Spark Source Mass Spectrometry Research Articles

スパークイオン源質量分析法によるニッケル基，鉄基耐熱合金の分析

スパークイオン源質量分析法によるニッケル基，鉄基耐熱合金の分析

Column cementation on aluminium powder as a preconcentration technique for trace element determinations by spark-source mass spectrometry : Part 1. Copper, lead, ruthenium and the noble metals

The technique of column cementation on aluminium metal powder for preconcentration from soution of copper, lead, ruthenium and the noble metals is shown to be quantitative over a wide range of concentrations. Optimum conditions of pH, temperature and solution flow rate are established. In conjunction with final measurements by spark-source mass spectrometry of the aluminium powder concentrate, detection limits are below 1 μg l −1 and concentration factors of >1000-fold are readily obtainable. Interference effects are discussed; the principal interference, that of iron, can be masked with fluoride.

Determination of trace impurities in sodium coolant from a Fast Breeder Reactor by inductively coupled plasma atomic-emission spectrometry

Trace impurities in samples of the liquid sodium coolant from the Dounreay Fast Reactor are determined by inductively coupled plasma (ICP) atomic-emission spectrometry of vacuum distillation residues. A 72-channel vacuum spectrometer with a 1-kW argon plasma source, fed by a coaxial capillary nebuliser, simultaneously measures 59 elements with a precision varying from <1% at concentrations 20 times the detection limit to 30% at detection levels. The ICP torch box is enclosed in a fume-cupboard fitted with a filtered extract system to allow safe handing of the radioactive solutions. Comparisons of some results have been made with spark-source mass spectrometry, d.c. arc emission spectrography, neutron-activation analysis and atomic-absorption spectrometry.

Exploitation of spark source mass spectrometry photoplates by digital image processing.

Digitalization of the 15 exposures all along the useful part of the photoplate is done on a high performance microdensitometer. Exploitation takes place on a high resolution color graphic monitor. Ionic species identification is performed directly on the display by comparison between the analysed spectrum image and a reference spectrum image, which shows all possible simple ionic kinds that the spectrograph may transfer. The software manipulates images very fast, bringing the analyst quickness and flexibility in the exploitation of spectra.

Recent developments in spark source mass spectrometry SSMS

Three directions of development are being followed up in SSMS. • - Basic investigations into ion formation • - Development of apparatus and • - Development of methods Particular progress has been made in quantitative multielement analysis. Examples are given of achievable accuracies.

Recent developments in spark source mass spectrometry SSMS

Recent developments in spark source mass spectrometry SSMS

Deep photoluminescence band related to oxygen in gallium arsenide

Temperature-dependent photoluminescence and photoluminescence excitation spectroscopy have been used to measure the 0.63-eV luminescence band present in O-doped semi-insulating GaAs. It is shown that the 0.63-eV band is related to the presence of O. The center responsible for the band forms a deep level similar to the main deep donor EL2. However, spark source mass spectrometry indicates that incorporation of O into GaAs is difficult.

Validation of the sulphur concentration of selected iron-base NBS standard reference materials by isotope-dilution spark-source mass-spectrometry

An isotope-dilution spark-source mass-spectrometric procedure has been developed for the accurate determination of sulphur in iron-base alloys. Dissolution in a sealed tube is used to prevent volatilization losses and to effect isotope equilibration. Application of this technique to the re-analysis of existing NBS Standard Reference Materials yields results that are generally in good agreement with the certified values.

Evidence of intrinsic double acceptor in GaAs

Acceptors present in undoped p-type conducting GaAs have been studied with photoluminescence, temperature-dependent Hall measurements, deep level transient spectroscopy, and spark source mass spectrometry. It is shown that p-type conduction is due to presence of the shallow acceptor CAs and the cation antisite double acceptor GaAs. The first and second ionization energies determined for GaAs are 77 and 230 meV from the valence-band edge.

Comprehensive quantitative analysis by spark source mass spectrometry: A technique on the brink

Spark Source Mass Spectrometry has been shown to be a particularly sensitive method for the detection of small concentrations of a wide range of elements in solid samples. However, unless improved commercial instrumentation becomes available it is a method which, in spite of its great potential, will fall into progressive decline.

Sample preparation for actinide solid state research

The actinide elements (5f elements) and their compounds constitute a very interesting group for solid state research. The electronic properties of the 5f elements show intermediate behavior between the well-understood, completely localized 4f system (lanthanides) and the 3d system (transition elements). The possibility of understanding some unexplained properties of the 3d elements through a systematic investigation of the electronic structures of the actinides considerably increased interest in samples with well-defined composition and structure and with well-known purity. In some cases, single crystals of low defect densities and high purity levels are needed to allow sophisticated investigations of physical properties. Actinide compounds are easily obtained at a high purity level by direct synthesis from pure elements using noncontaminating techniques. Examples of these techniques are the reaction of the actinide metal powder with the vapor of an oxidant in a sealed quartz ampoule, leviation melting on a water-cooled pedestal or melting in a Huking crucible. Actinide metals are produced by metallothermic reduction of commercially available oxides or carbides or by the van Arkel purification process. The metals are refined to the desired purity level by evaporation in vacuum for the more volatile elements (Ac, Pu, Am, Cm, Bk) and by the van Arkel process for the metals with low vapor pressure. Single crystals of actinide compounds have been grown by chemical vapor transport methods (oxides, chalcogenides), high temperature solution growth techniques (oxides), and pulling from the melt by the Czochralski method (oxides, intermetallics). Thin solid films have been prepared by vacuum evaporation or by focused ion-beam sputtering. The materials are analyzed for trace-level impurity content by inductively-coupled plasma spectroscopy, by spark source mass spectroscopy and by secondary-ion mass spectroscopy. The chemical composition of the compounds is determined by standard methods of analytical chemistry. Crystallographic structure is investigated by X-ray and electron diffraction; single crystals are investigated for homogeneity and inclusions using an electron microprobe and for defects by X-ray and neutron diffraction by optical and electron microscopy. The crystallographic orientation is obtained from X-ray Laue diffraction patterns.

A comparison between secondary-ion mass-spectrometry and spark-source mass-spectrometry for the quantitative analysis of steel wire

A comparison has been made between the results of the matrix-ion species ratio (MISR) method for quantification of secondary-ion mass-spectrometry data and spark-source mass-spectrometry analysis using photoplate detection for analysis of the steel basis of AlZn coated wire products. For SIMS quantification a suitable set of sensitivity factors, corrected for the actual surface sampling condition, was used. The results of both methods compare well. The SIMS results were, for most elements, within 25% of the concentration determined by SSMS. This could indicate that reasonably accurate results can be obtained by using the matrix-ion species ratio method for SIMS.

Recent advances in analytical spark source mass spectrometry

Spark source mass spectrometry is an established technique for the chemical analysis of trace and minor inorganic constituents in many types of material. Its merits are its inherent high sensitivity with detection limits down to a few nanograms per gram and an extremely wide elemental coverage, i.e. essentially all the elements present in the sample. Drawbacks that explain its lesser popularity compared with other techniques result from (1) the complexity and cost of the apparatus, (2) the time-consuming operation when detection is performed with an ion emulsion, and (3) inaccuracies inherent in ion formation and the measurement process. A review will be given of the basic theory, the instrumentation and a few representative applications. Special reference will be made to recent advances in methodology (e.g. the development of multi-element isotope dilution) and instrumentation: the development of the understanding of the r.f. spark ion formation process, alternative mechanisms for ionization, and the exploitation of ion detectors other than the photographic plate (electrical detection with electron multipliers and position-sensitive detectors).

A dominant electrical defect in GaAs

Several as-grown Bridgman and Czochralski GaAs crystals, with dominant electrical levels from 0.13–0.20 eV below the conduction band, have been studied by the temperature-dependent Hall-effect, spark-source mass spectroscopy, and secondary-ion mass spectroscopy. It is shown that no impurity is of a sufficient concentration to account for these levels, and therefore they are composed of single or multiple defects. The detailed nature of the defects has not yet been established but may involve an As vacancy. It is believed that this is the first time that a dominant electrically active center has been shown to be a pure defect in any as-grown semiconductor.

Use of implanted samples as standards in spark-source mass spectrometry with application to the analysis of III—V semiconductors

Summary The method described for the analysis of III—V semiconducting materials by sparksource mass spectrometry is especially suitable for the characterization of indium phosphide single crystals. As a means of standardization, some of the crystals were doped either uniformly during growth or by implantation of a well-defined dopant at levels of 1014–1015 atoms cm-2. Implantation is shown to be valuable for providing standards at low levels of impurities. The main impurities in indium phosphide single crystals are Si, C, O, B, N, Al, (S), Zn and As, but sixteen other elements are present below the detection limit. In a single crystal grown by the liquid encapsulation technique, two types of impurity segregation, along the axis of growth and along the radial axis, are revealed.

Lasers in solid state mass spectrometry

Abstract

Spark source mass spectrometry and atomic absorption spectrometry in the analysis of high purity materials

Abstract

Determination of impurities in high purity tantalum powder by spark source mass spectroscopy

Determination of impurities in high purity tantalum powder by spark source mass spectroscopy

Determination of sulphur in semiconductor-grade indium and indium phosphide by cathodic-stripping voltammetry

A procedure is presented for the determination of sulphur in indium and indium phosphide within the range 0.01–100 p.p.m. by mass, based upon hydrogen sulphide evolution and differential-pulse cathodic-stripping voltammetry of the sulphide ion. Good recoveries of sulphide added to indium are demonstrated. Agreement with results obtained by spark-source mass spectrometry and reproducibilities at 0.1 and 1 p.p.m. levels by mass are satisfactory. Sulphur concentrations at the level of 100 p.p.m. by mass found in sulphur-doped indium phosphide are in agreement with the measured electrical carrier concentrations. Use of the procedure in establishing the sources of sulphur contamination in the liquid-phase epitaxial growth of indium phosphide layers is discussed briefly.

Impurities in silicon nitride raw materials and correlation with mechanical strength of the hot-pressed body.

Spark-source mass spectrometry was used in order to determine the impurity elements from Li to La in nine commercial samples of Si3N4 raw materials. Total contents of thirty three impurity elements detected from Si3N4 raw powders which were prepared by a reaction of Si and N2 were 1.0 to 2.2wt%. Otherwhile there were few kinds of impurities in samples which were prepared by reactions of pure SiCl4-NH3 and SiO2-C-N2, and total impurity contents was 0.07-0.14%. Three-point bending strength at 1200°C for the hot-pressed body from α-rich powder with 2wt% Al2O3 and 5wt% Y2O3 was decreased with the total impurity contents. Similar correlations were observed between the 1200°C-strengths and respective contents of Ca, Ti or Fe. However the room temperature strength was independent on the total impurity contents. Hot-pressed bodies from β-, α≅β- and amorphous powder showed lower strengths than those expected from the correlation curve for α-rich powder.