United States
Environmental Protection
Agency
Environmental Monitoring Systems
Laboratory
Las Vegas NV 89114
Research and Development
EPA-600/S'4-84-038 June 1984
Project Summary
Characterization of Hazardous
Waste Sites—A Methods
Manual: Volume III. Available
Laboratory Analytical Methods
Russell H. Plumb, Jr.
A manual of available analytical pro-
cedures was prepared as Volume 3 of
the report. Characterization of Hazard-
ous Waste Sites—A Methods Manual.
This volume provides bench-level guid-
ance for the preparation of hazardous
waste, water, soil/sediment, biological
tissue, and air samples, and suitable
methods that can be used to analyze the
resultant digests/extracts for 244 of
the 359 substances listed in the Re-
source Conservation and Recovery Act
(RCRA) permit regulations. Each sam-
ple preparation procedure and analytical
method for the 929 analyte-matrix
combinations that have been accumu-
lated in this volume is classified as
either evaluated or available based on
the availability of precision and accuracy
data.
This Project Summary was developed
by EPA's Environmental Monitoring
Systems Laboratory, Las Vegas, NV. to
announce key findings of the research
project that is fully documented in a
separate report of the same title fsee
Project Report ordering information at
back).
Introduction
The RCRA regulations concerned with
the proper handling and disposal of
hazardous wastes specify 359 chemical
substances of concern. The bench-level
guidance needed to implement the regula-
tions should cover the topics of collection,
preparation, and analysis of samples from
diverse and complex matrices such as
wastes, water, soil/sediment, biota, and
air. However, existing analytical manuals
are frequently dedicated to a single
sample matrix (usually water) and nor-
mally provide detailed guidance on the
use of analytical procedures for only 50 to
125 substances. This manual is an expan-
sion of these earlier efforts and provides
guidance on the preservation and prepa-
ration for more sample matrices, as well
as analytical methods for more analytes.
This project is part of a larger effort to
prepare guidance manuals summarizing
available information on hazardous waste
site characterization, including prelimi-
nary site assessment, sample collection,
and sample analysis.
Organization of the Manual
Volume 3 of Characterization of Hazard-
ous Waste Sites—A Methods Manual
contains analytical procedures that are
available for chemical characterization of
samples obtained in hazardous waste site
investigations. The text of this volume is
divided into three chapters. Chapter 1
provides background information on the
development of this manual and a dis-
cussion of the format used to present
each analytical procedure. Chapter 2 is
divided into two main parts: the first
provides guidance for handling and frac-
tionation of hazardous waste samples in
the laboratory and the second provides a
protocol for general sample characteriza-
tion, identifying potentially unsafe condi-
tions that may be encountered when
certain samples are analyzed (i.e., pres-
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ence of strong oxidants, evolution of
potentially toxic gases, and/or extreme
pH values). Chapter 3 presents analytical
procedures for specific analytes.
A search of the literature, including
both existing manuals and professional
journals, was instituted to identify avail-
able methods. The search focused on
methods for the analysis of hazardous
waste, water, soil/sediment, biological
tissue, and air samples for any of the 359
compounds listed in the RCRA regula-
tions. A procedure was considered suit-
able for inclusion if the following criteria
were met:
• A demonstrated need exists for the
procedure.
• Detailed sample preparation guidance
is provided for a specific sample matrix.
• The analytical procedure is adequately
described.
• Precision and accuracy information is
available to define the expected per-
formance of the procedure.
The first criterion was satisfied if the
analyte was listed in Appendix VIII of the
RCRA regulations.* The second criterion
was considered to have been met if
detailed sample preparation guidance
(including digestion and/or extraction,
and sample extract cleanup) was avail-
able. The third requirement was satisfied
if sufficient information on instrument
operation (warm-up time, instrument
calibration, and operating conditions) was
located. The last criterion was satisfied if
method performance data were available
from one or more laboratories.
The search produced 929 analyte-
matrix combinations that fulfilled the
criteria (163 analytes in waste, 244
analytes in water, 203 analytes in soil/
sediment, 217 analytes in biological
tissue, and 102 analytes in air). These
methods are presented in 24 analytical
sections that are grouped as follows:
Section 1-9: Organic Analytical Pro-
cedures
Section 10-18: Inorganic Analytical Pro-
cedures
Section 19-24: Sample Screening and
Characterization Proce-
dures
The organic sections provide detailed
procedures for the determination of vola-
tile organic compounds, acid-extractable
compounds, base/neutral compounds,
pesticides and PCBs, organophosphorus
pesticides, organonitrogen pesticides,
phenyl acetic acids, dioxin, and poly-
nuclear aromatic hydrocarbons. The in-
organic sections provide detailed proce-
dures for elemental determination by
atomic absorption and inductively coupled
plasma emission spectroscopy, and pro-
cedures for mercury, methyl mercury,
arsenic, selenium, cyanide, sulfide, and
ammonia. Analytical methods in the
screening section provide guidance for
the determination of oxidant capacity,
reductant capacity, acidity, alkalinity,
conductivity, and percent moisture con-
tent.
A standard format was developed for
presenting the information on sample
preparation and the use of each analytical
procedure. This approach permits analyt-
ical research needs to be identified in
several ways. Each method is classified
as evaluated or available based on the
amount of precision and accuracy data
that was located. Methods classified as
available are usable, but a need exists for
a more extensive performance evaluation
of the procedure. Research needs are
further identified by reserving sections
whenever sample preparation guidance
could not be located for a particular
analyte-matrix combination. Sections
identified in this manner indicate a need
for either a more extensive literature
search, a performance evaluation of an
existing procedure, or a methods develop-
ment and evaluation effort. Finally, in-
formation on sample preservation and
preparation is presented in a flowchart
associated with each analytical section.
Gaps in these flowcharts identify needs
for specific performance evaluations.
This volume will require periodic up-
dating as additional analytical procedures
are located, as new methods are devel-
oped and evaluated, and as additional
performance data become available to
update the classification of methods
already included.
•U.S. Environmental Protection Agency. "Hazardous
Waste and Consolidated Permit Regulations,"
Federal Register. 40 CFR Part 261. May 19. 1980.
pp. 33084-33133.
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Russell H. Plumb, Jr., is with Lockheed Engineering and Management Services
Company, Las Vegas, NV 89114.
Werner F. Beckert is the EPA Project Officer (see below).
The complete report, entitled "Characterization of Hazardous Waste Sites, A
Methods Manual: Volume III. Available Laboratory Analytical Methods, "(Order
No. PB 84-191 048; Cost: $47.00, subject to change) will be available only from:
National Technical Information Service
5285 Port Royal Road
Springfield, VA 22161
Telephone: 703-487-4650
The EPA Project Officer can be contacted at:
Environmental Monitoring Systems Laboratory
U.S. Environmental Protection Agency
P.O. Box 15027
Las Vegas, NV 89114
it U S GOVERNMENT PRINTING OFFICE, 1984 — 759-015/7722
United States
Environmental Protection
Agency
Center for Environmental Research
Information
Cincinnati OH 45268
Official Business
Penalty for Private Use $300
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