United States
Environmental Protection
Agency
Industrial Environmental Research
Laboratory
Research Triangle Park NC 27711
Research and Development
EPA-600/S7-84-057 June 1984
Project Summary
Stable Isotope Dilution for
Hazardous Waste Incineration
P. W. Ryan
This research project was undertaken
with the general objective of evaluating
the potential utility of isotope dilution
gas chromatography/mass spectrom-
etry (GC/MS) in chemical analysis
related to incineration of hazardous
waste materials. The specific objective
was to determine if a proposed catalytic
exchange procedure could be adapted
to produce the labeled analog materials
necessary for isotope dilution GC/MS
analysis.
The proposed deuterium exchange
technique is described along with ex-
periments designed to test its applica-
bility. Results of the experiments show
that the technique can be successfully
applied to certain limited classes of
hazardous waste materials, but they do
not indicate sufficient versatility to meet
the most general needs of hazardous
waste incineration programs.
This Project Summary was developed
by EPA's Industrial Environmental Re-
search Laboratory, Research Triangle
Park. NC, to announce key findings of
the research project that is fully docu-
mented in a separate report of the same
title (see Project Report ordering infor-
mation at back).
Introduction
For purposes of evaluating and moni-
toring hazardous waste incineration pro-
cesses, the chemical analysis of influent
streams, effluent streams, and fugitive
emissions may be frequently required,
and combined GC/MS is a suitable
analytical technique for much of that
chemical analysis. Experience in related
analytical applications, for example
GC/MS determination of priority pollu-
tants in wastewater, has demonstrated
that the highest quality GC/MS analytical
data are obtained when isotope dilution
techniques are employed.
A major impediment to the use of
isotope dilution is the difficulty of obtain-
ing isotopically labeled analogs of the
target compounds for which analytical
data are required. Analogs are commerci-
ally available for about 50 of the priority
pollutant compounds, but must be ob-
tained by custom synthesis for use with
other substances, which severely limits
the extension of isotope dilution tech-
niques to new areas.
A proposal for circumventing this limita-
tion would use a catalytic exchange
technique to prepare deuterium labeled
materials at considerably less expense
than custom synthesis. There is evidence
that certain catalytic exchange techniques
• will produce tritium labeling in a non-
specific manner, that is not selective by
compound type, in complex organic mix-
tures devised from oil shale processing.
The object of this research project is to
assess the potential utility of catalytic
exchange for producing deuterium labeled
materials which are suitable for use as
isotope dilution analogs to hazardous
waste materials. If deuterium labeling
could be achieved starting with complex
mixtures, perhaps even with the inciner-
ator influent itself, then an inexpensive
and broadly applicable means would have
been found to extend isotope dilution
GC/MS analysis to a number of new
areas.
Conclusions
Catalytic exchange is not a simple
general technique that can be used to
generate deuterium labeled analogs of
hazardous wastes. It is, however, a tech-
nique that could prove valuable in applica-
tion to more limited classes of materials.
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The'technique shows a surprising capa-
bility to produce labeled analogs thor-
oughly, extensively, and specifically for
several phenols, polynuclear aromatic
hydrocarbons, and some other species.
For the compounds that are deuterated,
the product materials are suitable for use
as isotope dilution GC/MS standards or
as spiking materials for process character-
ization.
Based on the data generated in this
study for a selected set of compounds, the
major limitation of the technique seems
to be its lack of generality. For most
compounds and compound classes repre-
sented in the test mixture, no useful
labeled analogs were isolated from the
reaction vial.
Recommendations
This study has demonstrated that cata-
lytic exchange can be successfully applied
in specific cases, but without further
development it is not applicable to waste
materials in general. The unsuccessful
applications deserve further study to
determine whether simple methodology
revisions can resolve the problem. Time
of exposure to catalyst and selection of
extraction solvents are simple, potentially
useful variations of techniques which
might very well extend the list of suitable
compound classes.
This study has addressed the labeled
analog problem only in very general
terms, and has indicated some potentially
fruitful applications of catalytic exchange
in the area of hazardous waste analysis.
Further work could focus on explicit needs
of specific programs, with emphasis on
optimizing experimental techniques for a
specified, limited set of materials. Poly-
chlorinated biphenyl (PCB) incineration
efficiency, phenol containing wastewater
cleanup, or fugitive emissions of organic
species from synf uels processes might be
appropriate choices for areas of further
study.
P. W. Ryan is with S-Cubed. La Jolla. CA 92O38.
Merrill D. Jackson is the EPA Project Officer (see below).
The complete report, entitled "Stable Isotope Dilution for Hazardous Waste
Incineration," (Order No. PB 84-189 828; Cost: $8.50, subject to change) will
be available only from:
National Technical Information Service
5285 Port Royal Road
Springfield, VA22161
Telephone: 703-487-4650
The EPA Project Officer can be contacted at:
Industrial Environmental Research Laboratory
U.S. Environmental Protection Agency
Research Triangle Park, NC 27711
•&• U.S. GOVERNMENT PRINTING OFFICE. 1984 — 759-015/7719
United States
Environmental Protection
Agency
Center for Environmental Research
Information
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Official Business
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