Research Interests
My research interests fit broadly into two categories; sample introduction
methods for atomic spectrometry and the measurement of trace metals in
the environment.
Sample Introduction Methods for Atomic Spectrometry
Sample introduction has been the archilles heal of atomic spectrometry
methods for several decades. Traditionally, sample materials are converted
to liquids prior to analysis of elemental composition by atomic spectrometry.
This ensures homogeneity of the sample components and ease of transport
to the instrument. Common atomic spectrometric techniques use a flame or
plasma to achieve atomization. The problems come when trying to introduce
a liquid into a flame or plasma. Normal liquid sample introduction is extremely
inefficient usually allowing only a small proportion of the sample to enter
the spectrometer as small droplets while the rest goes to waste. I have
been interested in a couple of possible methods for increasing the efficiency
of sample introduction for atomic spectrometry.
Desolvation
Desolvation is method for reducing the amount of solvent introduced into
an atomic spectrometer. The general principle is to heat an aerosol
of the sample in order to evaporate the solvent, then remove the solvent
vapor using a condenser or drier. This essentially introduces a dry aerosol
of the sample into the spectrometer. Desolvation should allow a much
larger percent of the sample material to be analyzed. Most desolvation
methods, however, are not as efficient as expected and suffer from problems
such as memory effects and pressure fluctuations. One attractive
alternative to thermal heating is the use of microwave energy. Microwave
methods would be expected to heat more efficiently and evenly than thermal
methods due to the direct heating of aerosol droplets. (Fig.
1). Experimental results have been disappointing because of the inefficient coupling
of microwave energy with small droplets.
Projects:
"Numerical Analysis of Sprayed Sample Enrichment via Microwave Heating."
- Kevin Douglass, Undergraduate Project, Marist College (2001).
Presented at Mid-Hudson Section ACS Undergraduate Research Symposium,
New Paltz, NY (April 2001) and FACSS Conference, Detroit, MI (October 2001).
"Feasibility of a Desolvation System based on Direct Microwave Coupling
with an Aqueous Aerosol"- Kevin Douglass, Neil Fitzgerald, Bradley Ingebrethsen
and Julian F. Tyson, Spectrochim. Acta Part B. (in preparation).
Chemical Vapor Generation (Fig.2)
An alternative to liquid sample introduction is to chemically produce a volatile
form of the analyte that can be introduced to a spectrometer
in the gas form without introducing solvent. This can be achieved
efficiently for some elements (such as arsenic, selenium, tin, and lead)
by formation of the volatile hydride. Mercury is known to produce
a volatile elemental form in reducing conditions and has been used as a
standard method for mercury analysis for many years. Recently,
cadmium has been found to produce an atomic vapor allowing detection
in the low parts per trillion (ng/L) although the reaction mechanism remains
unclear. Evidence is also beginning to emerge to suggest that other
elements (such as gold, platinum, palladium and rhodium) may be determined
at low levels using similar techniques.
Projects:
"Trace Level Determination of Cadmium in Environmental Samples by Cold
Vapor Atomic Absorption Spectrometry" - Rebecca Wack, Undergraduate Project,
Marist College (completed May 2002).
Presented at the Mid-Hudson Section ACS Undergraduate Research Symposium
,New Paltz, NY (April 2002) and FACSS Conference, Providence, RI (October 2002).
Trace Metals in the Environment
Many trace elements in the environment are responsible for toxicity and
have significant environmental impact. The study of trace metals
can also give useful insight into the chemistry and physical process in
environmental systems. I have recently been involved in two areas
of study of trace metals in the environment.
Toxicity and Analysis of Metals Deposited from Automobile Catalytic Converters
This is a project performed in collaboration with Dr. Gagnon (Marist College)
looking at toxicity and levels of platinum, palladium and rhodium in the
environment. Several researchers have observed an increase in the
levels of these metals (although levels are currently very low) particularly
in roadside soil due deposition from catalytic converters. As there
does not seem to be a natural sink for these metals, it can be expected
that concentrations will continue to rise. Questions remain as
to the ability of metals to become mobile and absorbed into the food chain
and the toxicity of metal species to plants and animals (Fig.
3). There also appears to be an increasing need to reliably measure
and monitor these elements with relatively low cost, common instrumentation.
Projects:
"Study of Accumulation and Bioavailability of Platinum Group Metals
in Tomato Plants and Sphagnum" - Carrie Shapiro and Julie Gosewisch,
Undergraduate Project, Marist College (completed, May 2002)
Presented at the Eastern Colleges Science Conference, Niagara Falls, April 27th 2002
Study of Trace Metal Variations in Streams (Fig. 4)
The concentrations of trace metals in streams are strongly dependent on
local conditions such as acidity, temperature, recent weather events (rainfall,
snow melt, drought) and chemical composition. These variations can
often be explained by simply chemical concepts such as solubility, and chemical
reactivity. Many metals also have significant impact on the environment
due to their toxicity (e.g. aluminum, lead, and cadmium). The
study of trace metals variations in different stream types can, therefore,
provide much useful information about the chemical and physical mechanisms
involved.
Projects:
"Study of Trace Metal Variations in Buffered and Poorly Buffered Streams
in the Mohonk Reserve as a Function of Acidity and Temperature" - Neil
Fitzgerald, Marist College, in collaboration with Kathleen Weathers and
Denise Schmidt (Institute of Ecosystem Studies, Millbrook, NY), and Dr. Feldman (Marist College), funded
by the John S. Eaton Fellowship (expected completion June 2002).
· "Benthic Ecology and Chemistry of the Coxing Kill and Tributary in the Shawangunk Mountains" Richard Feldman, Vincent Porzio, Ryan Streck and Neil Fitzgerald,
poster presentation, The Northeast Natural History Conference, SUNY Albany, April 25th 2002