Browsing by Author "Dale, LS"

Now showing 1 - 7 of 7
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    Analysis of soil extract solutions by direct reading emission spectrometry
    (Australian Atomic Energy Commission, 1976-04) Dale, LS; Matulis, CE
    A rapid spectrometric method was developed for the determination of trace and major elements in aqueous soil extract samples. The rotating disc technique with high voltage excitation was used in conjunction with a direct reading spectrometer. The procedure determines simultaneously zinc, cobalt, lead, copper, nickel, manganese and vanadium at concentrations of between 1 and 1000 mg £-1 together with calcium, magnesium, aluminium and iron at levels usually in excess of 1000 mg £-1. Lutetium is used as an internal standard. The coefficients of variation for all elements range between 2 and 15 per cent.
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    Comparative survey of methods for the determination of uranium in ores
    (Australian Atomic Energy Commission, 1972-08) Florence, TM; Pakalns, P; Dale, LS
    Results are given for an inter-laboratory comparison of methods for the determination of uranium in ores. Four different uranium ores were carefully prepared and samples distributed to eleven participating laboratories. The ores were analysed by several techniques, including spectrophotometric, fluorimetric, X-ray fluorescence, radiometric, and titrimetric procedures. Statistical analysis of the results showed that there was no significant difference between the uranium values found using spectrophotometric, fluorimetric, or X-ray fluorescence methods. An Appendix contains some suggested modifications to the A.A.E.C. bromo-PADAP spectrophotometric method.
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    The determination of oxygen in metals using an impulse heating furnace equipped with a sample transfer lock.
    (Australian Atomic Energy Commission, 1975-05) Dale, LS; de Jong, S; Kelly, JW; Whittem, RN
    An impulse heating furnace has been constructed for the determination of low levels of oxygen down to 100 µg g-1 in metals. The furnace is equipped with a sample transfer lock which permits samples to be loaded into outgassed crucibles in a helium atmosphere. As a result, blank levels in the range 2 to 3 µg oxygen are obtained; the modification also results in shorter sample processing time. The apparatus is described, and its suitability for oxygen determinations at these levels has been verified by comparison of results obtained on reference and analysed materials.
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    A direct reading spectrometer for the determination of beryllium in site liquid effluent.
    (Australian Atomic Energy Commission, 1968-02) Dale, LS
    This report describes a single channel direct reading spectrometer for the determination of beryllium in liquid effluent samples from delay tanks on the site of the Australian Atomic Energy Commission's Research Establishment. The rotating disc technique with pulsed arc excitation is used to determine beryllium down to 0.1 p.p.m. The limit of detection is 0.01 p.p.m. and the coefficient of variation at the 0.1 p.p.m. level is + 20 per cent for a 95 per cent confidence level. The beryllium intensity is depressed by the presence of other constituents in the effluent. Calibration is therefore carried out with standards prepared from a composite effluent solution which yields a similar depression of the beryllium intensity. The results are biased for different tanks and range from + 20 per cent to - 10 per cent. The nature of the depression of the beryllium intensity has been studied in relation to the interference effects of foreign anions and cations and the sensitivity of the method is shown to be affected by pH and by the grade of graphite discs used.
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    Emission spectrochemical analysis of impurities in plutonium dioxide.
    (Australian Atomic Energy Commission, 1967-02) Dale, LS; Hurst, HJ
    A description is given of a method used at the A.A.E.C. Research Establishment for the analysis of impurities in plutonium dioxide. Plutonium is separated from its impurities by adsorption on to anion - exchange resin. The effluent containing the impurities is spectrographically analyzed using a graphite spark technique. Pyrolytic graphite electrodes which are non-porous and do not require sealing are used in preference to the normal greased electrodes which are unsuitable for the analysis of acidic solutions. The plutonium is analyzed for Fe, Al, Mg, Mn, Ni, Cr, Pb, Cd, Co, Ca, Sn, Mo, and Zn using vanadium as internal standard. The overall precision of the method is estimated to be + 20 per cent.
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    Precise determination of hydrogen in metals (with particular reference to zirconium) by the isotopic equilibration-mass spectrometry procedure
    (Australian Atomic Energy Commission, 1971-03) Dale, LS; de Jong, S
    A simple apparatus connected directly to a mass spectrometer enables the fairly rapid determination of hydrogen in metals to be carried out by isotopic equilibration with deuterium. Equilibrium conditions have been established from kinetic studies of the exchange process as a function of heating time. Results for titanium metal standards are in excellent agreement with the certified values, relative standard deviations (1σ) ranging from 3.3 per cent at 300 p.p.m. hydrogen to 0.8 per cent at 200 p.p.m. No standards are available for hydrogen in zirconium, Zircaloy, niobium, vanadium and hafnium. For these metals the equipment has been used to prepare samples with known hydrogen content. Analysis has verified the reliability of the technique. The sample size requirements are 0.1 to 0.5 g (usually 0.25 g) for the range 1000 to 10 p.p.m. hydrogen.
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    Use of a total intensity internal standard for the emission spectrographic analysis of multicomponent alloy systems
    (Australian Atomic Energy Commission, 1977-05) Dale, LS; Matulis, CE
    A summation of the normalised relative intensities of selected spectrum lines of the major components of an alloy is used as an internal standard for the emission spectrographic analysis of a group of alloys. The procedure depends on the sum of the concentrations of the major components being constant but does not rely on prior knowledge of these concentrations. The usefulness of the technique is demonstrated in the analysis of stainless steels, using argon spark excitation with point-to-plane geometry. In principle, the technique should be applicable to other alloy systems.