The importance of trace metals and their species is
reviewed and it is recognised that improved methods of
determination are required. High performance liquid
chromatography has grown in importance as a technique,
especially since the synthesis of better column
packings. The adaptability of reverse phase and ion
chromatography with new post-column reagents for
photometric detection for the determination of
transition metal cations, is discussed.
Separation of divalent transition metal by high
performance chromatography was improved by eluents used
in column ion chromatography, new eluents were also
assessed. Lactate eluents were particularly effective
and tartrate, oxalate and thiomalic buffers also showed
promise.
Two photometric reagents, dithizone and eriochrome
black T were used as post-column reagents, sensitivity
and calibration characteristics are determined. A novel
method of photometric detection, observes the decrease
in absorbance of the metallochromic indicator used.
Using lactate eluent with the Eriochrome Black T
post-column detector, linear calibrations from 10 µg
ml to 5 ng mlˉ¹ for cadmium, cobalt, copper,
indium, iron (III), iron (II), lead, magnesium, manganese,
nickel and zinc were achieved with limits of detection
between 0.5 and 5 ng.
The dithizone post-column realtor achieved
quantitative analysis from 10 ng ml to 10 µg
mlˉ¹ for cadmium, cobalt, copper, indium, lead,
nickel and zinc with limits of detection for the lactate
eluent between 1 and 8 ng except for lead(45 ng).
Applications of the eriochrome black T detector are
shown for the speciation of iron and the determination
of transition metals in river water and the analysis of
alloys.
The separation of oxyanions is discussed with
detection by a pyrocatechol violet ternary complex. The
possibility of fluorescent metal detection with
8-hydroxyquinoline-5-sulphonic acid and photometric
detection with a water soluble derivative of dithizone
is shown.
Date of Award | 1985 |
---|
Original language | English |
---|
Awarding Institution | |
---|
The Determination of Trace Metals by High Performance Liquid Chromatography with Photometric Detection
Hobbs, P. J. (Author). 1985
Student thesis: PhD