Elemental speciation is the investigation of the chemical form ofmetal and non- metal containing species in environmental and biological
systems for the determination of species specific essentiality
and toxicity. Speciation analysis is performed by combining modern
separation techniques with state-of-the-art element specific mass
spectrometry. Separation techniques used in this work include: capillary
electrophoresis (CE), high performance liquid chromatography (HPLC) and
gas chromatography (GC). Inductively coupled plasma mass spectrometry
(ICPMS) is the instrument of choice for ultra-trace elemental speciation
analyses due to the excellent sensitivity and selectivity specific to this
mass spectrometer.
Modern innovations in analytical instrumentation
specific for elemental speciation have provided researchers with
resources for the development of new hyphenated techniques and analytical
methods. The specific goal of this dissertation is to describe modern
advancements specific to elemental speciation.
In the first
section a novel interface coupling CE and hydride generation with ICPMS
detection for arsenic speciation is described. The novel concentric
tube interface design allowed for the separation, hydride generation,
and detection of four arsenic species in less than 10 minutes.
The majority of this dissertation focuses on method development for
the analysis of organophosphorus chemical warfare agent (CWA) degradation
products. Recent increases in worldwide terrorist activity as well as the
threat of chemical weapon attacks have led to the demand for rapid and
reliable analytical techniques for CWA analysis. Methods utilizing both
HPLC and GC separation techniques couple with 31P element
specific detection with ICPMS for the analysis of organophosphorus
chemical warfare agent degradation products are described. These works
are the first to utilize 31P detection with ICPMS for the
analysis of chemical warfare agent degradation products.