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

Abstract

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
nebulisation.

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 Award	1986
Original language	English