    Xinglong Gao

    2016-01-01

    Full Text Available Parachute inflation is coupled with sophisticated fluid-structure interaction (FSI and flight mechanic behaviors in a finite mass situation. During opening, the canopy often experiences the largest deformation and loading. To predict the opening phase of a parachute, a computational FSI model for the inflation of a parachute, with slots on its canopy fabric, is developed using the arbitrary Lagrangian-Euler coupling penalty method. In a finite mass situation, the fluid around the parachute typically has an unsteady flow; therefore, a more complex opening phase and FSI dynamics of a parachute are investigated. Navier-Stokes (N-S equations for uncompressible flow are solved using an explicit central difference method. The three-dimensional visualization of canopy deformation as well as the evolution of dropping velocity and overload is obtained and compared with the experimental results. This technique could be further applied in the airdrop test of a parachute for true prediction of the inflation characteristics.

  13. Centrosome isolation and analysis by mass spectrometry-based proteomics

    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...

  14. An Analysis of Mass Balance of Chilean Glaciers

    Ambinakudige, S.; Tetteh, L.

    2013-12-01

    Glaciers in Chile range from very small glacierets found on the isolated volcanoes of northern Chile to the 13,000 sq.km Southern Patagonian Ice Field. Regular monitoring of these glaciers is very important as they are considered as sensitive indicators of climate change. Millions of people's lives are dependent on these glaciers for fresh water and irrigation purpose. In this study, mass balances of several Chilean glaciers were estimated using Aster satellite images between 2007 and 2012. Highly accurate DEMs were created with supplementary information from IceSat data. The result indicated a negative mass balance for many glaciers indicating the need for further monitoring of glaciers in the Andes.

  15. Computer automated mass spectrometer for isotope analysis on gas samples

    Pamula, A.; Kaucsar, M.; Fatu, C.; Ursu, D.; Vonica, D.; Bendea, D.; Muntean, F.

    1998-01-01

    A low resolution, high precision instrument was designed and realized in the mass spectrometry laboratory of the Institute of Isotopic and Molecular Technology, Cluj-Napoca. The paper presents the vacuum system, the sample inlet system, the ion source, the magnetic analyzer and the ion collector. The instrument is almost completely automated. There are described the analog-to-digital conversion circuits, the local control microcomputer, the automation systems and the performance checking. (authors)

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

    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

  17. Mass transfer models analysis for the structured packings

    Suastegui R, A.O.

    1997-01-01

    The models that have been developing, to understand the mechanism of the mass transfer through the structured packings, present limitations for their application, existing then uncertainty in order to use them in the chemical industrial processes. In this study the main parameters used in the mass transfer are: the hydrodynamic of the bed of the column, the geometry of the bed, physical-chemical properties of the mixture and the flow regime of the operation between the flows liquid-gas. The sensibility of each one of these parameters generate an arduous work to develop right proposals and good interpretation of the phenomenon. With the purpose of showing the importance of these parameters mentioned in the mass transfer, this work is analyzed the process of absorption for the system water-air, using the models to the structured packings in packed columns. The models selected were developed by Bravo and collaborators in 1985 and 1992, in order to determine the parameters previous mentioned for the system water-air, using a structured packing built in the National Institute of Nuclear Research. In this work is showed the results of the models application and their discussion. (Author)

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

    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.

  19. CONCH: A Visual Basic program for interactive processing of ion-microprobe analytical data

    Nelson, David R.

    2006-11-01

    A Visual Basic program for flexible, interactive processing of ion-microprobe data acquired for quantitative trace element, 26Al- 26Mg, 53Mn- 53Cr, 60Fe- 60Ni and U-Th-Pb geochronology applications is described. Default but editable run-tables enable software identification of secondary ion species analyzed and for characterization of the standard used. Counts obtained for each species may be displayed in plots against analysis time and edited interactively. Count outliers can be automatically identified via a set of editable count-rejection criteria and displayed for assessment. Standard analyses are distinguished from Unknowns by matching of the analysis label with a string specified in the Set-up dialog, and processed separately. A generalized routine writes background-corrected count rates, ratios and uncertainties, plus weighted means and uncertainties for Standards and Unknowns, to a spreadsheet that may be saved as a text-delimited file. Specialized routines process trace-element concentration, 26Al- 26Mg, 53Mn- 53Cr, 60Fe- 60Ni, and Th-U disequilibrium analysis types, and U-Th-Pb isotopic data obtained for zircon, titanite, perovskite, monazite, xenotime and baddeleyite. Correction to measured Pb-isotopic, Pb/U and Pb/Th ratios for the presence of common Pb may be made using measured 204Pb counts, or the 207Pb or 208Pb counts following subtraction from these of the radiogenic component. Common-Pb corrections may be made automatically, using a (user-specified) common-Pb isotopic composition appropriate for that on the sample surface, or for that incorporated within the mineral at the time of its crystallization, depending on whether the 204Pb count rate determined for the Unknown is substantially higher than the average 204Pb count rate for all session standards. Pb/U inter-element fractionation corrections are determined using an interactive log e-log e plot of common-Pb corrected 206Pb/ 238U ratios against any nominated fractionation-sensitive species pair

  20. Charge collection control using retrograde well tested by proton microprobe irradiation

    Sayama, Hirokazu; Takai, Mikio; Kimura, Hiroshi; Ohno, Yoshikazu; Satoh, Shinichi; Sonoda, Kenichirou; Katani, Norihiko.

    1993-01-01

    Soft error reduction by high-energy ion-implanted layers has been investigated by novel evaluation techniques using high-energy proton microprobes. A retrograde well formed by 160 and 700 keV boron ion implantation could completely suppress soft errors induced by the proton microprobes at 400 keV. The proton-induced current revealed the charge collection efficiency for the retrograde well structure. The collected charge for the retrograde well in the soft-error mapping was proved to be lower than the critical charge of the measured DRAMs(dynamic random-access memories). Complementary use of soft-error mapping and ion-induced-current measurement could clarify well structures immune against soft errors. (author)

  1. Combining Raman Microprobe and XPS to Study High Temperature Oxidation of Metals

    Windisch, Charles F.; Henager, Charles H.; Engelhard, Mark H.; Bennett, Wendy D.

    2011-01-01

    Raman microprobe spectroscopy was applied in studies of high-temperature air oxidation of a ferritic alloy (HT-9) in the absence and presence of zirconia coatings with the objective of evaluating the technique as a way to quickly screen candidate cladding materials and actinide-based mixed oxide fuel mixtures for advanced nuclear reactors. When oxidation was relatively uniform, Raman spectra collected using microscope optics with low spatial resolution were found to be similar to those collected with conventional Raman spectroscopy. These spectra could be used to identify major oxide corrosion products and follow changes in the composition of the oxides due to heating. However, when the oxidation films were comprised of multiple layers of varying composition, or with layers containing metallic phases, techniques with higher depth resolution and sensitivity to zero-valence metals were necessary. The requirements were met by combining Raman microprobe using different optical configurations and x-ray photoelectron spectroscopy.

  2. Mass spectrometric analysis of stable carbon isotopes in abiogenic and biogenic natural compounds

    Sajjad, M.I.; Ahmed, M.; Tasneem, M.A.; Khan, I.A.; Latif, Z.

    1989-07-01

    This report describes the general methodology of sup/13/ carbon analysis on mass spectrometer and various preparation systems developed for conversion of samples into isotopically non-fractionated and purified carbon dioxide. Laboratory standards required for sup/13/ C analysis have been calibrated against international standards. The reproducibility/accuracy of sample preparation and analysis on mass spectrometer for sup/13/ C or sup/12/ C measurement is well within the internationally acceptable limits. (author)

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

    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.

  4. Lateral diffusion study of the Pt-Al system using the NAC nuclear microprobe.

    de Waal, H.; Pretorius, R.

    1999-10-01

    In this study a nuclear microprobe (NMP) was used to analyse phase formation during reaction in Pt-Al lateral diffusion couples. Phase identification was done by Rutherford backscattering spectroscopy. These results were compared with phase formation during conventional thin film Pt-Al interactions. The co-existence of multiple phases in lateral diffusion couples is discussed with reference to the effective heat of formation (EHF) model.

  5. Lateral diffusion study of the Pt-Al system using the NAC nuclear microprobe

    Waal, H. de E-mail: dewalla@nac.ac.za; Pretorius, R

    1999-09-02

    In this study a nuclear microprobe (NMP) was used to analyse phase formation during reaction in Pt-Al lateral diffusion couples. Phase identification was done by Rutherford backscattering spectroscopy. These results were compared with phase formation during conventional thin film Pt-Al interactions. The co-existence of multiple phases in lateral diffusion couples is discussed with reference to the effective heat of formation (EHF) model.

  6. Application of the microprobe dredging operation in the treatment of the meibomian gland dysfunction(MGD

    Qing-Qiang Wang

    2014-07-01

    Full Text Available AIM: To evaluate the function of the microprobe dredging technology in the treatment of meibomian gland dysfunction(MGDand to provide fast, efficient, economical and practical method of treatment for meibomian gland dysfunction(MGD. METHODS:The 100μm diameter stainless steel wire was made as the microprobe with the total length of 3cm, which the needle was about 5mm and hand shank was about 2.5cm. Selected 140 cases with dry eyes of meibomian gland dysfunction(MGD, patients were divided into two groups and made them have comparability. Observation group(n=70used microprobe to dredge meibomian gland pipe accompanied with drugs, hot compress and meibomian gland massage treatment. The control group(n=70was given conventional drugs, hot compress and meibomian massage treatment. To compare the tear break-up time(BUT, efficient rate and the cure rate of the two groups after treatment of 1d, 1wk, 2wk, 1 mo, 2mo and 3mo.RESULTS: BUT were significantly prolonged in observation group and control group after treatment, and the observation group improved more obviously; the efficient rate and cure rate of the observation group were significantly higher than that of the control group after 1d, 1wk, 2wk, 1mo, 2mo and 3mo treatment. CONCLUSION:Using microprobe to unclog the meibomian gland tube can provide the fast and efficient, economical and practical treatment for meibomian gland dysfunction(MGD, which can be promoted in the clinical practice.

  7. Distribution of copper and other elements in ryegrass roots, determined with a scanning proton microprobe

    Mazzolini, A.P.; Legge, G.J.F.

    1982-01-01

    A scanning proton microprobe has been used to determine the distribution of Cu and other elements in Wimmera ryegrass roots grown in solution cultures. Cu was found to be localized on or near the surface of the roots in randomly distributed discrete zones. The distribution of Cu was partially correlated with those of Fe, P and Ca and possibly indicates some form of association; co-precipitation in a precipitate of ferric phosphate or hydroxy-oxide is favoured

  8. Direct trace analysis of metals and alloys in a quadrupole ion-trap mass spectrometer

    Song, K S; Yang, M; Cha, H K; Lee, J M; Lee, G H

    1999-01-01

    An ion-trap mass spectrometer adopting a quadrupole ion-trap and laser ablation/ionization method was constructed. The developed system was tested for composition analysis of some metals (Cu, stainless), and alloys (hastalloy C, mumetal) by mass spectrometry. Samples were analyzed by using laser ablation from a sample probe tip followed by a mass analysis with the quadrupole ion-trap. The quadrupole ion-trap was modified to enable laser ablation by a XeCl excimer laser pulse that passed radially through the ring electrode. A mass scan of the produced ions was performed in the mass selective instability mode wherein trapped ions were successively detected by increasing the rf voltage through the ring electrode. Factors affecting the mass resolution, such as pressure of buffer gas and ablation laser power, are discussed.

  9. The study of voids in the AuAl thin-film system using the nuclear microprobe

    de Waal, H. S.; Pretorius, R.; Prozesky, V. M.; Churms, C. L.

    1997-07-01

    A Nuclear Microprobe (NMP) was used to study void formation in thin film gold-aluminium systems. Microprobe Rutherford Backscattering Spectrometry (μRBS) was utilised to effectively obtain a three-dimensional picture of the void structure on the scale of a few nanometers in the depth dimension and a few microns in the in-plane dimension. This study illustrates the usefulness of the NMP in the study of materials and specifically thin-film structures.

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

    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.)

  11. Kinematic separation and mass analysis of heavy recoiling nuclei

    Oganesyan, Yu.Ts.; Eremin, A.V.; Belozerov, A.V.

    2002-01-01

    Within the past twelve years, the recoil separator VASSILISSA has been used for investigation of evaporation residues produced in heavy-ion induced complete-fusion reactions. In the course of the experimental work in the region of the elements with 92 ≤ Z ≤ 94, fourteen new isotopes have been identified by the parent-daughter correlations. The study of the decay properties and formation cross sections of the isotopes of elements 110, 112, and 114 was performed with the use of the high intensity 48 Ca beams; 232 Th, 238 U and 242 Pu targets were used in the experiments. At the beam energies corresponding to the calculated cross-section maxima of the 3n evaporation channels, the isotopes 277 110, 283 112, and 287 114 were produced and identified. For further experiments aimed at the synthesis of the superheavy element isotopes (Z ≥ 110) with the intensive 48 Ca extracted beams, the improvements in the ion optical system of the separator and of the focal plane detector system have been made. As a result, for heavy recoiling nuclei with masses A ∼ 250, the mass resolution of about 2.5 % was achieved with a good energy and position resolutions of the focal plane detectors

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

    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

  13. The Mars Microprobe Mission: Advanced Micro-Avionics for Exploration Surface

    Blue, Randel

    2000-01-01

    The Mars Microprobe Mission is the second spacecraft developed as part of the New Millennium Program deep space missions. The objective of the Microprobe Project is to demonstrate the applicability of key technologies for future planetary missions by developing two probes for deployment on Mars. The probes are designed with a single stage entry, descent, and landing system and impact the Martian surface at speeds of approximately 200 meters per second. The microprobes are composed of two main sections, a forebody section that penetrates to a depth below the Martian surface of 0.5 to 2 meters, and an aftbody section that remains on the surface. Each probe system consists of a number of advanced technology components developed specifically for this mission. These include a non-erosive aeroshell for entry into. the atmosphere, a set of low temperature batteries to supply probe power, an advanced microcontroller to execute the mission sequence, collect the science data, and react to possible system fault conditions, a telecommunications subsystem implemented on a set of custom integrated circuits, and instruments designed to provide science measurements from above and below the Martian surface. All of the electronic components have been designed and fabricated to withstand the severe impact shock environment and to operate correctly at predicted temperatures below -100 C.

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

    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.

  15. Several problems of cumulative effective mass fraction in anti-seismic analysis

    Wang Wei; Sheng Feng; Li Hailong; Wen Jing; Luan Lin

    2005-01-01

    Cumulative Effective Mass Fraction (CEMF) is one of important items which sign the accuracy in antiseismic analysis. Based on the primary theories of CEMF, the paper show the influence of CEMF on the accuracy in antiseismic analysis. Moreover, some advices and ways are given to solve common problems in antiseismic analysis, such as how to increase CEMF, how to avoid the mass's loss because of the torsional frequency's being close to the frequency corresponding to the peak of seismic response spectrum, how to avoid the mass's loss because of the constraints, and so on. (authors)

  16. A versatile system for the rapid collection, handling and graphics analysis of multidimensional data

    O'Brien, P.M.; Moloney, G.; O'Oconnor, A.; Legge, G.J.F.

    1991-01-01

    The paper discusses the performances of a versatile computerized system developed at the Microanalytical Research Centre of the Melbourne University, for handling multiparameter data that may arise from a variety of experiments - nuclear, accelerator mass spectrometry, microprobe elemental analysis or 3-D microtomography. Some of the most demanding requirements arise in the application of microprobes to quantitative elemental mapping and to microtomography. A system to handle data from such experiments had been under continuous development. It has been reprogramed to run on a DG DS7540 workstation. The whole system of software has been rewritten, greatly expanded and made much more powerful and faster, by use of modern computer technology - a VME bus computer with a real-time operating system and a RISC workstation running UNIX and the X-window environment

  17. Acceleration Signal Characteristics for Intuitional Mass Analysis of Metallic Loose Parts

    Lee, Kwang-Hyun; Jung, Chang-Gyu

    2016-01-01

    Nuclear power plants (NPPs) have operated LPMS (Loose Parts Monitoring System) for early detection of the possible presence of metallic parts in the reactor coolant system (RCS); however, analysis of the metallic impact wave characteristics in the LPMS is an important issue because information, such as the mass of the metallic part and the impact location, is not provided. Most studies have concentrated on fieldwork using the frequency characteristics for the analysis of the metallic part mass. Thus, the field engineers cannot analyze signals without special software and access to the system. This paper is intended to introduce a process of intuitional mass analysis using the attenuation rate of the acceleration signal and the intervals between peak signals. Most studies related to mass analysis of a metallic part impact signal in LPMS have used the frequency spectrum. This paper presents a method of using the acceleration signal characteristics for intuitional mass analysis of loose metallic parts. With the method proposed in this paper, because the mass of a metallic part can be understood intuitionally without any special analysis program, intuitional analysis used in parallel with frequency spectrum analysis will be in effect

  18. Acceleration Signal Characteristics for Intuitional Mass Analysis of Metallic Loose Parts

    Lee, Kwang-Hyun; Jung, Chang-Gyu [KHNP CRI, Daejeon (Korea, Republic of)

    2016-10-15

    Nuclear power plants (NPPs) have operated LPMS (Loose Parts Monitoring System) for early detection of the possible presence of metallic parts in the reactor coolant system (RCS); however, analysis of the metallic impact wave characteristics in the LPMS is an important issue because information, such as the mass of the metallic part and the impact location, is not provided. Most studies have concentrated on fieldwork using the frequency characteristics for the analysis of the metallic part mass. Thus, the field engineers cannot analyze signals without special software and access to the system. This paper is intended to introduce a process of intuitional mass analysis using the attenuation rate of the acceleration signal and the intervals between peak signals. Most studies related to mass analysis of a metallic part impact signal in LPMS have used the frequency spectrum. This paper presents a method of using the acceleration signal characteristics for intuitional mass analysis of loose metallic parts. With the method proposed in this paper, because the mass of a metallic part can be understood intuitionally without any special analysis program, intuitional analysis used in parallel with frequency spectrum analysis will be in effect.

  19. Quality assurance for mass spectrometry research and development analysis

    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)

  20. Comprehensive Mass Analysis for Chemical Processes, a Case Study on L-Dopa Manufacture

    To evaluate the “greenness” of chemical processes in route selection and process development, we propose a comprehensive mass analysis to inform the stakeholders from different fields. This is carried out by characterizing the mass intensity for each contributing chemical or wast...

  1. The LLNL Multi-User Tandem Laboratory PIXE microprobe

    Heikkinen, D.W.; Bench, G.S.; Antolak, A.J.; Morse, D.H.; Pontau, A.E.

    1992-01-01

    We have recently completed the construction of a new ion beamline primarily for particle-induced x-ray emission (PIXE) analysis. This will supplement our current ion microtomography (IMT) material characterization capabilities using accelerator microanalysis. In this paper we describe the PIXE beamline and give some results that characterize the system. We also report the results of some initial experiments

  2. Metabolome analysis - mass spectrometry and microbial primary metabolites

    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...

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

    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...

  4. Accelerator mass spectrometry: ultrasensitive analysis of global science

    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

  5. Analysis of diffusive mass transport in a cracked buffer

    Garisto, N.C.; Garisto, F.

    1989-11-01

    In the disposal vault design for the Canadian Nuclear Fuel Waste Management Program, cylindrical containers of used nuclear fuel would be placed in vertical boreholes in rock and surrounded with a bentonite-based buffer material. The buffer is expected to absorb and/or retard radionuclides leaching from the fuel after the containers fail. There is some evidence, however, that the buffer may be susceptible to cracking. In this report we investigate numerically the consequences of cracking on uranium diffusion through the buffer. The derivation of the mass-transport equations and the numerical solution method are presented for the solubility-limited diffusion of uranium in a cracked buffer system for both swept-away and semi-impermeable boundary conditions at the rock-buffer interface. The results indicate that for swept-away boundary conditions the total uranium flux through the cracked buffer system is, as expected, greater than through the uncracked buffer. The effect of the cracks is strongly dependent on the ratio D/D eff , where D and D eff are the pore-water and the effective buffer diffusion coefficient, respectively. However, although a decrease in D eff enhances the effect of cracks on the total cumulative flux (relative to the uncracked buffer), it also decreases the total cumulative flux through the cracked buffer system (relative to a cracked buffer with a larger D eff value). Finally, for semi-impermeable boundary conditions, the effect of cracks on the total radionuclide flux is relatively small

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

    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

  7. Mercury mass measurement in fluorescent lamps via neutron activation analysis

    Viererbl, L.; Vinš, M.; Lahodová, Z.; Fuksa, A.; Kučera, Jan; Koleska, M.; Voljanskij, A.

    2015-01-01

    Roč. 116, NOV (2015), s. 56-59 ISSN 0969-806X R&D Projects: GA TA ČR TA01010237; GA MŠk LM2011019 Institutional support: RVO:61389005 Keywords : fluorescent lamp * mercury measurement * neutron activation analysis * research reactor Subject RIV: BG - Nuclear , Atomic and Molecular Physics, Colliders Impact factor: 1.207, year: 2015

  8. Chromatographic-mass spectrometric analysis of ethanol extract of ...

    Methods: The dried root of Maesa perlaria var. formosana was extracted with 95 % ethanol for composition analysis under the following optimum GC-MS conditions: 250 °C inlet temperature, 250 °C MSD detector temperature, and GC oven temperature programmed as follows: initial temperature held at 70 °C for 15 min, ...

  9. MALDI-TOF mass spectrometry for quantitative gene expression analysis of acid responses in Staphylococcus aureus.

    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.

  10. Analysis of Protein O-GlcNAcylation by Mass Spectrometry

    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...

  11. Network analysis of PTSD symptoms following mass violence.

    Sullivan, Connor P; Smith, Andrew J; Lewis, Michael; Jones, Russell T

    2018-01-01

    Network analysis is a useful tool for understanding how symptoms interact with one another to influence psychopathology. However, this analytic strategy has not been fully utilized in the PTSD field. The current study utilized network analysis to examine connectedness and strength among PTSD symptoms (employing both partial correlation and regression network analyses) among a community sample of students exposed to the 2007 Virginia Tech shootings. Respondents (N = 4,639) completed online surveys 3-4 months postshootings, with PTSD symptom severity measured via the Trauma Symptom Questionnaire. Data were analyzed via adaptive least absolute shrinkage and selection operator (LASSO) and relative importance networks, as well as Dijkstra's algorithm to identify the shortest path from each symptom to all other symptoms. Relative importance network analysis revealed that intrusive thoughts had the strongest influence on other symptoms (i.e., had many strong connections [highest outdegree]) while computing Dijkstra's algorithm indicated that anger produced the shortest path to all other symptoms (i.e., the strongest connections to all other symptoms). Findings suggest that anger or intrusion likely play a crucial role in the development and maintenance of PTSD (i.e., are more influential within the network than are other symptoms). (PsycINFO Database Record (c) 2018 APA, all rights reserved).

  12. Development of analysis methodology for hot leg break mass and energy release

    Song, Jin Ho; Kim, Cheol Woo; Kwon, Young Min; Kim, Sook Kwan

    1995-04-01

    A study for the development of an analysis methodology for hot leg break mass and energy release is performed. For the blowdown period a modified CEFLASH-4A methodology is suggested. For the post blowdown period a modified CONTRAST boil-off model is suggested. By using these computer code improved mass and energy release data are generated. Also, a RELAP5/MOD3 analysis for finally the FLOOD-3 computer code has been modified for use in the analysis of hot leg break. The results of analysis using modified FLOOD-3 are reasonable as we expected and their trends are good. 66 figs., 8 tabs. (Author) .new

  13. Laser Raman microprobe spectroscopy as a diagnostic for the characterisation of diamond and diamond like carbon (DLC) thin films

    Johnston, C.

    1990-10-01

    Invariably when manufacturing an artificial diamond film a mixture of carbon is deposited - tetragonally bonded (diamond), trigonally bonded (graphite) and other allotropic crystalline forms and amorphous carbons. This imposes a need for careful analysis to determine exactly what carbon types constitute the films. Raman spectroscopy is particularly sensitive to crystal and atomic structure and has a number of advantages which make it one of the most useful techniques for interrogating diamond and DLC thin films. Although Raman spectroscopy alone cannot fully characterise the film, it can give more information than simply what particular form of carbon or other impurities are present in the film. It can be used to determine the ratio of sp 2 to sp 3 bonding within the film, and to some extent the crystallite or domain size and the internal stress of the film. The use of laser Raman microprobe spectroscopy as a diagnostic tool in the analysis of diamond and DLC thin films is demonstrated for a variety of carbon films on various substrates and the characterisation of these films is discussed. (author)

  14. Factor analysis of combined organic and inorganic aerosol mass spectra from high resolution aerosol mass spectrometer measurements

    Y. L. Sun

    2012-09-01

    Full Text Available Positive matrix factorization (PMF was applied to the merged high resolution mass spectra of organic and inorganic aerosols from aerosol mass spectrometer (AMS measurements to investigate the sources and evolution processes of submicron aerosols in New York City in summer 2009. This new approach is able to study the distribution of organic and inorganic species in different types of aerosols, the acidity of organic aerosol (OA factors, and the fragment ion patterns related to photochemical processing. In this study, PMF analysis of the unified AMS spectral matrix resolved 8 factors. The hydrocarbon-like OA (HOA and cooking OA (COA factors contain negligible amounts of inorganic species. The two factors that are primarily ammonium sulfate (SO4-OA and ammonium nitrate (NO3-OA, respectively, are overall neutralized. Among all OA factors the organic fraction of SO4-OA shows the highest degree of oxidation (O/C = 0.69. Two semi-volatile oxygenated OA (OOA factors, i.e., a less oxidized (LO-OOA and a more oxidized (MO-OOA, were also identified. MO-OOA represents local photochemical products with a diurnal profile exhibiting a pronounced noon peak, consistent with those of formaldehyde (HCHO and Ox(= O3 + NO2. The NO+/NO2+ ion ratio in MO-OOA is much higher than that in NO3-OA and in pure ammonium nitrate, indicating the formation of organic nitrates. The nitrogen-enriched OA (NOA factor contains ~25% of acidic inorganic salts, suggesting the formation of secondary OA via acid-base reactions of amines. The size distributions of OA factors derived from the size-resolved mass spectra show distinct diurnal evolving behaviors but overall a progressing evolution from smaller to larger particle mode as the oxidation degree of OA increases. Our results demonstrate that PMF analysis of the unified aerosol mass spectral matrix which contains both

  15. Liquid chromatography mass spectrometry for analysis of microbial metabolites

    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. Molecular Isotopic Distribution Analysis (MIDAs) with adjustable mass accuracy.

    Alves, Gelio; Ogurtsov, Aleksey Y; Yu, Yi-Kuo

    2014-01-01

    In this paper, we present Molecular Isotopic Distribution Analysis (MIDAs), a new software tool designed to compute molecular isotopic distributions with adjustable accuracies. MIDAs offers two algorithms, one polynomial-based and one Fourier-transform-based, both of which compute molecular isotopic distributions accurately and efficiently. The polynomial-based algorithm contains few novel aspects, whereas the Fourier-transform-based algorithm consists mainly of improvements to other existing Fourier-transform-based algorithms. We have benchmarked the performance of the two algorithms implemented in MIDAs with that of eight software packages (BRAIN, Emass, Mercury, Mercury5, NeutronCluster, Qmass, JFC, IC) using a consensus set of benchmark molecules. Under the proposed evaluation criteria, MIDAs's algorithms, JFC, and Emass compute with comparable accuracy the coarse-grained (low-resolution) isotopic distributions and are more accurate than the other software packages. For fine-grained isotopic distributions, we compared IC, MIDAs's polynomial algorithm, and MIDAs's Fourier transform algorithm. Among the three, IC and MIDAs's polynomial algorithm compute isotopic distributions that better resemble their corresponding exact fine-grained (high-resolution) isotopic distributions. MIDAs can be accessed freely through a user-friendly web-interface at http://www.ncbi.nlm.nih.gov/CBBresearch/Yu/midas/index.html.

  17. Fat mass to fat-free mass ratio reference values from NHANES III using bioelectrical impedance analysis.

    Xiao, J; Purcell, S A; Prado, C M; Gonzalez, M C

    2017-10-06

    Low fat-free mass (FFM) or high fat mass (FM) are abnormal body composition phenotypes associated with morbidity. These conditions in combination lead to worse health outcomes, and can be identified by a high FM/FFM ratio. Here, we developed sex, age, and body mass index (BMI) stratified, population-based FM/FFM reference values using bioelectrical impedance analysis (BIA) measurements. White, non-Hispanic individuals aged 18-90 years old with data for weight, stature and BIA resistance measures from the third National Health and Nutrition Examination Survey (NHANES) III were included. Previously validated and sex-specific BIA prediction equations were used to calculate FM and FFM. FM/FFM values were generated at 5th, 50th and 95th percentiles for each sex, age (18-39.9, 40-59.9, 60-69.9 and 70-90 years), and BMI category (underweight, normal weight, overweight, class I/II and class III obesity). A total of 6372 individuals who had estimated FM and FFM values were identified (3366 females, 3006 males). Median values of FM/FFM were 0.24 and 0.40 for young (≤39.9 years) males and females with normal BMI, and 0.34 for males and 0.59 for females who were overweight. For elderly individuals aged >70 years, median FM/FFM for males and females were respectively 0.28 and 0.45 for those with normal BMI, and 0.37 and 0.61 for those in the overweight category. These FM/FFM reference values provide information on body composition characteristics that account for age, sex and BMI, which can be useful to identify individuals at risk for body composition abnormalities. Copyright © 2017 Elsevier Ltd and European Society for Clinical Nutrition and Metabolism. All rights reserved.

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

    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.

  19. TOF plotter - a program to perform routine analysis time-of-flight mass spectral data

    Knippel, Brad C.; Padgett, Clifford W.; Marcus, R. Kenneth

    2004-01-01

    The main article discusses the operation and application of the program to mass spectral data files. This laboratory has recently reported the construction and characterization of a linear time-of-flight mass spectrometer (ToF-MS) utilizing a radio frequency glow discharge ionization source. Data acquisition and analysis was performed using a digital oscilloscope and Microsoft Excel, respectively. Presently, no software package is available that is specifically designed for time-of-flight mass spectral analysis that is not instrument dependent. While spreadsheet applications such as Excel offer tremendous utility, they can be cumbersome when repeatedly performing tasks which are too complex or too user intensive for macros to be viable. To address this situation and make data analysis a faster, simpler task, our laboratory has developed a Microsoft Windows-based software program coded in Microsoft Visual Basic. This program enables the user to rapidly perform routine data analysis tasks such as mass calibration, plotting and smoothing on x-y data sets. In addition to a suite of tools for data analysis, a number of calculators are built into the software to simplify routine calculations pertaining to linear ToF-MS. These include mass resolution, ion kinetic energy and single peak identification calculators. A detailed description of the software and its associated functions is presented followed by a characterization of its performance in the analysis of several representative ToF-MS spectra obtained from different GD-ToF-MS systems

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

    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.

  1. The analysis of uranium in environmental sample by mass spectrometer combined with isotopic dilution

    Fu Zhonghua; Jia Baoting; Han Jun

    2003-01-01

    Uranium in the environmental sample was analyzed by mass spectrometer combined with isotopic dilution. Before mass spectrometer analysis, samples were dissolved in a concentrated acidic solution containing HNO 3 , HF and HClO 4 and chemically processed to suit the analysis requirement. Analysis results indicated that the uranium content was 0.08 μg/g in river water, 0.1 μg/g in evergreen foliage, and 5-11 μg/g in surface soil respectively. (authors)

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

    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.

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

    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.

  4. Analysis of the plasmodium falciparum proteome by high-accuracy mass spectrometry

    Lasonder, Edwin; Ishihama, Yasushi; Andersen, Jens S

    2002-01-01

    -accuracy (average deviation less than 0.02 Da at 1,000 Da) mass spectrometric proteome analysis of selected stages of the human malaria parasite Plasmodium falciparum. The analysis revealed 1,289 proteins of which 714 proteins were identified in asexual blood stages, 931 in gametocytes and 645 in gametes. The last...

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

    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.

  6. Climate Change Discourse in Mass Media: Application of Computer-Assisted Content Analysis

    Kirilenko, Andrei P.; Stepchenkova, Svetlana O.

    2012-01-01

    Content analysis of mass media publications has become a major scientific method used to analyze public discourse on climate change. We propose a computer-assisted content analysis method to extract prevalent themes and analyze discourse changes over an extended period in an objective and quantifiable manner. The method includes the following: (1)…

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

    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

  8. SUMS preliminary design and data analysis development. [shuttle upper atmosphere mass spectrometer experiment

    Hinson, E. W.

    1981-01-01

    The preliminary analysis and data analysis system development for the shuttle upper atmosphere mass spectrometer (SUMS) experiment are discussed. The SUMS experiment is designed to provide free stream atmospheric density, pressure, temperature, and mean molecular weight for the high altitude, high Mach number region.

  9. Speciation analysis of 129I in seawater using coprecipitation and accelerator mass spectrometry and its applications

    Xing, Shan; Hou, Xiaolin; Aldahan, Ala

    2017-01-01

    Speciation analysis of long-lived 129I in seawater can provide useful information on the source of water masses. This paper presents an improved method for speciation analysis of 129I based on coprecipitation of iodide as AgI with Ag2SO3 and AgCl. By adding a small amount of 127I carrier...

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

    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

  11. $ANBA; a rapid, combined data acquisition and correction program for the SEMQ electron microprobe

    McGee, James J.

    1983-01-01

    $ANBA is a program developed for rapid data acquisition and correction on an automated SEMQ electron microprobe. The program provides increased analytical speed and reduced disk read/write operations compared with the manufacturer's software, resulting in a doubling of analytical throughput. In addition, the program provides enhanced analytical features such as averaging, rapid and compact data storage, and on-line plotting. The program is described with design philosophy, flow charts, variable names, a complete program listing, and system requirements. A complete operating example and notes to assist in running the program are included.

  12. New improvements in the characterization of refractory gold in pyrites: an electron microprobe, Moessbauer spectrometry and ion microprobe study

    Marion, P.; Holliger, P.; Boiron, M.C.; Cathelineau, M.; Wagner, F.E.

    1991-01-01

    Studies of pyrites by Moessbauer spectroscopy have shown the presence of gold in a combined state probably inserted within the lattice. In order to enhance detection limits for in-situ quantitative gold analyses, new SIMS investigations have been made thanks to a Resistive Anode Encorder record of the ion emissions, which provides digital images or scans of any part of the analyzed volume. Quantitative analysis of gold have been carried out thanks to 2 MeV ion implantation of gold in reference sulfide crystals, and the bulk composition of a pyrite grain has been determined. Some strong enrichments in gold and arsenic at the crystal margin attest fluctuations in the fluid chemistry and may be interpreted as a final growth zone, which is similar to that observed on arsenopyrite crystals. This multidisciplinary approach constitutes a powerful tool for the investigation of the insertion and distribution of trace elements within crystals, especially gold in sulfides at low contents down to a few ppm. (author)

  13. Pb, U, Ti, Hf and Zr distributions in zircons determined by proton microprobe and fission track techniques

    Clark, G.J.; Gulson, B.L.; Cookson, J.A.

    1979-01-01

    A proton microprobe has been used to determine Pb, Tl, Hf and Zr distributions across four single zircon crystals separated from a 'rapakivi' granite. The Pb and Zr data are quantitative: Pb and Tl concentrations were below the measurable limits for determinations in situ by most other techniques. The distribution of U in the same crystals was determined by the fission track technique. Limits on precision of U allow only a qualitative correlation of U and Pb, whereas the Tl and Pb correlation is more exactly determined. Zircons with distinct cores and overgrowths exhibited uniform Zr and Hf concentrations across the crystals, whereas the high U rims and 'inclusions' (domains) also had high Tl and Pb contents. Since almost all the Pb in these zircons is derived by radioactive decay of U, the Tl substitution has paralleled that of U. The results indicate that the high U domains are 'hot spots' rather than a separate mineral phase. The strong positive correlation of U and Pb indicates that there is little U daughter product migration relative to U, within the crystal. However, for the zircon population investigated here, the data are equivocal on the question of whether U addition to zircon crystals is associated with new zircon growth or not. In either case, the heterogeneous U and Pb distributions complicate any interpretations of U-Pb isotopic analysis for such zircon populations. (author)

  14. Dynamic analysis of CO₂ labeling and cell respiration using membrane-inlet mass spectrometry.

    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.

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

    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

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

    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

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

    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

  18. Method of N-15 analysis by mass-spectroscopy on ion implanter MPB-200

    Vo Van Thuan; Dang Duc Nhan; Nguyen Phuc; Nguyen Tien Dung; Nguyen Van Dach

    1993-01-01

    The industrial implanter MPB-200 has been modified to a light-isotope mass spectrometer. Mass-resolution has been improved by combination of quadrupole focusing system and a collimator with additional scattering shielding. Single beam method has been set up, in which mass-spectrum are obtained by scanning magnetic field of the separator. A start-stop control system has been added to operate automatically the magnet and registration system, from which signals are transferred to a XT/AT computer for saving and analysis. The mass-resolution is satisfactory for analysis of light isotopes with mass number A less than 40. A testing measurement has been done with standard samples of natural and enriched N-15 isotope, at acceleration energy of 50 keV, beam current less than 100 nA, vacuum of 4x10E-6 and collimator's shell of 1 mm. Obtained resolution and background condition allowed to achieve a good linear dependence of relative isotope ratio data vs real abundance in the range from natural 0.365% to 5.0% with a 3% error (96% of reliability). Routine N-15 may achieve (5-10)% accuracy by a 7-10 minutes measurement for every sample. Sensitivity of the mass-spectrometer is better almost by one order in comparing with one of emission spectrometers. The new mass-spectroscopy system is applied to research in agriculture, biology and environmental study. (author). 4 refs, 4 figs

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

    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

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

    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...

  1. Reliability and mass analysis of dynamic power conversion systems with parallel or standby redundancy

    Juhasz, Albert J.; Bloomfield, Harvey S.

    1987-01-01

    A combinatorial reliability approach was used to identify potential dynamic power conversion systems for space mission applications. A reliability and mass analysis was also performed, specifically for a 100-kWe nuclear Brayton power conversion system with parallel redundancy. Although this study was done for a reactor outlet temperature of 1100 K, preliminary system mass estimates are also included for reactor outlet temperatures ranging up to 1500 K.

  2. Reliability and mass analysis of dynamic power conversion systems with parallel of standby redundancy

    Juhasz, A. J.; Bloomfield, H. S.

    1985-01-01

    A combinatorial reliability approach is used to identify potential dynamic power conversion systems for space mission applications. A reliability and mass analysis is also performed, specifically for a 100 kWe nuclear Brayton power conversion system with parallel redundancy. Although this study is done for a reactor outlet temperature of 1100K, preliminary system mass estimates are also included for reactor outlet temperatures ranging up to 1500 K.

  3. Mass balance re-analysis of Findelengletscher, Switzerland; benefits of extensive snow accumulation measurements

    Leo eSold

    2016-02-01

    Full Text Available A re-analysis is presented here of a 10-year mass balance series at Findelengletscher, a temperate mountain glacier in Switzerland. Calculating glacier-wide mass balance from the set of glaciological point balance observations using conventional approaches, such as the profile or contour method, resulted in significant deviations from the reference value given by the geodetic mass change over a five-year period. This is attributed to the sparsity of observations at high elevations and to the inability of the evaluation schemes to adequately estimate accumulation in unmeasured areas. However, measurements of winter mass balance were available for large parts of the study period from snow probings and density pits. Complementary surveys by helicopter-borne ground-penetrating radar (GPR were conducted in three consecutive years. The complete set of seasonal observations was assimilated using a distributed mass balance model. This model-based extrapolation revealed a substantial mass loss at Findelengletscher of -0.43m w.e. a^-1 between 2004 and 2014, while the loss was less pronounced for its former tributary, Adlergletscher (-0.30m w.e. a^-1. For both glaciers, the resulting time series were within the uncertainty bounds of the geodetic mass change. We show that the model benefited strongly from the ability to integrate seasonal observations. If no winter mass balance measurements were available and snow cover was represented by a linear precipitation gradient, the geodetic mass balance was not matched. If winter balance measurements by snow probings and snow density pits were taken into account, the model performance was substantially improved but still showed a significant bias relative to the geodetic mass change. Thus the excellent agreement of the model-based extrapolation with the geodetic mass change was owed to an adequate representation of winter accumulation distribution by means of extensive GPR measurements.

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

    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...

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

    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

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

    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

  7. Screening and confirmation criteria for hormone residue analysis using liquid chromatography accurate mass time-of-flight, Fourier transform ion cyclotron resonance and orbitrap mass spectrometry techniques

    Nielen, M.W.F.; Engelen, M.C. van; Zuiderent, R.; Ramaker, R.

    2007-01-01

    An emerging trend is recognised in hormone and veterinary drug residue analysis from liquid chromatography tandem mass spectrometry (LC/MS/MS) based screening and confirmation towards accurate mass alternatives such as LC coupled with time-of-flight (TOF), Fourier transform ion cyclotron resonance

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

    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

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

    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,

  10. A hard X-ray scanning microprobe for fluorescence imaging and microdiffraction at the Advanced Photon Source

    Cai, L.; Lai, B.; Yun, W.; Ilinski, P.; Legnini, D.; Maser, J.; Rodrigues, W.

    1999-01-01

    A hard x-ray scanning microprobe based on zone plate optics and undulator radiation, in the energy region from 6 to 20 keV, has reached a focal spot size (FWHM) of 0.15 microm (v) x 0.6 microm (h), and a photon flux of 4 x 10 9 photons/sec/0.01%BW. Using a slit 44 meters upstream to create a virtual source, a circular beam spot of 0.15 microm in diameter can be obtained with a photon flux of one order of magnitude less. During fluorescence mapping of trace elements in a single human ovarian cell, the microprobe exhibited an imaging sensitivity for Pt (L a line) of 80 attograms/microm 2 for a count rate of 10 counts per second. The x-ray microprobe has been used to map crystallographic strain and multiquantum well thickness in micro-optoelectronic devices produced with the selective area growth technique

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

    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

  12. Genome-wide association analysis identifies three new susceptibility loci for childhood body mass index

    Felix, Janine F.; Bradfield, Jonathan P.; Monnereau, Claire; van der Valk, Ralf J.P.; Stergiakouli, Evie; Chesi, Alessandra; Gaillard, Romy; Feenstra, Bjarke; Thiering, Elisabeth; Kreiner-Møller, Eskil; Mahajan, Anubha; Pitkänen, Niina; Joro, Raimo; Cavadino, Alana; Huikari, Ville; Franks, Steve; Groen-Blokhuis, Maria M.; Cousminer, Diana L.; Marsh, Julie A.; Lehtimäki, Terho; Curtin, John A.; Vioque, Jesus; Ahluwalia, Tarunveer S.; Myhre, Ronny; Price, Thomas S.; Vilor-Tejedor, Natalia; Yengo, Loïc; Grarup, Niels; Ntalla, Ioanna; Ang, Wei; Atalay, Mustafa; Bisgaard, Hans; Blakemore, Alexandra I.; Bonnefond, Amelie; Carstensen, Lisbeth; Eriksson, Johan; Flexeder, Claudia; Franke, Lude; Geller, Frank; Geserick, Mandy; Hartikainen, Anna-Liisa; Haworth, Claire M.A.; Hirschhorn, Joel N.; Hofman, Albert; Holm, Jens-Christian; Horikoshi, Momoko; Hottenga, Jouke Jan; Huang, Jinyan; Kadarmideen, Haja N.; Kähönen, Mika; Kiess, Wieland; Lakka, Hanna-Maaria; Lakka, Timo A.; Lewin, Alexandra M.; Liang, Liming; Lyytikäinen, Leo-Pekka; Ma, Baoshan; Magnus, Per; McCormack, Shana E.; McMahon, George; Mentch, Frank D.; Middeldorp, Christel M.; Murray, Clare S.; Pahkala, Katja; Pers, Tune H.; Pfäffle, Roland; Postma, Dirkje S.; Power, Christine; Simpson, Angela; Sengpiel, Verena; Tiesler, Carla M. T.; Torrent, Maties; Uitterlinden, André G.; van Meurs, Joyce B.; Vinding, Rebecca; Waage, Johannes; Wardle, Jane; Zeggini, Eleftheria; Zemel, Babette S.; Dedoussis, George V.; Pedersen, Oluf; Froguel, Philippe; Sunyer, Jordi; Plomin, Robert; Jacobsson, Bo; Hansen, Torben; Gonzalez, Juan R.; Custovic, Adnan; Raitakari, Olli T.; Pennell, Craig E.; Widén, Elisabeth; Boomsma, Dorret I.; Koppelman, Gerard H.; Sebert, Sylvain; Järvelin, Marjo-Riitta; Hyppönen, Elina; McCarthy, Mark I.; Lindi, Virpi; Harri, Niinikoski; Körner, Antje; Bønnelykke, Klaus; Heinrich, Joachim; Melbye, Mads; Rivadeneira, Fernando; Hakonarson, Hakon; Ring, Susan M.; Smith, George Davey; Sørensen, Thorkild I.A.; Timpson, Nicholas J.; Grant, Struan F.A.; Jaddoe, Vincent W.V.

    2016-01-01

    A large number of genetic loci are associated with adult body mass index. However, the genetics of childhood body mass index are largely unknown. We performed a meta-analysis of genome-wide association studies of childhood body mass index, using sex- and age-adjusted standard deviation scores. We included 35 668 children from 20 studies in the discovery phase and 11 873 children from 13 studies in the replication phase. In total, 15 loci reached genome-wide significance (P-value < 5 × 10−8) in the joint discovery and replication analysis, of which 12 are previously identified loci in or close to ADCY3, GNPDA2, TMEM18, SEC16B, FAIM2, FTO, TFAP2B, TNNI3K, MC4R, GPR61, LMX1B and OLFM4 associated with adult body mass index or childhood obesity. We identified three novel loci: rs13253111 near ELP3, rs8092503 near RAB27B and rs13387838 near ADAM23. Per additional risk allele, body mass index increased 0.04 Standard Deviation Score (SDS) [Standard Error (SE) 0.007], 0.05 SDS (SE 0.008) and 0.14 SDS (SE 0.025), for rs13253111, rs8092503 and rs13387838, respectively. A genetic risk score combining all 15 SNPs showed that each additional average risk allele was associated with a 0.073 SDS (SE 0.011, P-value = 3.12 × 10−10) increase in childhood body mass index in a population of 1955 children. This risk score explained 2% of the variance in childhood body mass index. This study highlights the shared genetic background between childhood and adult body mass index and adds three novel loci. These loci likely represent age-related differences in strength of the associations with body mass index. PMID:26604143

  13. Comparative glacio-climatological analysis of mass balance variability along the geographical margin of Europe

    Lehoczky, Annamária; Kern, Zoltán; Pongrácz, Rita

    2014-05-01

    Glacio-climatological studies recognise glacier mass balance changes as high-confident climate indicators. The climatic sensitivity of a glacier does not simply depend on regional climate variability but also influenced via large- and mesoscale atmospheric circulation patterns. This study focuses on recent changes in the mass balance using records from three border regions of Europe, and investigates the relationships between the seasonal mass balance components, regional climatic conditions, and distant atmospheric forcing. Since glaciers in different macro-climatological conditions (i.e., mid-latitudes or high-latitudes, dry-continental or maritime regions) may present strongly diverse mass balance characteristics, the three analysed regions were selected from different glacierised macroregions (using the database of the World Glacier Monitoring Service). These regions belong to the Caucasus Mountains (Central Europe macroregion), the Polar Ural (Northern Asia macroregion), and Svalbard (Arctic Islands macroregion). The analysis focuses on winter, summer, and annual mass balance series of eight glaciers. The climatic variables (atmospheric pressure, air temperature, precipitation) and indices of teleconnection patterns (e.g., North Atlantic Oscillation, Pacific Decadal Oscillation) are used from the gridded databases of the University of East Anglia, Climatic Research Unit and the National Oceanic and Atmospheric Administration, National Center for Environmental Prediction. However, the period and length of available mass balance data in the selected regions vary greatly (the first full record is in 1958, Polar Ural; the last is in 2010, Caucasus Mountains), a comparative analysis can be carried out for the period of 1968-1981. Since glaciers from different regions respond to large- and mesoscale climatic forcings differently, and because the mass balance of glaciers within a region often co-vary, our specific objectives are (i) to examine the variability and the

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

    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.

  15. Thermal analysis with expendable cartridge

    Susaki, K.; Landgraf, F.J.G.

    1981-01-01

    The pratical method of thermal analysis with expendable cartridge and some aspects of its use are presented. The results of the method applied to the system Nb-Mn are presented together with data from microprobe. (Author) [pt

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

    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

  17. Carrier phases for iodine in the Allende meteorite and their associated 129Xer/127I ratios: A laser microprobe study

    Kirschbaum, C.

    1988-01-01

    A new mass spectrometer of high sensitivity coupled to a laser microprobe sample extraction system was used to determine the 129 Xe r /I ratios of minerals which carry 129 Xe r in the Allende meteorite. In sodalite-rich fine-grained inclusions Ok correlates with Cl verifying that sodalite carries the majority of I. One sample heated above the decomposition point of sodalite had a small amount of residual I indicating the presence of at least one other carrier. The Cl/I ratio of the matrix was different from that of the fine-grained inclusions and the 129 Xe r correlates with trapped Xe. This implies either a different Cl/I ratio for sodalite in the matrix or a different carrier for I in matrix. In melilite from one coarse-grained inclusion, I is variable and correlates with both Xe and, surprisingly, 131 Xe produced from Ba during the irradiation. In coarse-grained inclusions with Cl-rich alteration products in cracks, most of the 129 Xe r is found in those cracks. A residual amount of 129 Xe r is present in melilite samples which show no Cl-rich alteration products, and is a trace impurity in the melilite. The 129 Xe r / 127 I ratio of sodalite from the fine-grained inclusions, and matrix is similar--between 1.25 and 1.35 x 10 -4 . This implies an age for these samples within 2 million years of a Bjurbole chondrule included in the irradiation as a standard. The 129 Xe r / 127 I ratio of a sample of a fine-grained inclusion heated to 1,100 degree C is 2.4 x 10 -4 or 16 million years before the Bjurbole chondrule. A coarse-grained inclusion on the other hand showed a 129 Xe r / 127 I ratio of 3.15 x 10 -5 or 35 million years after the Bjurbole chondrule

  18. Fast probing of glucose and fructose in plant tissues via plasmonic affinity sandwich assay with molecularly-imprinted extraction microprobes.

    Muhammad, Pir; Liu, Jia; Xing, Rongrong; Wen, Yanrong; Wang, Yijia; Liu, Zhen

    2017-12-01

    Determination of specific target compounds in agriculture food and natural plant products is essential for many purposes; however, it is often challenging due to the complexity of the sample matrices. Herein we present a new approach called plasmonic affinity sandwich assay for the facile and rapid probing of glucose and fructose in plant tissues. The approach mainly relies on molecularly imprinted plasmonic extraction microprobes, which were prepared on gold-coated acupuncture needles via boronate affinity controllable oriented surface imprinting with the target monosaccharide as the template molecules. An extraction microprobe was inserted into plant tissues under investigation, which allowed for the specific extraction of glucose or fructose from the tissues. The glucose or fructose molecules extracted on the microprobe were labeled with boronic acid-functionalized Raman-active silver nanoparticles, and thus affinity sandwich complexes were formed on the microprobes. After excess Raman nanotags were washed away, the microprobe was subjected to Raman detection. Upon being irradiated with a laser beam, surface plasmon on the gold-coated microprobes was generated, which further produced plasmon-enhanced Raman scattering of the silver-based nanotags and thereby provided sensitive detection. Apple fruits, which contain abundant glucose and fructose, were used as a model of plant tissues. The approach exhibited high specificity, good sensitivity (limit of detection, 1 μg mL -1 ), and fast speed (the whole procedure required only 20 min). The spatial distribution profiles of glucose and fructose within an apple were investigated by the developed approach. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. X-ray microprobe characterization of materials: the case for undulators on advanced storage rings

    Sparks, C.J. Jr.

    1984-01-01

    The unique properties of X rays offer many advantages over electrons and other charged particles for the microcharacterization of materials. X rays are more efficient in exciting characteristic X-ray fluorescence and produce higher fluorescent signals to backgrounds than obtained with electrons. Detectable limits for X rays are a few parts per billion and are 10 -3 to 10 -5 less than for electrons. Energy deposition in the sample by X rays is 10 -3 to 10 -4 less than for electrons for the same detectable concentration. High-brightness storage rings, especially in the 6 GeV class with undulators, will be approximately 10 3 brighter in the X-ray energy range from 5 keV to 35 keV than existing storage rings and provide for X-ray microprobes that are as bright as the most advanced electron probes. Such X-ray microprobes will produce unprecedented low levels of detection in diffraction, EXAFS, Auger, and photoelectron spectroscopies for both chemical characterization and elemental identification. These major improvements in microcharacterization capabilities will have wide-ranging ramifications not only in materials science but also in physics, chemistry, geochemistry, biology, and medicine

  20. Data smoothing techniques applied to proton microprobe scans of teleost hard parts

    West, I.F.; Gauldie, R.W.; Coote, G.E.

    1992-01-01

    We use a proton microprobe to examine the distribution of elements in otoliths and scales of teleost (bony) fish. The elements of principal interest are calcium and strontium in otoliths and calcium and fluorine in scales. Changes in the distribution of these elements across hard structures may allow inferences about the life histories of fish. Otoliths and scales of interest are up to a centimeter in linear dimension and to reveal the structures of interest up to 200 sampling points are required in each dimension. The time needed to accumulate high X-ray counts at each sampling point can be large, particularly for strontium. To reduce microprobe usage we use data smoothing techniques to reveal changing patterns with modest X-ray count accumulations at individual data points. In this paper we review performance for revealing pattern at modest levels of X-ray count accumulations of a selection of digital filters (moving average smoothers), running median filters, robust locally weighted regression filters and adaptive spline filters. (author)

  1. Millimeter length micromachining using a heavy ion nuclear microprobe with standard magnetic scanning

    Nesprías, F.; Debray, M.E.; Davidson, J.; Kreiner, A.J.

    2013-01-01

    In order to increase the scanning length of our microprobe, we have developed an irradiation procedure suitable for use in any nuclear microprobe, extending at least up to 400% the length of our heavy ion direct writing facility using standard magnetic exploration. Although this method is limited to patterns of a few millimeters in only one direction, it is useful for the manufacture of curved waveguides, optical devices such Mach–Zehnder modulators, directional couplers as well as channels for micro-fluidic applications. As an example, this technique was applied to the fabrication of 3 mm 3D-Mach–Zehnder modulators in lithium niobate with short Y input/output branches and long shaped parallel-capacitor control electrodes. To extend and improve the quality of the machined structures we developed new scanning control software in LabView™ platform. The new code supports an external dose normalization, electrostatic beam blanking and is capable of scanning figures at 16 bit resolution using a National Instruments™ PCI-6731 High-Speed I/O card. A deep and vertical micromachining process using swift 35 Cl ions 70 MeV bombarding energy and direct write patterning was performed on LiNbO 3 , a material which exhibits a strong natural anisotropy to conventional etching. The micromachined structures show the feasibility of this method for manufacturing micro-fluidic channels as well

  2. Millimeter length micromachining using a heavy ion nuclear microprobe with standard magnetic scanning

    Nesprías, F. [Gerencia de Investigación y Aplicaciones, Comisión Nacional de Energía Atómica, Av. Gral Paz 1499 (1650), San Martín, Buenos Aires (Argentina); Debray, M.E., E-mail: debray@tandar.cnea.gov.ar [Gerencia de Investigación y Aplicaciones, Comisión Nacional de Energía Atómica, Av. Gral Paz 1499 (1650), San Martín, Buenos Aires (Argentina); Escuela de Ciencia y Tecnología. Universidad Nacional de Gral. San Martín, M. De Irigoyen 3100 (1650), San Martín, Buenos Aires (Argentina); Davidson, J. [Gerencia de Investigación y Aplicaciones, Comisión Nacional de Energía Atómica, Av. Gral Paz 1499 (1650), San Martín, Buenos Aires (Argentina); CONICET, Avda. Rivadavia 1917 (C1033AAJ), Ciudad Autónoma de Buenos Aires (Argentina); Kreiner, A.J. [Gerencia de Investigación y Aplicaciones, Comisión Nacional de Energía Atómica, Av. Gral Paz 1499 (1650), San Martín, Buenos Aires (Argentina); Escuela de Ciencia y Tecnología. Universidad Nacional de Gral. San Martín, M. De Irigoyen 3100 (1650), San Martín, Buenos Aires (Argentina); CONICET, Avda. Rivadavia 1917 (C1033AAJ), Ciudad Autónoma de Buenos Aires (Argentina); and others

    2013-04-01

    In order to increase the scanning length of our microprobe, we have developed an irradiation procedure suitable for use in any nuclear microprobe, extending at least up to 400% the length of our heavy ion direct writing facility using standard magnetic exploration. Although this method is limited to patterns of a few millimeters in only one direction, it is useful for the manufacture of curved waveguides, optical devices such Mach–Zehnder modulators, directional couplers as well as channels for micro-fluidic applications. As an example, this technique was applied to the fabrication of 3 mm 3D-Mach–Zehnder modulators in lithium niobate with short Y input/output branches and long shaped parallel-capacitor control electrodes. To extend and improve the quality of the machined structures we developed new scanning control software in LabView™ platform. The new code supports an external dose normalization, electrostatic beam blanking and is capable of scanning figures at 16 bit resolution using a National Instruments™ PCI-6731 High-Speed I/O card. A deep and vertical micromachining process using swift {sup 35}Cl ions 70 MeV bombarding energy and direct write patterning was performed on LiNbO{sub 3}, a material which exhibits a strong natural anisotropy to conventional etching. The micromachined structures show the feasibility of this method for manufacturing micro-fluidic channels as well.

  3. Single ion hit detection set-up for the Zagreb ion microprobe

    Smith, R. W.; Karlušić, M.; Jakšić, M.

    2012-04-01

    Irradiation of materials by heavy ions accelerated in MV tandem accelerators may lead to the production of latent ion tracks in many insulators and semiconductors. If irradiation is performed in a high resolution microprobe facility, ion tracks can be ordered by submicrometer positioning precision. However, full control of the ion track positioning can only be achieved by a reliable ion hit detection system that should provide a trigger signal irrespectively of the type and thickness of the material being irradiated. The most useful process that can be utilised for this purpose is emission of secondary electrons from the sample surface that follows the ion impact. The status report of the set-up presented here is based on the use of a channel electron multiplier (CEM) detector mounted on an interchangable sample holder that is inserted into the chamber in a close geometry along with the sample to be irradiated. The set-up has been tested at the Zagreb ion microprobe for different ions and energies, as well as different geometrical arrangements. For energies of heavy ions below 1 MeV/amu, results show that efficient (100%) control of ion impact can be achieved only for ions heavier than silicon. The successful use of the set-up is demonstrated by production of ordered single ion tracks in a polycarbonate film and by monitoring fluence during ion microbeam patterning of Foturan glass.

  4. An extended magnetic quadrupole lens for a high-resolution nuclear microprobe

    Breese, M.B.H. E-mail: m.breese@surrey.ac.uk; Grime, G.W.; Linford, W.; Harold, M

    1999-09-02

    This paper describes the design requirements and initial performance of a new style of magnetic quadrupole lens for use in a high-resolution nuclear microprobe, which is presently being constructed in Oxford. Such a microprobe necessitates the use of a small image distance from the exit face of the final quadrupole lens to the image plane in order to produce a large demagnification. This means that the final lens should be as close to the sample chamber as possible. However, with conventional magnetic quadrupoles the current-carrying coils protrude by a typical distance of 10-20 mm beyond the pole face, thereby significantly limiting the minimum image distance. The approach taken here is to recess the coils into the body of the lens, so that they are almost flush with the pole pieces and lens yoke, enabling an image distance of 55 mm. Three-dimensional magnetic field calculations within this lens structure predict that the field in the extended pole piece 'nose' region is only slightly less than that in the main lens body. Experimental field profiles, measured using a Hall probe, are used to confirm these calculations.

  5. An extended magnetic quadrupole lens for a high-resolution nuclear microprobe

    Breese, M.B.H.; Grime, G.W.; Linford, W.; Harold, M.

    1999-01-01

    This paper describes the design requirements and initial performance of a new style of magnetic quadrupole lens for use in a high-resolution nuclear microprobe, which is presently being constructed in Oxford. Such a microprobe necessitates the use of a small image distance from the exit face of the final quadrupole lens to the image plane in order to produce a large demagnification. This means that the final lens should be as close to the sample chamber as possible. However, with conventional magnetic quadrupoles the current-carrying coils protrude by a typical distance of 10-20 mm beyond the pole face, thereby significantly limiting the minimum image distance. The approach taken here is to recess the coils into the body of the lens, so that they are almost flush with the pole pieces and lens yoke, enabling an image distance of 55 mm. Three-dimensional magnetic field calculations within this lens structure predict that the field in the extended pole piece 'nose' region is only slightly less than that in the main lens body. Experimental field profiles, measured using a Hall probe, are used to confirm these calculations

  6. Study of the toughening mechanisms in bone and biomimetic hydroxyapatite materials using Raman microprobe spectroscopy.

    Pezzotti, Giuseppe; Sakakura, Seiji

    2003-05-01

    A Raman microprobe spectroscopy characterization of microscopic fracture mechanisms is presented for a natural hydroxyapatite material (cortical bovine femur) and two synthetic hydroxyapatite-based materials with biomimetic structures-a hydroxyapatite skeleton interpenetrated with a metallic (silver) or a polymeric (nylon-6) phase. In both the natural and synthetic materials, a conspicuous amount of toughening arose from a microscopic crack-bridging mechanism operated by elasto-plastic stretching of unbroken second-phase ligaments along the crack wake. This mechanism led to a rising R-curve behavior. An additional micromechanism, responsible for stress relaxation at the crack tip, was recognized in the natural bone material and was partly mimicked in the hydroxyapatite/silver composite. This crack-tip mechanism conspicuously enhanced the cortical bone material resistance to fracture initiation. A piezo-spectroscopic technique, based on a microprobe measurement of 980 cm(-1) Raman line of hydroxyapatite, enabled us to quantitatively assess in situ the microscopic stress fields developed during fracture both at the crack tip and along the crack wake. Using the Raman piezo-spectroscopy technique, toughening mechanisms were assessed quantitatively and rationally related to the macroscopic fracture characteristics of hydroxyapatite-based materials. Copyright 2003 Wiley Periodicals, Inc.

  7. Improved 206Pb/238U microprobe geochronology by the monitoring of a trace-element-related matrix effect; SHRIMP, ID-TIMS, ELA-ICP-MS and oxygen isotope documentation for a series of zircon standards

    Black, L.P.; Kamo, S.L.; Allen, C.M.; Davis, D.W.; Aleinikoff, J.N.; Valley, J.W.; Mundil, R.; Campbell, I.H.; Korsch, R.J.; Williams, I.S.; Foudoulis, C.

    2004-01-01

    Precise isotope dilution-thermal ionisation mass spectrometry (ID-TIMS) documentation is given for two new Palaeozoic zircon standards (TEMORA 2 and R33). These data, in combination with results for previously documented standards (AS3, SL13, QGNG and TEMORA 1), provide the basis for a detailed investigation of inconsistencies in 206Pb/238U ages measured by microprobe. Although these ages are normally consistent between any two standards, their relative age offsets are often different from those established by ID-TIMS. This is true for both sensitive high-resolution ion-microprobe (SHRIMP) and excimer laser ablation-inductively coupled plasma-mass spectrometry (ELA-ICP-MS) dating, although the age offsets are in the opposite sense for the two techniques. Various factors have been investigated for possible correlations with age bias, in an attempt to resolve why the accuracy of the method is worse than the indicated precision. Crystallographic orientation, position on the grain-mount and oxygen isotopic composition are unrelated to the bias. There are, however, striking correlations between the 206Pb/238U age offsets and P, Sm and, most particularly, Nd abundances in the zircons. Although these are not believed to be the primary cause of this apparent matrix effect, they indicate that ionisation of 206Pb/238U is influenced, at least in part, by a combination of trace elements. Nd is sufficiently representative of the controlling trace elements that it provides a quantitative means of correcting for the microprobe age bias. This approach has the potential to reduce age biases associated with different techniques, different instrumentation and different standards within and between laboratories. Crown Copyright ?? 2004 Published by Elsevier B.V. All rights reserved.

  8. Depth Probing Soft X-ray Microprobe (DPSXRM) for High Resolution Probing of Earth's Microstructural Samples

    Dikedi, P. N.

    2015-12-01

    The Cambrian explosion; occurrence of landslides in very dry weather conditions; rockslides; dead, shriveled-up and crumbled leaves possessing fossil records with the semblance of well preserved, flat leaves; abundance of trilobite tracks in lower and higher rock layers; and sailing stones are enigmas demanding demystifications. These enigmas could be elucidated when data on soil structure, texture and strength are provided by some device with submicrometre accuracy; for these and other reasons, the design of a Depth Probing Soft X-ray Microprobe (DPSXRM), is being proposed; it is expected to deliver soft X-rays, at spatial resolution, ϛ≥600nm and to probe at the depth of 0.5m in 17s. The microprobe is portable compared to a synchrotron radiation facility (Diamond Light Source has land size of 43,300m2); spatial resolution,ϛ , of the DPSXRM surpasses those of the X-ray Fluorescence microanalysis (10µm), electron microprobe (1-3µm) and ion microprobe (5->30µm); the DPSXRM has allowance for multiple targets. Vanadium and Manganese membranes are proposed owing to respective 4.952KeV VKα1 and 5.899KeV MnKα1 X-rays emitted, which best suits micro-probing of Earth's microstructural samples. Compound systems like the Kirk-Patrick and Baez and Wolter optics, aspheric mirrors like elliptical and parabolic optics, small apertures and Abbe sine condition are employed to reduce or remove astigmatism, obliquity, comatic and spherical aberrations—leading to good image quality. Results show that 5.899KeV MnKα1 and 4.952KeV VKα1 soft X-rays will travel a distance of 2.75mm to form circular patches of radii 2.2mm and 2.95mm respectively. Zone plate with nth zone radius of 1.5mm must be positioned 1.5mm and 2mm from the electron gun if circular patches must be formed from 4.952KeV VKα1 and 5.899KeV MnKα1 soft X-rays respectively. The focal lengths of 0.25μm≤ƒ≤1.50μm and 0.04μm≤ƒ≤0.2μm covered by 4.952KeV VKα1 and 5.899KeV Mn Kα1 soft X-Rays, will

  9. Heat And Mass Transfer Analysis of a Film Evaporative MEMS Tunable Array

    O'Neill, William J.

    This thesis details the heat and mass transfer analysis of a MEMs microthruster designed to provide propulsive, attitude control and thermal control capabilities to a cubesat. This thruster is designed to function by retaining water as a propellant and applying resistive heating in order to increase the temperature of the liquid-vapor interface to either increase evaporation or induce boiling to regulate mass flow. The resulting vapor is then expanded out of a diverging nozzle to produce thrust. Because of the low operating pressure and small length scale of this thruster, unique forms of mass transfer analysis such as non-continuum gas flow were modeled using the Direct Simulation Monte Carlo method. Continuum fluid/thermal simulations using COMSOL Multiphysics have been applied to model heat and mass transfer in the solid and liquid portions of the thruster. The two methods were coupled through variables at the liquid-vapor interface and solved iteratively by the bisection method. The simulations presented in this thesis confirm the thermal valving concept. It is shown that when power is applied to the thruster there is a nearly linear increase in mass flow and thrust. Thus, mass flow can be regulated by regulating the applied power. This concept can also be used as a thermal control device for spacecraft.

  10. The bio-PIXE setup on the Debrecen scanning proton microprobe

    Kertesz, Zs.; Szikszai, Z.; Uzonyi, I.; Simon, A.; Kiss, A.Z.

    2004-01-01

    Complete text of publication follows. Besides the ongoing applications in archeometry, geology, material science and atmospheric aerosol study, in recent years the IBA Group in Debrecen has joined several biological and biomedical research projects. Such studies require the knowledge of accurate quantitative elemental concentrations and distributions in organic, inhomogeneous thin samples on a microscopic scale. In most cases, to carry out quantitative investigations on biomedical samples down to the cell level, the combination of proton induced X-ray emission (PIXE), Rutherford backscattering (RBS) spectrometry and scanning transmission ion microscopy (STIM) analytical methods are used simultaneously. STIM provides information on the density and structure of the sample, PIXE measures the concentration of the inorganic major and trace elements, and finally RBS serves to characterize the organic matrix, to determine the beam dose, and sometimes the sample thickness. The drawback of this combined method is that to evaluate the RBS data the hydrogen to carbon ratio in the sample must be known. The setup developed at the Debrecen microprobe facility [1] is based on the combined application of on-axis STIM and simultaneous PIXE-PIXE analytical techniques. In the PIXE-PIXE method the sample matrix is determined directly by measuring X-rays from all elements in the sample including the light elements such as carbon and oxygen, using two Si(Li) X-ray detectors. In this arrangement an ultra thin windowed Si(Li) X-ray detector serves to characterize the matrix by measuring low energy X-ray lines (0.2-9 keV) while a large area Be-windowed detector is used to detect the medium and high energy X-ray lines (>4 keV). In this way elements with atomic number higher than 5 can be detected simultaneously, reducing both radiation damage of the sample and measurement time. In addition, the knowledge of the hydrogen content of the sample is not needed, since it influences the

  11. Structural design and analysis of test mass module for DECIGO Pathfinder

    Wakabayashi, Y; Ejiri, Y; Suzuki, R; Sugamoto, A; Obuchi, Y; Okada, N; Torii, Y; Ueda, A; Kawamura, S; Araya, A; Ando, M; Sato, S

    2010-01-01

    Deci-hertz Interferometer Gravitational-Wave Observatory: DECIGO is a project aimed at future detection of deci-hertz gravitational waves in space. DECIGO Pathfinder: DPF is a precursor mission to test the key technologies with one spacecraft. Our work in this article was to examine the strength of the DPF test mass module to ensure that it is sufficiently robust for launch with a launch vehicle. We designed the test mass module, and examined the structural strength of this model by structural analysis, Quasi-static acceleration analysis and Modal analysis using FEA (Finite Element Analysis). We found that the results of each analysis fulfilled all requirements. We are confident that the DPF test mass module will withstand Quasi-static acceleration or coupling with vibration of launch vehicle during launch, if the design matches the current design. For more detail, further analysis including Response analysis and Thermal analysis are recommended. In addition, it will be necessary to lighten the model in the next step.

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

    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.

  13. Charm and beauty quark masses in the MMHT2014 global PDF analysis

    Harland-Lang, L.A.; Motylinski, P.; Thorne, R.S. [University College London, Department of Physics and Astronomy, London (United Kingdom); Martin, A.D. [Durham University, Institute for Particle Physics Phenomenology, Durham (United Kingdom)

    2016-01-15

    We investigate the variation in the MMHT2014 PDFs when we allow the heavy-quark masses m{sub c} and m{sub b} to vary away from their default values.Wemake PDF sets available in steps of Δm{sub c} = 0.05 GeV and Δm{sub b} = 0.25 GeV, and present the variation in the PDFs and in the predictions. We examine the comparison to the HERA data on charm and beauty structure functions and note that in each case the heavy-quark data, and the inclusive data, have a slight preference for lower masses than our default values.We provide PDF sets with three and four active quark flavours, as well as the standard value of five flavours. We use the pole mass definition of the quark masses, as in the default MMHT2014 analysis, but briefly comment on the MS definition. (orig.)

  14. Charm and beauty quark masses in the MMHT2014 global PDF analysis

    Harland-Lang, L. A. [Department of Physics and Astronomy, University College London, WC1E 6BT, London (United Kingdom); Martin, A. D. [Institute for Particle Physics Phenomenology, Durham University, DH1 3LE, Durham (United Kingdom); Motylinski, P.; Thorne, R. S., E-mail: thorne@hep.ucl.ac.uk [Department of Physics and Astronomy, University College London, WC1E 6BT, London (United Kingdom)

    2016-01-06

    We investigate the variation in the MMHT2014 PDFs when we allow the heavy-quark masses m{sub c} and m{sub b} to vary away from their default values. We make PDF sets available in steps of Δm{sub c}=0.05 GeV and Δm{sub b}=0.25 GeV, and present the variation in the PDFs and in the predictions. We examine the comparison to the HERA data on charm and beauty structure functions and note that in each case the heavy-quark data, and the inclusive data, have a slight preference for lower masses than our default values. We provide PDF sets with three and four active quark flavours, as well as the standard value of five flavours. We use the pole mass definition of the quark masses, as in the default MMHT2014 analysis, but briefly comment on the (MS)-bar definition.

  15. Charm and beauty quark masses in the MMHT2014 global PDF analysis.

    Harland-Lang, L A; Martin, A D; Motylinski, P; Thorne, R S

    We investigate the variation in the MMHT2014 PDFs when we allow the heavy-quark masses [Formula: see text] and [Formula: see text] to vary away from their default values. We make PDF sets available in steps of [Formula: see text] and [Formula: see text], and present the variation in the PDFs and in the predictions. We examine the comparison to the HERA data on charm and beauty structure functions and note that in each case the heavy-quark data, and the inclusive data, have a slight preference for lower masses than our default values. We provide PDF sets with three and four active quark flavours, as well as the standard value of five flavours. We use the pole mass definition of the quark masses, as in the default MMHT2014 analysis, but briefly comment on the [Formula: see text] definition.

  16. Mass and loss analysis of a space-type radiation cooled insulated DC transmission line

    Schwarze, g.E.

    1986-01-01

    As both the power levels and transmission distances increase such as for large future nuclear power systems, the transmission line becomes an important element in the power chain between the source and load bus. Thus, the transmission line's characteristics must be determined so that the effect of these characteristics on the total power system can be assessed. These design characteristics include the specific mass, percent power loss, size, voltage and power levels, and operating temperatures of the conductor and insulating materials. In a previous paper, the dc transmission line's characteristics of a noninsulated solid cylindrical conductor were determined. In that analysis the expression derived for the transmission line's mass only included the conductor mass and the operating temperature of the line was that of the conductor. In the analysis of this paper, a single layer of insulation is added to the solid cylindrical conductor. In this analysis the dependency of the dc transmission line's mass, loss, and size on the power and voltage levels, conductor and insulation surface temperatures, transmission distance, and conductor and insulation material properties is determined. This analysis can be extended to multi-layers of insulation but the complexity of the analysis increases as the number of layers increase

  17. Fully automatic and precise data analysis developed for time-of-flight mass spectrometry.

    Meyer, Stefan; Riedo, Andreas; Neuland, Maike B; Tulej, Marek; Wurz, Peter

    2017-09-01

    Scientific objectives of current and future space missions are focused on the investigation of the origin and evolution of the solar system with the particular emphasis on habitability and signatures of past and present life. For in situ measurements of the chemical composition of solid samples on planetary surfaces, the neutral atmospheric gas and the thermal plasma of planetary atmospheres, the application of mass spectrometers making use of time-of-flight mass analysers is a technique widely used. However, such investigations imply measurements with good statistics and, thus, a large amount of data to be analysed. Therefore, faster and especially robust automated data analysis with enhanced accuracy is required. In this contribution, an automatic data analysis software, which allows fast and precise quantitative data analysis of time-of-flight mass spectrometric data, is presented and discussed in detail. A crucial part of this software is a robust and fast peak finding algorithm with a consecutive numerical integration method allowing precise data analysis. We tested our analysis software with data from different time-of-flight mass spectrometers and different measurement campaigns thereof. The quantitative analysis of isotopes, using automatic data analysis, yields results with an accuracy of isotope ratios up to 100 ppm for a signal-to-noise ratio (SNR) of 10 4 . We show that the accuracy of isotope ratios is in fact proportional to SNR -1 . Furthermore, we observe that the accuracy of isotope ratios is inversely proportional to the mass resolution. Additionally, we show that the accuracy of isotope ratios is depending on the sample width T s by T s 0.5 . Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

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

    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.

  19. Mass shootings: a meta-analysis of the dose-response relationship.

    Wilson, Laura C

    2014-12-01

    A meta-analysis was conducted to examine the dose-response theory as it relates to posttraumatic stress symptoms (PTSSs) following mass shootings. It was hypothesized that greater exposure to a mass shooting would be associated with greater PTSSs. Trauma exposure in the current study was broadly defined as the extent to which a person experienced or learned about a mass shooting. The meta-analysis identified 11 qualifying studies that included 13 independent effect sizes from a total of 8,047 participants. The overall weighted mean effect size, based on a random effects model, was r = .19, p shooting on the relationship between exposure and PTSSs. Because so few studies satisfied the inclusion criteria, the present study also documents that this area of the literature is underresearched. Copyright © 2014 International Society for Traumatic Stress Studies.

  20. Toward the Atomic-Level Mass Analysis of Biomolecules by the Scanning Atom Probe.

    Nishikawa, Osamu; Taniguchi, Masahiro

    2017-04-01

    In 1994, a new type of atom probe instrument, named the scanning atom probe (SAP), was proposed. The unique feature of the SAP is the introduction of a small extraction electrode, which scans over a specimen surface and confines the high field, required for field evaporation of surface atoms in a small space, between the specimen and the electrode. Thus, the SAP does not require a sharp specimen tip. This indicates that the SAP can mass analyze the specimens which are difficult to form in a sharp tip, such as organic materials and biomolecules. Clean single wall carbon nanotubes (CNT), made by high-pressure carbon monoxide process are found to be the best substrates for biomolecules. Various amino acids and dipeptide biomolecules were successfully mass analyzed, revealing characteristic clusters formed by strongly bound atoms in the specimens. The mass analysis indicates that SAP analysis of biomolecules is not only qualitative, but also quantitative.