Inductively Coupled Plasma Atomic Emission Spectroscopy for the Analysis of Trace Elements in Boron Materials

  • Peter Hulmston

    Student thesis: Doctoral ThesisDoctor of Philosophy


    An investigation into the application of inductively
    coupled plasma atomic emission spectroscopy (ICP/AES) to the
    quantitative determination of trace level multi-element impurities
    in boron materials has been undertaken. Two ICP-Spectroscopic
    systems were developed and applied. An ICP-Spectrograph system,
    which uses photographic detection and computer controlled microdensitometry
    for plate evaluation, provided wide element coverage
    and is well suited to dealing with complex emission spectra. The
    ICP-Scanning monochromator system, which is equipped with photoelectric
    detection, gave the better sensitivity and precision.
    Combined, the two systems provided useful detection limits
    (typically <1 ppm), good accuracy and precision for 50 elements.

    In order to apply ICP/AES to cases where the sample
    quantity was limited a recirculating nebuliser was developed and
    tested. A xl0 improvement in efficiency over conventional methods
    of nebulisation was achieved without any deterioration in
    sensitivity or precision. A microprocessor controlled version
    provided a suitable approach to routine analysis and a detailed
    study into the nebulisation characteristics showed that the
    nebuliser was free from the instabilities apparent in other designs
    of closed system nebulisers.

    Sample introduction by hydride generation was
    investigated and provided ng/ml detection limits for several
    elements which were not sufficiently sensitive by pneumatic

    A comparison of ICP/AES, neutron activation analysis and
    spark source mass spectrometry showed that only by using all three
    techniques could the full requirements be met. ICP-Mass spectrometry
    and X-ray fluorescence have been examined and preliminary
    assessments indicated that both techniques have considerable
    potential for boron analyses.
    Date of Award1986
    Original languageEnglish


    • Inductively
    • coupled plasma
    • atomic emission
    • spectroscopy
    • trace element analysis
    • boron

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