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Development and some applications of techniques for the determination of trace metals by furnace atomic absorption spectrometry

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Noller, BN (1978) Development and some applications of techniques for the determination of trace metals by furnace atomic absorption spectrometry. PhD thesis, University of Tasmania.

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Abstract

The role of the analytical chemist is considered with respect to
the impact of new trace analytical techniques on environmental science.
Reference is made to the role of atomic absorption spectrometry (AAS),
particularly furnace AAS, anodic stripping voltammetry (ASV) as an
alternative to the latter and important factors influencing precision
and accuracy in trace analysis.
Application of trace analysis techniques to study atmospheric
elemental particulates (distinct from volatile molecular species) and
important related factors are reviewed. Supporting data from studies
using high volume particulate sampling and flame AAS methods were
undertaken to provide comparative data for studies indicated below.
Micro-air sampling techniques based on furnace AAS were improved
and further developed into routine methods for particulate collections
(Pb, Cd, Zn, Cu) using graphite cups (with inserted discs of Millipore
membrane and graphite cups alone) as air-filtration device and simultan~
eous furnace atomizer. Emphasis was placed on the identification and
elimination of contamination using a modified procedure and use of an
alternative practical graphite cup sample container system. Other
factors investigated were the physical properties of graphite cups and
associated collection devices, nature of particle penetration through
various filter media anrl significance of meteorological parameters.
Unique studies undertaken covered the spectrum of particulate levels
likely to be found (elements indicated as particulates in aerosols
containing <100 to >10 (to the power) 8 total particles cm- 3). These include the time
variation of Pb atmospheric particulates in urban and baseline conditions,
identification of source types by time variation with wind speed and direction, short term measurement and time variation of atmospheric Pb
as "fall-out" and the direct measurement of Pb and Cd in cigarette
mainstream smoke. from single cigarettes. The overall applicability of
micro-air sampling techniques for elemental particulate measurements is
summarized with respect to the contents of the given review.
The role of trace analytical techniques for the determination of
trace elements in biological systems is considered with particular
reference to furnace AAS and the determination of the elements Pb (nonessential)
and Cu (essential) in blood. Furnace AAS methods for Pb and
Cu based on blood solutions in 5% Triton X-100 (from a method described
for Pb 'in blood) were developed and evaluated through studies of accuracy
and precision. Comparison with the alternative technique ASV, was made
for Pb. The blood Pb method was applied to survey levels in Hobart dogs·
and cats and indicated dogs were potential environmental Pb monitors.
The blood Cu method was applied to survey children and adults from Hobart
and environs and showed the possibility of pin-pointing individuals
(categorized as healthy) with certain physiological and pathological
conditions.
A fundamental study concerning the nature of high temperature
molecular species with respect to- furnace AAS was undertaken using Raman
spectrometry. A high temperature furnace (of unique design) was
constructed, based on a Perkin Elmer HGA-70 "Heated Graphite Atomizer"
to permit recording of Raman spectra (Cary 82 laser Raman spectrometer,
Ar+ excitation) of the vapours from Zn, Cd, Pb halide and phosphate
systems (individually and mixed with alkali halides) in sealed silica
tubes and over a temperature range 300-ll00°C. Interpretations in
terms of vapour species lost during drying, ashing and atomize furnace
AAS cycles are made, with special reference to vapour complex formation.
The use of the Raman spectrometer as detector to measure molecular
concentrations (technique analogous to furnace AAS) based on properties'
of the Raman and associated effects is proposed.

Item Type: Thesis (PhD)
Keywords: Atomic absorption spectroscopy, Trace elements
Copyright Holders: The Author
Copyright Information:

Copyright 1978 the author

Additional Information:

Includes bibliographical references. Thesis (Ph.D.)--University of Tasmania, 1978

Date Deposited: 03 Feb 2015 03:07
Last Modified: 11 Mar 2016 05:56
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