Thesis-2007-Landon.pdf (16.63 MB)
Download fileThe application of ICP-MS to high matrix samples such as those found in the ceramics industry
thesis
posted on 2014-03-05, 14:17 authored by Mark R. LandonAlthough the benefits of ICP-MS are well documented, the determination of
analytes at low levels in high concentrations of matrix elements has proved
difficult. As ICP-MS is a 'flow into' instrument the deposition of salts throughout
the system is a common cause of significant loss of signal. The application of
desolvation of aluminosilicate samples, to aid in the production of more robust
plasma conditions, was investigated to increase the efficiency of the ICP in
processing the sample. The performance of the ICP-MS was monitored with
different cone arrangements and by running the skimmer cones at elevated
temperatures.
An alternative to modification of the instrument is to employ chemical modification
of the sample and hence the separation of Au and Pt from an aluminosilicate
matrix via the use of solid phase extraction (SPE) columns were investigated as a
means of dealing with high levels of dissolved solids. OVB based SPE columns
were found to give high retentions of Au and Pt when chelated with ammonium
pyrrolidinediethylcarbamate (APOC).
A second alternative that avoided digestion of the aluminosilicate matrices, was to
carry out the analysis using laser ablation (LA). LA-ICP-MS is becoming
increasingly used for trace elemental analysis but as yet no universal calibration
method is available. The general problems associated with matrix matched
standards are inherent as the ablation mechanism and plasma conditions can
differ dramatically with very small changes in matrix composition. Hence the
addition of chromophores was employed to increase the absorption of the laser
energy. The use of vanillic, nicotinic and pyrazinoic acid were used to improve the
ablation of pressed powder discs at the laser wavelength of 213 nm. Synthetic
aluminosilicate discs and standard additions were both employed for the
calibration and determination of Ti.
History
School
- Science
Department
- Chemistry
Publisher
© Mark R. LandonPublication date
2007Notes
A Doctoral Thesis. Submitted in partial fulfilment of the requirements for the award of Doctor of Philosophy of Loughborough University.EThOS Persistent ID
uk.bl.ethos.446481Language
- en