ANNOTATED BIBLIOGRAPHY OF ANALYTICAL METHODS FOR CERCLA
HAZARDOUS SUBSTANCES
by
H. B. Kerfoot, J. L. Engels, D. F. Arnold, and A. R. Bujold
Lockheed Engineering and Management Services Company
Las Vegas, Nevada 89114
Prepared for the
Office of Emergency and Remedial Response
Contract Number 68-03-3050
Project Officer
Werner F. Beckert
Quality Assurance Division
Environmental Monitoring Systems Laboratory
Las Vegas, Nevada 89114
ENVIRONMENTAL MONITORING SYSTEMS LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
LAS VEGAS, NEVADA 89114
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NOTICE
Although the research described in this report has been funded wholly or
n part by the U.S. Environmental Protection Agency through Interagency
Agreement 68-03-3050 to the Lockheed Engineering and Management Services
Company, Las Vegas, Nevada, it has not been subjected to Agency policy review
.nd therefore does not necessarily reflect the views of the Agency. Mention
if trade names or commercial products does not constitute endorsement or
ecommendation for use.
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CONTENTS
Page
Figures and Tables iv
Executive Summary v
Acknowledgment viii
Glossary ix
Registered Trademarks xii
Introduction 1
Background 1
Scope 3
Purpose 4
Contents and Use of This Report 6
Contents 6
Reportable quantity values and safety information 7
Method descriptions 8
Use of this report 11
General 11
Compound-specific use 11
Multicompound uses 13
Report Preparation 14
Method search 14
Cost search 18
Factors influencing cost figures 19
Results 24
Background 24
General 24
Sampling 25
Sample preparation 26
Analyte determination 26
Technical results 26
Organic listings 29
Inorganic listings 34
Financial results 38
Mobile laboratory survey results 39
Instrumentation 39
Procedures 39
Cost factors 44
References 45
Appendices (Separate Volumes)
A. Analytical Methods Available A-l
B. Multi-Compound Methods B-l
C. The F and K Waste Streams under the Resource Conservation and
Recovery Act of 1976 (RCRA) C-l
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FIGURE
Number page
1 Flow chart depicting use of the Appendices 12
TABLES
Number Page
1 Method Sources 15
2 Examples of Costs for Frequently Mentioned Methods 22
3 Substances for Which Single- or Multicompound Methods
Were Located 27
4 Number of Substances for Which Methods Were Located 28
5 Organic Compounds for Which Gas Detector Tubes Are Available ... 31
6 Inorganic Substances for Which Gas Detector Tubes Are Available . . 35
7 Elements Determined by X-Ray Fluorescence 35
8 Analytes that can be Determined in Water Samples Using Test Kits. . 37
9 Inorganics Measured in Water and Soil Samples Under CERCLA 38
10 Method and Cost Search Results 38
11 Instruments Used in Selected Commercial Mobile Laboratories .... 40
12 MERL-Edison Mobile Laboratory Responses and Analytes 41
13 Hazardous Compounds Analyzed by the MERL-Edison Mobilie
Laboratory 42
iv
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EXECUTIVE SUMMARY
Measurement of the magnitude and distribution of releases of hazardous
substances is required in support of efforts under the Comprehensive Environ-
mental Response, Compensation, and Liability Act of 1980 (CERCLA). A Compre-
hensive Hazardous Substances List (the List), comprised of substances specified
in Sections 311 and 307a of the Clean Water Act, Section 112 of the Clean Air
Act, and the P and U Lists and F and K Waste Streams of the Resource Conserva-
tion and Recovery Act (RCRA), delineates the substances under the purview of
CERCLA. The Comprehensive Hazardous Substances List contains approximately 617
unique listings, of which about two-thirds pertain to organic compounds and
one-third to inorganic or organometallic substances.
Under Section 102(b) of CERCLA, each substance on the List is assigned a
Reportable Quantity (RQ) value that specifies the amount of the substance, the
release of which must be reported to the National Response Center. The U.S.
EPA Office of Emergency and Remedial Response (OERR) is considering adjustment
of these RQ values, and in order to do so requires information about the techni-
cal feasibility and financial impact of measurements of releases of hazardous
substances. This report provides such information in support of the OERR
rulemaking effort.
This report discusses the state of the art of analytical chemistry in the
context of CERCLA, and presents the results of a search for specific analytical
methods for each substance under the purview of CERCLA in three media - air,
soil, and water - at two levels of sophistication - field analyses and labora-
tory methods. This report is not a critical review, but a non-critical survey,
and deals only with demonstrated analytical methods. Specific facts about each
analytical method located are presented as Method Descriptions. The Method
Descriptions comprise an annotated bibliography, and each one gives a method
summary, the interferences listed, the quality control prescribed, the EPA/
technical status or sensitivity of the method, the reference, and the cost of
analysis by that method. The Method Descriptions are in two Appendices - A
and B - for single- and multicompound methods, respectively. By a single-
compound method the authors mean a method demonstrated to be applicable to the
determination of only one compound on the List, although it may also have been
demonstrated to be applicable to compounds not on the List. Appendix C gives
rudimentary guidance to appropriate analytical methods for the RCRA F and K
Waste Streams, within the framework of Appendices A and B.
Overall, field methods have been located for 34 percent of the 1,851 possi-
ble compound/matrix combinations, and laboratory methods for 80 percent of them.
Analytical methods seem better developed for inorganics than for organics at
first glance, but most methods located for the determination of inorganics are for
only a portion of the whole compound and, as such, do not unequivocally identify
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or measure the CERCLA-hazardous substance, as required by CERCLA. For a total of
596, or 96 percent, of the 621 possible inorganic substance/matrix combinations,
one or more laboratory methods were located. For organic compounds, laboratory
methods were located for 71 percent of the possible substance/matrix combinationr
These methods are usually satisfactory for at least tentative identification of
the analyte. Field methods for organics, without the sophistication of laboratory
equipment, were located for only 21 percent of the possible 1230 organic
compound/matrix combinations.
The weakest technology for any analyte/matrix/level-of-sophistication
combination was found to be in the field analysis of soil samples for organic
compounds. This type of method was located for only 19 analytes. Field analy-
sis of soil/sediment samples for inorganic substances was also found to be weak,
with only 67 substances accounted for. As in nearly all of the inorganic pro-
cedures, these methods are typically elemental methods, not compound-specific
ones, and do not identify the substance as a CERCLA compound, as required under
CERCLA. Field water and air analytical methods, in combination with novel
sample preparation procedures, could be applied to broaden the scope of both
organic and inorganic field analyses. Similarly, empty spots in other tech-
nologies could be filled by the development of sample preparation procedures and
utilization of existing analytical methods. However, the most promising way
of conducting field site characterization is the use of mobile laboratories and
laboratory equipment manufactured to be field-portable. These two types of
analysis would allow methods of higher technology, once restricted to fixed-
site use, to be used in the field. Additionally, use of the broad listings of
all compounds of a given type (e.g., 'cyanides', 'arsenic and compounds') in
regulations would help match the regulatory situation to analytical capabili-
ties, since inorganic analytical capabilities would then match the regulations
more closely.
The cost of analysis has been obtained from one of three sources: bid
prices from government contracts, list prices from commercial analytical facil-
ities, or price estimates based on individual cost of each step in the anal-
ysis. The cost for the determination of organic compounds ranges from approxi-
mately $75.00 to $300.00 per sample for laboratory analysis of lots of six
samples, while field analysis costs vary from $5.00 to $40.00 per sample.
Inorganic analysis costs vary from a range of approximately $15.00 to approxi-
mately $175.00 per sample for laboratory analysis of lots of six samples to a
range of $5.00 to $40.00 for field analysis. Cost figures given do not include
sampling costs, except for field analysis figures.
The availability of analytical methods is necessary, both for compliance
by the regulated community with Superfund rules and regulations, and for
enforcement of them by the EPA. With no field or laboratory analytical methods
located for approximately 35 substances in air, water, or soil samples, strict
enforcement of and compliance with Superfund regulations becomes impossible in
cases of releases of those substances. In addition, EPA enforcement efforts
and citizen compliance are made difficult or impossible by the sparseness of
analytical methods for many of the other substances on the Superfund Comprehensive
Hazardous Substances List. Furthermore, much of the technology located in the
method-search effort for this report has not been evaluated by the EPA, and the
location of the information is often not known to the regulated community, or
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even to EPA personnel. This Annotated Bibliography should partially alleviate
these problems. To make the information contained in this report easily
available to regulators and users, it is at present being investigated
if computerizing this report is feasible.
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ACKNOWLEDGMENT
The authors wish to acknowledge 0. John Logsdon of Rocky Mountain
Analytical Laboratories, Arvada, Colorado, and Dan Grove and Jack Custer of
Alert Laboratories, Canton, Ohio, for providing detailed pricing and
cost information. We also wish to acknowledge the technical assistance of
Joseph Sherma, Lafayette College, in furnishing methods in the process of a
particularly thorough review of the interim and final versions of this docu-
ment. Mr. Phil Malley and Mr. Robert Scavetta of Lockheed EMSCO helped greatly
by reviewing and editing the Appendices of the report. In addition, we wish to
acknowledge the especially useful advice on format and document preparation
from Ms. Donna Nidy and Cindy Stine of the CSC Associates Word Processing
Center at EMSL-Las Vegas. J. Gareth Pearson of the EPA EMSL-Las Vegas was
particularly helpful in crystallizing important document features and furnish-
ing advice on format in the initial phases of the project.
viii
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GLOSSARY
Absorption
Adsorbent
Adsorption
Analyte
Breakthrough volume
Bubbler
Calibration
Composite sample
Cumulative sample
Cryogenic
collection
Derivatization
Desorption
Elute
- the process of trapping an analyte in a liquid or solid.
the solid material on the surface of which adsorption
occurs.
the process of trapping an analyte on the surface of a
solid.
molecule or ion for which analysis is being performed.
the volume of air which, when sampled, begins to allow
analyte to escape from the sampling medium.
sampling device consisting of a gas dispenser immersed in
an absorbing liquid.
- the establishment of a relationship between the response
of a measurement system and the amount of analyte present,
usually by measurement of the response due to several
calibration standards, in order to quantify the amount
of analyte in samples.
a sample composed of two or more increments.
a sample that is an average sample over a time period.
The collected sample is retained in a single vessel or
the separated component accumulated in one place.
- a sampling process wherein an air sample is passed
through a trap cooled by liquid argon, ice, or similar
material in order to collect volatile compounds.
process wherein the analyte is converted to another
chemical species through chemical reaction.
the process of releasing a substance from a sorbed
(trapped or fixed) state by elution or heating.
to remove sorbed materials from a sorbent by use of a
fluid.
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Filter
Functional group
Immiscible
Impinger
Instantaneous
sampling
Interference
Internal standard
Matrix
Sample matrix
Matrix effects
Method blank
Moiety
Molar
- a porous material used to separate solids from liquids
or gases. (See Reference 12 for a detailed discussion
of use and specifications of filters for air sampling.)
a particular configuration or group of atoms in an
organic molecule.
liquids that do not combine to make one phase, or a
solution.
- see "Bubbler".
- obtaining a sample in a time period that is negligible
compared to the time scale of fluctuations in the level
of analyte present.
a substance that interferes with an analysis by
obscuring the true signal from the analyte, making the
analyte inactive towards detection, or making the analyte
unavailable for detection.
a known quality of a reference compound added to a
collected sample, and generally to standards as well,
for use in quantification of other compounds (see
"calibration").
Limit of detection -
the minimum quantity or concentration of analyte which
produces a measurable response, that is, a signal above
the noise level. The "instrumental detection limit" and
"method detection limit" refer to the limit of detection
in terms of the amount or concentration of analyte
introduced into the instrumental measurement system and
the amount or concentration of analyte carried through
the complete analytical process, respectively.
- The type of material containing the analyte (e.g., air
water, soil).
interferences in an analysis due to substances present
in the specific sample matrix of a particular sample.
an artificial sample containing no analyte (e.g.,
distilled water), used to check for contamination of
samples during analysis.
part or all of a compound (e.g., atom, ion, molecule).
pertaining to a solution containing one mole (6 x
atoms/ions/molecules) solute per liter of solution.
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Phase
Quantification
a physically separate part of a heterogeneous system.
- the assignment of a numerical value to the amount or
concentration of analyte in a sample.
Reference standard -
Sensitivity
Solute
Sonication
Sorbent -
Soxhlet extraction
TFE
a solution or sample of a precisely known concentration,
used to assess the accuracy of an analysis.
the amount or concentration of analyte that will produce
a certain level of response, such as 1 percent (0.044
absorbance units), from an analytical instrument.
- the substance dissolved in a solvent.
a method of adding energy, to aid in an extraction,
in the form of sound waves.
a solid or liquid which traps or fixes an analyte by
absorption or adsorption.
a particularly efficient manner of extracting analytes
from solid samples, using continuous-flow contact of
the sample with warm solvent.
a fluorocarbon plastic that does not contain plasticizers
that leach into solutions.
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Registered Trademarks
Trademark
Company
Alka-Seltzer®
Amberlite®
Asbestest®
Auto-Analyzer®
Bendix/Gastec®
Bromo-Seltzer®
Florisil®
Guthion®
Hach®
Mylar®
Miles Laboratory, Inc.
1127 Myrtle Street
Elkhart, Indiana 46514
Rohm and Haas Company
Independence Mall West
Philadelphia, Pennsylvania
19105
E.G. Apparatus Corporation
3831 Tyrone Blvd. North
St. Petersberg, Florida 33709
Technicon Corporation
511 Benedict Avenue
Tarrytown, New York 10599
Bendix Corporation, EPID
12345 Starkey Road, Suite 8
Largo, Florida 33543
Warner-Lambert Pharmaceutical Company
201 Tabor Road
Morris Plains, New Jersey 07950
Floridin Company
3 Penn Center
Pittsburgh, Pennsylvania
15225
Chemagro Corporation
P.O. Box 4913
Kansas City, Missouri
64120
Hach Company
P.O. Box 389
Loveland, Colorado
80539
E.I. DuPont de Nemours and Company,
Inc.
1007 Market Street
Wilmington, DE 19898
(continued)
xii
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Trademark
Company
Norit A®
Nuchar®
Phaltan®
Porapak T®
Quantofix®
Stractan® 10
Teflon®
Tenax®
Zincon®
American Norit Company, Inc.
6301 Glidden Way
Jacksonville, Florida 32208
West Virgina Paper and Pulp Company
New York, NY 10017
Chevron Chemical Company
200 Bush Street
San Francisco, California 94120
Waters Associates, Inc.
34 Maple Street
Milford, Massachusetts 01757
Macherey-Nagel and Company
Postfach 307, 516 Duren, Germany
Available from:
Gallard-Schlesinger Chemical
Mfg. Corp.
584 Mineola Avenue
Carle Place, L.I., New York 11514
St. Regis Corporation
237 Park Avenue
New York, New York 10017
E.I. du Pont de Nemours and
Company, Inc•
1007 Market Street
Wilmington, Delaware 19898
Reid-Provident Laboratories, Inc.
640 Tenth Street, N.W.
Atlanta, Georgia 30308
Hach Company
P.O. Box 389
Loveland, Colorado 80539
xiii
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INTRODUCTION
BACKGROUND
In 1980 the United States Congress enacted PL 96-510, the Comprehensive
Environmental Response, Compensation, and Liability Act of 1980 (CERCLA, the
Act, or Superfund). CERCLA regulates hazardous substances, in order to mini-
mize the chance of uncontrolled releases into the environment and to ensure
speedy responses to such situations. Under Sections 103(a) and 103(b) of
CERCLA, any party responsible for the release of an amount of a CERCLA-
designated hazardous substance greater than or equal to the Reportable Quantity
(RQ) for that substance must notify the National Response Center of the release.
The 617 substances that fall under the purview of CERCLA are specified in
Section 101(14) of the Act. Under Section 102 of CERCLA, the U.S. Environ-
mental Protection Agency (EPA) may also designate other hazardous substances.
The substances designated in Section 101(14) of the Act are comprised of
those specified in Sections 311 and 307(a) of the Clean Water Act (297 and 65
substances, respectively), Section 112 of the Clean Air Act (7 substances), and
all of the hazardous substances identified in Section 3001 of the Resource
Conservation and Recovery Act (RCRA). The substances designated in RCRA are
contained in two lists of specific chemical products, wastes, or intermediates
(the P and U lists; 107 and 233 entries, respectively) and two lists of process-
specific industrial waste streams (the F and K lists; 13 and 67 waste streams,
respectively). CERCLA also specifies that substances designated in Section 7
of the Toxic Substances Control Act (TSCA) are covered, but no compounds are
currently regulated under that legislation. A Comprehensive Hazardous Sub-
stances List (the List) containing the 617 substances specified in Section
101(14) of the Act has been published,-'- and is reproduced at the end of this
volume (see page 49). In addition to these chemical listings, the Act speci-
fies 114 radionuclides of concern under CERCLA. The EPA has a memorandum of
understanding with the Nuclear Regulatory Commission to deal with these,2 and
this report will not address them.
Under Section 102(b) of CERCLA, each substance is initially assigned
either the same Reportable Quantity value as that given it in the Federal Water
Pollution Control Act, or, if none is specified there, a value of one pound.
RQ values assigned in the Federal Water Pollution Control Act range from 0.454
kilograms (1 pound) to 2270 kilograms (5000 pounds). Adjustment of these RQ
values, in order to minimize unnecessary notifications of the National Response
Center and still protect the public health and welfare, is being carried out by
the Office of Emergency and Remedial Response of the U.S. EPA under Section 102
of the Act.
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In order to determine whether release of a Reportable Quantity of a CERCLA
hazardous substance has occurred, methods of chemical analysis for these sub-
stances in environmental samples are needed. For that reason, as well as to
aid in the assessment of the feasibility of possible changes in RQ-values, a
survey of the state of the art of analytical chemistry in the Superfund context
has been undertaken. This report discusses the technical feasibility and cost o
such analyses and presents a compound-by-compound cataloguing of analytical
methods for three sample matrices: air, water, and soil/sediment.
In order to characterize a release of a hazardous substance properly, both
quantitative and qualitative information is required. Field methods are neces-
sary to rapidly characterize the site and to gauge the extent and location of
contamination of air, soil, and water there. Such information can then be used
to design a suitable sampling plan for the implementation of laboratory analyses.
These analyses should yield information that is legally defensible about the
amount of the hazardous substance(s) present in samples and should clearly and
unequivocally identify it as a substance on the List.
The difficulties associated with satisfying these requirements for measure-
ments made in support of the Act are compounded by the broad scenario encom-
passed by releases of CERCLA-hazardous substances. Under Superfund, such a
release can be either episodic or continuous, and the analytical techniques
necessary for such circumstances can range from those appropriate for very high
concentrations to those suitable for ultra-trace levels. The hazardous sub-
stances involved can be solids, liquids, gases, or mixtures of more than one
phase, and can be either nearly pure substances, which may be well characterized
and labeled, or can be mixtures of unknown composition. The variability in the
degree of knowledge of both the identity of the hazardous substances involved
and the physical state of them is made even more vexing by the variability of
the potential matrix into which they may be released. Soils and sediments can
have extremely different characteristics that vary greatly from one area of the
United States to another. Salt waters, brackish waters, and highly anaerobic
waters may well have different characteristics that can hamper analysis to
varying degrees. Different levels of particulates and humidity in air across
the nation can affect the efficiency of air sampling. In addition, interactions
with the sample matrix or other components of mixtures containing CERCLA-
hazardous substances can further complicate the situation. The broad scope of
potential situations encompassed in the scenario of a release of CERCLA hazardous
substances highlights the weaknesses and limitations of modern analytical
technology.
Due to these reasons, the three general classifications of sample matrices
(air, soil/sediment, and water) used in this report belie the complexities
associated with them. Consideration of the general effects associated with
each broad class of sample matrix is made in the individual Method Descriptions-
However, individual interferences that may be present in the specific matrix of
a particular sample cannot be considered, as such factors are release-specific.
For example, sediment samples frequently contain sulfur and sulfides due to
anaerobic conditions. This type of general interference may be considered in
the discussion of an analytical method if it is specifically mentioned in the
source of the method. However, particular organic compounds that may be present
in one specific soil sample are not taken into account.
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SCOPE
Since the Comprehensive Hazardous Substances List specified in Section
101(14) of the Act is a composite of other regulatory lists, substances are
frequently listed by more than one regulatory synonym. In addition, several
entries on the List are for broad classes of compounds, like "Arsenic and
Compounds" and "Phthalate Esters". The F and K Waste Streams of RCRA present
a situation even more vaguely defined because particular substances are not
listed, but the origins of mixtures are specified- In addition, some sub-
stances are regulated under RCRA (and, therefore, CERCLA) due to their charac-
teristics of ignitability, corrosivity, reactivity, or extraction procedure
(EP) toxicity, but are not specified as particular compounds.
This report addresses only the specific compounds designated on the List.
For these, searches were performed to obtain applicable analytical methods for
air, water, and soil/sediment samples at two levels of sophistication: field
methods and laboratory methods. Consideration of substances that fall under
the purview of RCRA, and consequently CERCLA, due to the characteristics of
ignitability, corrosivity, reactivity, or EP toxicity is beyond the scope of
this study. This report is not intended to be a critical review and lists only
information found. It does not attempt to assume applicability of a technique
reported for determination of one compound to the determination of another or
for a compound in a sample matrix other than the one for which the method was
developed, with or without modification. An effort to provide guidance to the
potential components of the F and K Waste Streams, within the framework of the
List, is presented in Appendix C. The U.S. EPA Office of Solid Waste is
currently studying the composition of many of these process-specific waste
streams.
Releases of hazardous substances of concern under CERCLA can vary in
nature. Both episodic and certain continuous releases are of concern. These
two classes can both be divided into well-characterized releases, where the
hazardous substances present in the release are known, and poorly characterized
releases, where the identities of the substances in the releases are not known.
CERCLA requires that specific identification of a compound from the List be
made, and the instance of a well-characterized release fits these requirements
well. However, poorly characterized releases can present problems with verifi-
cation of the presence of a CERCLA-designated hazardous substance. Because of
problems associated with total analysis of samples to identify and measure all
substances present, this report is for the most part aimed at methods for use
in the context of well-characterized releases. This is not to say that methods
that are suitable for poorly characterized releases are not included; in fact,
analytical methods applicable to more than one CERCLA-designated hazardous
substance have been put into a separate appendix, Appendix B, to emphasize
their potential as screening methods. However, total analysis and characteri-
zation of a sample is a long and complex process, which must be designed based
on particular sample characteristics, and this document does not provide any
guidance for such efforts.
This report divides the compounds of interest under the Act into two groups
- inorganic and organic compounds - due to the similarity of analytical methods
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used within each group. In some instances, however, classification of a
compound as a member of one group or the other is difficult. For example, this
problem arises with organometallic compounds (e.g., tetraethyl lead) and some
salts (e.g., ammonium picrate). The system used for such classifications in
this report has an impact on the organization of the presentation of informa-
tion and is described later in this report (See "Structure").
The analytical methods located for each compound/matrix combination are
classified as one of two types - field methods, for rapid semi-quantitative
measurement, and laboratory methods, for more precise and accurate determi-
nations. The distinction between a field method and a laboratory method is
nebulous, and could be based on either the quality of the results or on the
equipment requirements for the analysis. This report arbitrarily defines field
methods as those using portable equipment that does not require line voltage.
The use of line voltage from nearby power lines or a gasoline-powered generator
for power-intensive equipment such as a gas chromatograph/mass spectrometer
(GC/MS) or an inductively coupled atomic plasma spectrometer (ICP) is a situ-
ation not considered to be part of a field method in this report. This deci-
sion is not a judgment that mobile laboratory responses are ineffective or
inappropriate; many examples of rapid response by the U.S. EPA Municipal Environ-
mental Research Laboratory in Edison, New Jersey (MERL-Edison) demonstrate the
usefulness of such an approach to on-site analysis.2»3 However, in order to
clearly delineate the distinction between field and laboratory methods and to
highlight analytical methods that are an alternative to technology-intensive
laboratory methods, we have chosen the above definition of a field method.
At the time this study was initiated, it was believed that the use of
mobile laboratories was a minor consideration with regard to CERCLA analyses.
Mobile laboratory analytical capabilities had been described elsewhere .2>3
However, during the two years of compiling this report, the use of mobile
laboratories has increased. Therefore, a supplementary survey of the subject
was prepared, and a portion of the information from the survey is included in
the Results section of this report.^
The search for applicable analytical methods began with known sources of
CERCLA, other EPA, and standard analytical methods, and continued through
computerized searches of the literature. By the time computer-searching was
ended, it became apparent that many of the methods located were in the early
stages of development. A description of the method-search strategy used is
presented later in this report.
The effort to determine the costs of cited analytical procedures relied on
two sources of information. For standard environmental analyses, cost figures
could be obtained from price lists and bid figures. However, for analytical
procedures that are more infrequently encountered, cost figures were not so
readily obtained and commercial analytical facilities were directly contacted
to obtain a cost estimate. A description of the cost search is presented later
in this report.
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PURPOSE
The primary goal of this report is to inform the U.S. EPA-OERR of the
status of analytical chemistry in the context of releases of Superfund-hazardous
substances, in support of rulemaking efforts in the Regulations Branch of that
office. In order to satisfy OERR's needs, specific information about analytical
methods for each CERCLA-hazardous substance is presented in the Appendices of
this report. Less-detailed gross statistical information about the results of
our study is given in the main body of the report.
In planning the content and structure of the Appendices, attention was paid
to the needs of both OERR and, secondarily, other potential users of the
information presented. The Appendices comprise an annotated bibliography of
potential analytical methods for Superfund-hazardous substances. As such, they
could be useful to EPA managers as a decision-making resource, to EPA scientists
and technicians as a source of analytical methods, and to the regulated community
as a transfer of current technology.
The depth and scope of the Method Descriptions are intended to satisfy the
needs of the EPA OERR. Again, an attempt to make the document useful to others
was made, within the constraints of time and budgetary limitations. This
document reports the results of a search for analytical methods and does not
purport to be a critical review or to make any technical judgment about the
analytical methods described or their applicability. In many cases, analytical
methods are described that do not specifically identify the particular compound
in the specified matrix, but measure hydrolysis or dissociation products.
Examples are metallic sodium, sodium methylate, aluminum phosphide, and the
phosphorus halides for inorganics, and certain acid halides for organics.
Obviously these substances do not exist in an aqueous matrix, and only their
hydrolysis products can be expected to be found.
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CONTENTS AND USE OF THIS REPORT
CONTENTS
This report is composed of a main body, three Appendices, and an Index.
The main body of the report summarizes the contents of the Appendices, gives an
overview of the state of the art for analyses for hazardous substances under
CERCLA, and highlights problems with the List and analytical chemical technol-
ogy- The Appendices list analytical methods for substances on the Comprehen-
sive Hazardous Substances List and for the RCRA F and K Waste Streams. Appen-
dix A and Appendix B are primarily an annotated bibliography of analytical
methods, furnishing a reference, a brief description of the reference contents,
and cost information for each method. Appendix B describes methods applicable
to more than one CERCLA hazardous substance, while Appendix A is a substance-
by-substance listing of single-substance methods, or cross-references to
Appendix B for each of the six matrix/level-of-sophistication combinations of
concern. Appendix A also provides limited safety information and states the
current reportable quantity (RQ) for each substance. Appendix C refers the
user to parts of Appendix A and Appendix B which could be useful for specific
RCRA F and K Waste Streams; these references are not meant to be exhaustive,
but comprise the results of a limited investigation of the industrial processes
involved. The Index, beginning on page 48 of this volume, gives the consensual
name, or the name used in this report, for each regulatory synonym for sub-
stances on the Comprehensive Hazardous Substances List.
Since the Comprehensive Hazardous Substances List is a compilation of
several individual regulatory lists of chemical species, no single system of
nomenclature is consistently used, and there are many compounds for which more
than one entry is given. The Index of this report lists each regulatory
synonym for the chemical species of interest and specifies the name chosen for
use in the Appendices. No single system of nomenclature has been used in the
choice of these consensual names, but an attempt has been made to use the
regulatory synonym that is the most common and widely accepted. In that way,
the use of inverted structures is eschewed (e.g., prefer "1,1,2,2-tetrachloro-
ethane" over "ethane, 1,1,2,2-tetrachloro-") and an attempt is made to avoid
use of trivial names unless they are very common. In the case of many pesti-
cides, the formal name is extremely long and convoluted and the trivial or
trade name is the consensual name. For example, the name "Aldrin" is chosen
over "1,2,3,4,10,10-Hexachloro-4,4a,5,8,8a-hexahydro-l,4:5,6-endo,exo-dimethano-
naphthalene". The U.S. EPA Office of Emergency and Remedial Response requested
public comment on the type of nomenclature and the number of synonyms to be
used in the publication of the List.l
-------
As mentioned above, the Index to this report lists all of the regulatory
synonyms for entries on the Comprehensive Hazardous Substances List, and provides
the name used for each throughout the Report and Appendices. The entries in the
Index and those in Appendix A are in alphabetical order. The prefixes n-,
iso~, tert-, sec-, cis-, trans-, o~, m~, £-, N-, 0- and numerals are not
considered in alphabetizing, but bis-, di-, hexa-, mono-, penta-, poly-,
tetra-, and tri- are used.
In order to use a consistent set of rules in the division into organic and
inorganic classifications, several decisions were made. The use of the result-
ing rigid set of rules is intended to help users know in which part of Appendix
A to look for a compound of interest. The rules have been chosen as an edito-
rial choice and not as a scientific judgment. We list all metal-containing
compounds as inorganic substances, all non-metal salts of organic acids as
organic substances, and alkylated non-metallic inorganics as organic compounds.
All carbonates and bicarbonates are considered to be inorganic substances.
Under these rules dodecylbenzenesulfonic acid, ammonium benzoate, and methyl
hydrazine are considered organic compounds, while calcium dodecylbenzene-
sulfonate, ammonia, and hydrazine are inorganic. While arguments could be
raised over specific assignments of substances as organic or inorganic, these
rules for classification were chosen solely for the purpose of systematically
organizing the entries in the Appendices.
Reportable Quantity Values and Safety Information
As mentioned above, Appendix A is a substance-by-substance listing of
CERCLA-hazardous substances which provides cross-references to Appendix B for
multicompound methods, or a Method Description for single-compound methods.
The first entry in each listing in Appendix A is the Reportable Quantity (RQ)
value of the CERCLA-hazardous substance, as specified in the Federal Register.1
As discussed in the Background section of this document, each substance is
assigned the same RQ value as in the Clean Water Act or, if none is specified
for it there, a value of 0.454 kilograms (1 pound). Modifications of some of
the resulting RQ values have been made, based on environmental and/or health
factors. It is probable that further changes will be made in these values,
particularly for those substances that are listed (in the Safety Information
section) as potentially carcinogenic, potentially chronically toxic, or both.
This is because, after the carcinogenicity and/or chronic toxicity of the sub-
stance is evaluated, a decision will be made as to a suitable RQ value. Until
then, the statutory value of 0.454 kilograms (1 pound) applies.
Immediately following the RQ value for the CERCLA substance is a section
that furnishes limited safety information. Factors about the substance that may
be pertinent to field or laboratory personnel safety are listed here, such as
if the substance has been shown to exhibit mammalian toxicity at or below
certain levels. These levels are: an oral LD5Q (dose lethal to 50 percent of
the test population) of 10 milligrams per kilogram, a dermal LD5Q of 4 milligrams
per kilogram, or an inhalation LC5Q (concentration lethal to 50 percent of the test
population) of 40 parts per million. Where possible the route of entry for the
substance has been specified. In addition, chronic toxicity was indicated for
any substance which received a chronic toxicity score of 40 or higher in evalua-
tions by the EPA Environmental Criteria and Assessment Office. Substances that
-------
have been identified by EPA as having an appreciable chronic or subacute toxic
effect, but that have not been evaluated, are listed as being potentially
chronically toxic; those that have been identified as carcinogens, but have not
yet been evaluated, are denoted as potentially carcinogenic. Specific hazards
associated with a given substance are also mentioned, including reactivity,
toxic products of reaction with water, chemical compatibilities, and flash
points below 100°F. The major source of this information is a technical back-
ground document to support rulemaking pursuant to CERCLA 102(b), prepared by
the U.S. EPA, OERR.
Readers may note that a particularly low RQ value is listed for a certain
substance, but that no specific safety information is furnished. This situa-
tion can arise because the factors used to decide RQ values were not restricted
to human (or mammalian) safety, but also included aquatic toxicity and other
factors that would not appear in safety information. Additionally, the sources
of information used for the compilation of these safety data are not comprehen-
sive and the safety information is not purported to be exhaustive. Therefore,
for those substances the toxicity or hazards of which are known to be severe,
but for which little or no safety information is otherwise provided, the Safety
Section contains a caution to obtain such data from other sources. The follow-
ing are suggested:
Sittig, M. Handbook of Toxic and Hazardous Chemicals; Noyes Publications:
Park Ridge, New Jersey, 1981.
Hazardous Chemicals Data Book, Environmental Health Review No. 4, G. Weiss,
Ed.; Noyes Data Corporation: Park Ridge, New Jersey, 1980.
Sax, N. I. Dangerous Properties of Industrial Materials, 5th ed.; Van Nostrand
Reinhold: New York, 1979.
The Condensed Chemical Dictionary, 10th ed.; G. G. Hawley, Ed.; Van Nostrand
Reinhold: New York, 1981.
Following the Safety Information section of the Appendix A entry, Method
Descriptions or cross-references to Appendix B for six matrix/level-of-
sophistication combinations are covered.
Method Descriptions
In addition to RQ values and safety information, the compound listings in
Appendix A contain descriptions of analytical methods for the CERCLA-hazardous
substances. Therefore, Appendix A lends itself readily to compound-specific
location of analytical methods. Some methods in Appendix A may be applicable
to more than one compound, but are useful for the determination of only one
compound specified on the List.
Appendix B is used to find methods applicable to more than one compound
on the List. Such analytical methods have more versatility and greater poten-
tial for screening of poorly characterized releases. Each Method Description
in Appendix B states the compounds from the List to which the method has been
demonstrated to be applicable. Some entries on the List are broad, generic
8
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classes of compounds, as "Phthalate Esters" and "Arsenic and Compounds".
Currently, no RQ values are being set for such listings. Accordingly, such
classifications are not considered in the assessment of capabilities for
analysis for CERCLA substances.
The Method Descriptions presented in Appendices A and B contain varying
amounts of information in one of two formats. Methods that were classified as
Laboratory Methods contain six sections: Method Summary, Interferences,
Quality Control, EPA/Technical Status, Reference, and Cost. Field Methods have
the same six sections as Laboratory Methods, except that the EPA/Technical
Status is replaced by a Sensitivity section.
The Method Summary section of each entry presents the general analytical
technique used to inform readers of the equipment and personnel requirements.
The section also gives salient method details, such as detector type for gas
chromatographic methods and use of internal standards.
The Interferences section lists interferences that are specifically
mentioned in the source of the method. Only what is present in the reference
is noted in this section.
The Quality Control section gives quality control procedures dictated in
the reference and frequently reports that "no procedures are given". This is
because a fixed quality control protocol is very case-specific: the level of
duplicate, replicate, and fortified samples can vary greatly, depending on the
amount of confidence in the analytical results desired, the sample matrix, and
other factors. For purposes of this report we follow the standard definition
of quality control - those actions followed to ensure a specified quality of
the product.5»6 Therefore, steps given to demonstrate method precision and
accuracy are listed in the Quality Control section. A rigid quality control
protocol is not actually a part of an analytical method, but part of an overall
quality assurance scheme that also includes a statistically valid sampling plan
and valid end-use of the analytical results.
The EPA/Technical Status portion of the method description tells the
reader whether a method is approved for use under a given EPA regulatory
program and whether or not information on the precision and accuracy of the
technique is given in the references. This information is provided to allow
the reader to see how thoroughly the method has been evaluated. The precision
and accuracy information mentioned is a part of method validation or technical
review and, since it dictates no actions by the analyst, is not considered to
be quality control. Because of variations in the form of such information from
source to source and the high degree of dependence of such data on the char-
acteristics of the particular individual sample matrix, no attempt is made to
specifically list the precision and accuracy information furnished. Also
included in the EPA/Technical Status part is the method detection limit, if
provided. The method detection limit is defined as the concentration of
analyte in a sample (as opposed to a standard or blank) that yields a detector
signal equal to twice the standard deviation of the background noise in the
signal of a sample with a concentration close to but above zero. The method
detection limit must use information from a large number and wide variety of
samples analyzed in many laboratories in order to be valid. The method
-------
detection limit tells the performance of the method with average samples in the
presence of normal interferences associated with them. The method detection
limit may not be given in the reference(s) being described, but other types of
data may be provided. The instrumental detection limit uses a rea'gent blank in
place of the sample(s) used in measurement of the method detection limit. In
this way, the instrumental detection limit gives a value for the ability of the
instrument and procedure to detect an analyte in the absence of sample-matrix
interferences. A third term, sensitivity, is used to indicate the concentra-
tion or amount of analyte that elicits a 1-percent (0.044 absorbance units)
detector response. This value is a measure of instrument sensitivity only and
does not take into account either sample treatment (e.g., extraction, diges-
tion) efficiencies, or sample-matrix interferences. When a limit of detection
is provided in the reference, and is defined differently than the above terms,
that definition is specified. If a term is not defined in the reference, it is
used undefined in the Method Description.
For field methods a Sensitivity section replaces the EPA/Technical Status
section because of the lack of official EPA approval of field methods, and the
importance of knowing the sensitivity of such methods. Strict use of analytical
chemical terminology requires that the term "sensitivity" be used only to indi-
cate the amount or concentration of a substance that will elicit a specified
degree of response from an instrument. The use of "sensitivity" for this
section of the Method Description is made because the term is easier to intui-
tively grasp by all of the potential users of this report than the more appro-
priate term "limit of detection".
The References section identifies the documents that were used to write
the Method Description. If a bibliography was used and the primary reference
not obtained, the bibliography is mentioned in the References Section and the
primary reference is cited (parenthetically) in the Method Summary Section.
This was necessary in the case of some foreign-language articles and articles
in not easily accessible journals.
Appendix B entries present a list of compounds to which the particular
method is applicable, along with their CAS Registry Numbers, before the text of
the Method Description. In every instance, care was taken not to add any
compounds to those specifically mentioned in the source(s) of the method,
regardless of how reasonable that addition might seem. Therefore, it may well
be that the lists of compounds preceding many method descriptions could contain
more entries. This imposed limitation is expressed in the Appendix B Method
Descriptions by including the adjective "above" in the phrase "for analysis of
the above compounds". This wording is not meant to rule out the possibility
that other subbstances may respond to the procedure. There are several
Appendix B Method Descriptions that have the same name, but different matrices
and/or lists of candidate compounds. For each, the list of compounds amenable
to determination by the method should be checked carefully to be certain that
the compound of interest is listed there. Several compounds are also included
in more than one list for a given matrix/level-of-sophistication. This results
from one of two circumstances: First, Method Descriptions were prepared for
all Phase I methods located, regardless of how many times a compound is
mentioned. (Phase I methods are from EPA, Federal, or other standard reference
sources. See the Report Preparation section of this text for a full discussion
10
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of method sources.) Second, for Phase II methods, when a multicompound method
was located that was applicable to a compound/matrix/level-of-sophistication
combination for which no method had been located previously, that method was
included. When such a Method Description was compiled, all CERCLA-hazardous
substances to which it had been demonstrated to be applicable were included,
whether another method had been located for them or not. In this way, several
multicompound methods applicable to the determination of a particular compound
in the same sample matrix may be provided, each with a different set of com-
pounds listed to which the method is applicable.
USE OF THIS REPORT
General
This report provides information to the OERR and others at three levels.
The overview of the situation given in the Executive Summary may be sufficient
for some intended uses. A more detailed discussion is offered in the text.
When more detailed and specific information is required than is presented in
the text, the user may consult the Appendices. The Appendices can be used to
investigate analytical techniques for a single compound, or to assess capabil-
ities for multicompound or screening analyses. Figure 1 is a flow chart that
depicts the uses of the Index and Appendices A, B, and C.
Compound-Specific Use
To obtain information on analytical capabilities and costs for a specific
chemical or compound, such as would be needed in a release where the specific
hazardous substances are known, a stepwise procedure should be followed.
First, one should consult the Index, where the name used in the report for
that substance is given.
The Index gives the Chemical Abstracts Service (CAS) Registry Number for
each substance and tells the consensual name used in the appendices. The CAS
Registry Number can be used to ascertain the identity of the compound in ques-
tion. Armed with the consensual name for the hazardous substance of interest,
the user may then locate the listings of analytical methods for that compound
in Appendix A.
The user will find six different classifications listed under each
compound in Appendix A: field methods for three sample matrices - air,
soil/sediment, and water - and laboratory methods for the same three matrices.
Under each of the six classifications or matrix/level-of-sophistication combin-
ations, one of three types of entry will be found: a blank space, indicating
that no method was located; a Method Description, describing analysis for that
compound; or a reference to a multicompound method listed in Appendix B. If
the user is referred to Appendix B, the Table of Contents for Appendix B should
be consulted to locate the page for the applicable Method Description. Since,
in some cases, several Method Descriptions exist with the same title and
different matrices and/or lists of analytes that have been demonstrated to be
amenable to determination by that method, users should be certain to check the
sample matrix and the analyte list above the Method Summary when consulting
Appendix B.
11
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USE OF APPENDICES/INDEX
(USERSN
COMPOUND I
NAME I
INDEX
NO
LISTING
/NOT CERCLA CMPDX
OR NOT A REGULATORS
V^ SYNONYM J
APPENDIX A
"CONSENSUS"
NAME
APPENDIX B
APPENDIX C
Figure 1. Flow chart depicting use of the Appendices,
12
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Multicompound Use
In instances of poorly characterized releases, measurement of the degree
and nature of environmental contamination will require extensive analysis.
Analytical techniques that are suited to detection or measurement of more than
one hazardous substance are attractive in these situations. Appendix B is a
compilation of such analytical methods.
The methods of Appendix B are presented in alphabetical order by the
method name within Section A (Inorganic) and B (Organic) of Parts I (Field) and
II (Laboratory), and are listed in the Appendix B Table of Contents. The name
used for each method attempts to be descriptive of the analytes to which the
method is applicable.
The F and K Waste Streams from RCRA legislation are described in Appendix
C. For each specific waste stream, substances that are potential components
of the waste stream are listed. These listings are not exhaustive, both
because they are limited to CERCLA-hazardous substances and because these waste
streams are of a variable composition with their chemical components not speci-
fied. No particular single analytical technique is specific for these streams.
From Appendix C, users may obtain the consensual names for appropriate analytes
or the name of a particular multicompound method of interest for a given waste
stream.
13
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REPORT PREPARATION
METHOD SEARCH
The location of analytical methods for the substances of interest was
performed in two phases, according to a hierarchy of method sources. A hier-
archical system of sources of analytical methods was devised so as to use first
those sources better demonstrated to be applicable to the CERCLA scenario. In
Phase One of the method search, sources were utilized that were expected to
yield well-developed methods with demonstrated method quality. Table 1 shows
the hierarchy of method sources that comprised the method search. All Phase
One methods located have been incorporated in this report. These include
methods currently in use in the CERCLA program, such as those in Invitation for
Bid documents,'" methods used for the Resource Conservation and Recovery Act
(RCRA),9 the National Pollutant Discharge Elimination System of the Clean Water
Act, >11 and other EPA programs; other Federal methods [e.g., National Insti-
tute for Occupational Safety and Health (NIOSH) methods^]; and consensual
methods [e.g., methods from the American Society for Testing and Materials
(ASTM)13»14 and the American Public Health Association (APHA)15]. (The refer-
enced documents used for Federal Methods are often available from the Super-
intendent of Documents, U.S. Government Printing Office, Washington, D.C.,
20402). If one or more analytical methods for a given substance/matrix/level-
of-sophistication were located during Phase One, the search for that specific
combination was ended. For substance/matrix/level-of-sophistication combina-
tions still lacking an appropriate method, reference was made to Phase Two
sources.
Phase Two of the method search process was composed of searches of sources
of methods that are less well established and less tailored to environmental
analyses. These sources began with specialized text and literature searches
and progressed to contacts with commercial analytical facilities, experts in
the field, and equipment manufacturers.
Due to the nature of the Phase One sources, early searches were performed
in a more reference-specific manner than later ones. By the time Phase Two
began, searches had become compound-specific. The nature of the sources in
each phase of the search influenced greatly the information located. For
methods from current CERCLA contracts, a complete quality control protocol is
furnished, because the methods have reached a production-line status. However,
for methods located in the literature, frequently no interferences are
reported, no quality control protocol or precision and accuracy data are fur-
nished, and even operating conditions are often not completely described. The
degree of acceptance of a given method influences its level of use.. When a
method is more widely used, it becomes better developed and may eventually
become part of a contract, with a rigid analytical and quality control protocol.
14
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TABLE 1. METHOD SOURCES
Type of Method
Phase One Sources
Current CERCLA Methods
EPA Methods
Federal Methods
(U.S. and Canada)
Consensus Methods
Invitation for Bid7'8
Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, SW-8469
Proposed Modifications to SW-846 (10-17-83)
Manual of Analytical Methods for the
Analysis of Pesticides in Human and
Environmental Samples
Methods for Chemical Analysis of Water
and Wastes10
Methods for Organic Chemical Analysis of
Municipal and Industrial Wastewater11
Characterization of Hazardous Waste
Sites - A Methods Manual, Vol. 3, "Avail-
able Laboratory Analytical Methods"
(OSHA) NIOSH Manual of Analytical Methods,
Vol. l-T^2
(OSHA) NIOSH Analytical Methods Standard
Completion Program
(USGS) Methods for Analysis of Organic
Substances in Water
(EML) EML Procedures Manual
(Alberta Environment) Methods Manual for
Chemical Analysis of Atmospheric Pollutants
(Alberta Environment) Methods Manual for
Chemical Analysis of Water and Wastes
(AOAC) AOAC Methods, 13th ed.
(APHA) Standard Methods for the Examination
of Water and Wastewater, 14th ed.
(APHA) Methods of Air Sampling and Analysis,
2nd ed."1"5
(continued)
15
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TABLE 1. (Continued)
Type of Method Phase One Sources
Consensus Methods
(ASTM) Standards on Chromatography13
(ASTM) ASTM Book of Standards, Vols.
11.01, 11.02, 11.03, 11.04, 14.Ol14
Phase Two Representative Sources
Other Methods
Recent Methods
Incipient Methods
(Specialized References) Sampling and
Analysis of Toxic Organics in the
Atmosphere, STP-721, 1982.
Handbook of PAH, Marcel-Dekker, 1983.
(Journals, etc.) Analytical Chemistry
Environmental Science and Technology
Management of Uncontrolled Hazardous
Waste Sites
(Manufacturers, Experts) Draeger
Detector Tube Handbook
Personal Communications.
Therefore, the source of an analytical method influences the information
content of the Method Description provided.
Most of the Phase Two method search was performed hy computer, utilizing
the Dialog® On-line Information Retrieval Services and the CAS ONLINE® data-
bases. The five Dialog® CA Search files, produced by the Chemical Abstracts
Service (CAS) of the American Chemical Society, were used extensively to locate
analytical methods for the Interim Report, the starting point for this docu-
ment. References to compounds on the Comprehensive Hazardous Substances List
(the List) were located in these databases by CAS Registry Number (CAS Number).
Citations were received by mail (in 7 to 14 days), and the texts of the
abstracts (from Chemical Abstracts) were each obtained and evaluated for method
suitability. Articles corresponding to abstracts describing application
methods were acquired from the University of Nevada, Las Vegas (UNLV) Library,
the EPA EMSL-LV Library, or commercial sources. Method Descriptions were
prepared from these articles, except in the rare case of foreign-language or
unavailable articles, where the abstract from Chemical Abstracts was used.
16
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When the computer search was initiated for the Interim Report, a great
amount of information was being sought, and the search strategy reflected that
situation, seeking any matrix/level of sophication combination for 144 sub-
stances, or 24 percent of the List. For the Final Report, the needed methods
become fewer, as did possible references to them, and the amount of irrelevant
material obtained increased. Thus, it was necessary to refine the search
strategy, as the search progressed.
For the Final Report, most of the search was performed on CAS ONLINE®.
The search results were printed online, including abstracts. This procedure
saved substantial time, since the abstracts were available for evaluation as
soon as the computer session was completed. The search was conducted in speci-
fic CA Sections, such as "Organic Analytical Chemistry", "Water," or "Agrochemi-
cal Bioregulators," in order to limit inappropriate output. The restriction of
the search to about 20 of the 80 CA Sections also allowed a reduction of exclu-
sionary terms in the search statement. These terms can exclude desired as well
as undesired information. For example, if a term "not blood" is included in a
search statement for a water method, a method suitable for both blood and water
analyses will not be recognized. The use of CA Sections in searching can also
permit a smaller number of search terms, reducing both the possibility of
interferences and the time of the search. For the first part of the Final
Report method search, all the CAS numbers of substances for which no methods
had been found were entered in the computer and saved. These numbers were
entered in subsets of five, so that changes would not require reentering the
entire list.
A matrix-specific search statement, specifying English-language articles
and the words "air" or "water" or "soil" or "sediment" or "environment," was
also saved. Combination of the saved CAS Registry numbers and this search
statement was made to locate references and to update search results. A
search statement to locate methods without a specified sample matrix was also
saved, so that such methods could be located for substances with no method
identified for any specific matrix. After this search was completed and
results evaluated, another one was initiated to locate methods for substances
for which analytical information had been located for some, but not all,
matrices. Separate lists were prepared for organic and inorganic substances
that were without a method in a particular matrix (air, soil, or water), for a
total of six lists. These lists were entered in the computer and saved, along
with a search statement tailored for each set of substances. Each search was
conducted in the applicable CA Sections. An example of a search is the follow-
ing: Organic substances requiring an analytical method for soil were saved in
the computer as OSOIL/Q. This list was recalled and combined with the search
statement English/LA and (soil? or sediment?) and (anal? or detn or determin?
or trace or residu?). The question marks in the statement allow variations in
the ends of the terms, such as analysis or analytical, soil or soils. Some of
the terms were changed, omitted, or added for searching particular CA Sections.
An additional search was planned that used Dialog® databases other than
the CA Search files to locate methods still needed. Accordingly, after the CAS
ONLINE® search, the Dialindex™ file, a low-cost index to all of Dialog's®
databases, was used to search for methods not found in the CA File. The names
of five compounds were entered into the computer along with the numbers of the
17
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eleven files to be scanned, and the computer provided the number of citations
for each compound in each of the files. The individual files were then
accessed and searched using the compound name and sample matrices of interest.
It was found that the productivity of this type of searching was quite low.
Because CAS Registry Numbers could not be used in most of these files, only the
consensual name was searched, so a valid reference to a nonregulatory synonym
would be lost. Also the commands had to be reentered for every file. The
search was stopped after the first five substances due to the meager results
obtained and the large amount of time expended.
As before, relevant journal articles were obtained from the library of the
University of Nevada, Las Vegas (UNLV) and the library of the U.S. EPA Environ-
mental Monitoring Sytems Laboratory (EMSL), Las Vegas. The CAS abstract
numbers were used to order copies of hard-to-find articles from the CAS Docu-
ment Delivery Service.
COST SEARCH
Costs of analyses performed internally vary widely from firm to firm and
the figures are not readily available; therefore, the cost information about
analytical methods in this report is based on list prices from commercial
analytical firms. The price provided for each method is for one sample. An
assumption is made that the sample is one of six submitted at the same time,
both to minimize the large influence the number of samples has on the cost per
analysis, and to partially reflect the fact that multiple samples are to be
expected from a release site. A bid price is given as well, when available: it
represents a fixed cost for an analysis following a rigid protocol, for a large
quantity of samples. A bid price indicates the lowest probable cost for
analysis by a particular method, but it also reflects the capacity and pro-
jected workload of the laboratory when the bid is made. It should be noted
that most commercial laboratories offer discounts of 50 percent or more on many
analyses for large numbers of samples.
Costs for common analyses were obtained from commercial price lists.^
Further information or clarification was provided by specialists in various
fields through personal communications (Mr. John Rhodes, Columbia Scientific
Industries, Austin, Texas, June 23, 1983 and July 19, 1984; X-ray analysis.
Mr. W. Gary Wilson, Environmental Research and Technology, Inc., Concord,
Massachusetts, July 6, 1983; air sampling. Dr- Anthony Wong, California Ana-
lytical Laboratories, Inc., Sacramento, California, June 22, 1983; dioxin
analysis). For methods about which no cost information had been found, a
modular pricing structure was developed. A cost was obtained for each step
involved in a particular sample preparation and analysis, and the costs were
totaled to obtain an overall figure. Most of the modular prices were supplied
by Mr- 0. John Logsdon, Rocky Mountain Analytical Laboratory, Arvada, Colorado,
and Mr. Jack Custer and Mr- Dan Grove, Alert Laboratories, Canton, Ohio; some
were found in price brochures. Sources for bid prices were primarily govern-
ment literature and the Environmental Protection Agency Superfund Sample
Management Office (Ms. Linda Haas, EPA Sample Management Office, Viar and Co.,
personal communication, June 24, 1983, October 25, 1983, and August 8, 1984).
18
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Errors can occur in developing a cost estimate from modules for two
reasons. The Method Summary might omit or simplify the description of a proce-
dure, so the cost for the complete procedure may not be represented. Also, the
cost of an analysis may not be given in a price list because it is inherently
difficult to define - perhaps due to a large number of variables - and these
difficulties exist with modular pricing as well.
In a few instances, the cost information for a method description is
followed by the notation (est.). For these methods, cost data were incomplete
but an estimate was attempted from what was available. When it was not possi-
ble to update cost information from the 1983 Interim Report, the notation
(1983) follows the cost figure. All the cost information in this section has
been documented; however, many of the sources do not wish for their firms to be
identified with a specific price quotation. It must be emphasized that the
cost information presented in this report should not in any way be considered
to constitute a price list.
Factors Influencing Cost Figures
Quantity Considerations—
It has already been noted that increasing the number of samples submitted
at one time reduces the cost per sample, within limits. The number of compo-
nents analyzed per sample, as well as the number of related analyses performed
at one time, can also affect the cost.
Gas chromatography (GC), gas chromatography/mass spectrometry (GC/MS),
X-ray fluorescence spectrometry, and inductively coupled plasma spectrometry
(ICP), among other techniques, can provide information simultaneously about
several components in a sample. It is common for laboratories to charge a base
price for such analyses, plus an additional charge for each component over a
certain number. Therefore, in this report, GC and GC/MS cost information is
valid for five or fewer components per sample, and X-ray fluorescence spectrom-
etry for ten components. Pricing structures for analysis by ICP were found
both with and without a base price; the system without one is used here because
it indicates more clearly the cost for determination of just the component in
question.
Another cost consideration is that a laboratory may discount a group of
analyses. For example, if the acid extractable and base/neutral extractable
fractions of a sample are both analyzed at once, it may cost less than if each
fraction were analyzed individually.
Sampling Considerations—
The cost information provided with the method descriptions in this report
does not include sampling costs. The hourly fee of $40.00 to $70.00 charged by
commercial laboratories for field work applies to sampling.
Water and Soil/Sediment Samples—The cost of the actual collection of
water or soil/sediment samples is normally small because it does not require
much time. Samples for laboratory analysis need appropriate containers for
collection and shipment. Sample container kits for RCRA analyses can be pur-
chased from the laboratory that will perform the analysis, or the cost may be
19
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included in the cost of the analysis. The charge for a kit containing two
bottles and a cooler, shipped via UPS to the sampling site, is $35.00 to $60.00
(list). Small augers and dredges for soil/sediment collection may be included
in the cost of the field work; larger ones can be rented.
Air Samples—For air samples, the sampling situation changes. It may take
several hours to collect the sample. Also, air sampling is actually part of
the sample preparation since the analyte is removed from the sample matrix by
filtration, dissolution, adsorption, or absorption as the sample is collected.
The costs of air sampling are mostly due to the hourly charges for labor in the
field. The fee does not include travel or related expenses, which would differ
with each combination of laboratory and field site.
The time required for collecting an air sample depends on the concentra-
tion of the analyte and the analytical method to be used. If a four-hour
collection time is assumed, the cost for labor alone is $160.00 to $280.00. As
stated earlier, costs are based on six samples. If all six samples can be
taken during four hours, the labor cost per sample for collection time is then
$27.00 to $47.00.
Another consideration in air sampling costs is the cost of supplies. The
cost of chemicals is usually negligible. Use of equipment such as impingers
(bubblers) and pumps are generally included in labor charges. The cost of
consumable supplies may be added to the sampling cost. These supplies include
Tenax® cartridges, about $10.00 each, and charcoal tubes, about $1.00 each.
Quality Considerations—
Properties of the sample can affect the cost of analysis by influencing
the necessary sample preparation steps. These properties include the sample
matrix (air, water, or soil), complexity of the matrix, sample toxicity, and
analyte concentration.
The sample matrix greatly influences the sample preparation required.
Filters containing particulates from air samples usually undergo dissolution,
acid digestion, or ashing. The cost for these procedures may already be
included in the cost of the analysis. An X-ray fluorescence determination of
metals can be performed directly on the filter with no sample preparation
required. When analytes must be desorbed from the sample cartridges; the
charge is about $10.00. Solutions containing gaseous or soluble analytes from
air samples are often already in a suitable form for the analytical procedure.
Water samples may be ready for analysis as supplied, or may require filtration
or a simple extraction. Soil/sediment samples usually need longer extractions
or additional preparatory steps. Costs for soil/sediment samples are typically
10-25 percent higher than those for water samples.
The complexity of the sample, referring to the number of potential inter-
ferences it contains, also affects sample preparation. The removal of these
interferences, or special procedures to avoid them, can add up to 100 percent
to the basic cost of the analysis.
20
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Samples containing highly hazardous materials frequently require special
handling and use of special equipment or a containment facility, and may in-
crease the cost of analysis by up to 100 percent.
The analysis of substances at concentrations near the limits of detection
may call for additional or more sophisticated sample preparation or instrumen-
tation, thus adding to the cost of analysis. For instance, graphite furnace
atomic absorption (AA) spectrometry might be used rather than flame AA to
analyze a metal concentration. The cost would then increase from approximately
$10.00 to $20.00 to approximately $18.00 to $50.00. Analysis by high resolu-
tion mass spectrometry costs about 50 percent more than by low resolution mass
spectrometry, mainly because of higher labor costs.
Considerations Relating to Field Analysis—
By far the largest portion of field costs are due to the hourly charge for
labor, typically $40.00 to $70.00 per hour. Travel and other expenses are
additional charges. Colorimetric and other wet chemical analyses take varying
amounts of time, depending on the method used. The analysis may call for a
period when active work is not performed; for example, time may be required to
allow a reaction to occur. If this period is over twenty minutes, it is as-
sumed that analysis is being performed on another sample. With this exception,
it is assumed that only one sample at a time can be analyzed in the field. The
cost information for wet chemical methods for field use includes a higher
degree of estimation than the information provided for other methods. Time
estimates for some field methods are based in part on those provided in Waste-
water Analysis Handbook, Hach Company, Loveland, CO, April 1978.
An additional cost in field analyses is that of equipment. Some equip-
ment may be supplied by the laboratory; instruments may have to be rented or
purchased. The cost information for instrumental field methods includes rental
charges, prorated to the time estimated for sample preparation and analysis.
The use of rental fees for costs of instrumentation, rather than purchase
prices was made because rental costs can be correlated to an individual
analysis more readily.
Cost figures for non-routine analyses have been developed by use of a
modular pricing system. The costs of the specific sampling (as applicable),
sample preparation, and sample analysis steps were added to arrive at an esti-
mated total analytical price. Table 2 gives some examples of the figures used
and obtained by such a procedure. For example, laboratory analysis of air
samples by HPLC/UV for polycyclic aromatic hydrocarbons requires Soxhlet extrac-
tion, solvent exchange and instrumental analysis by HPLC/UV, at costs of $20-45,
$10-15, and $100 respectively. The total cost, $130.00-$160.00, is the sum of
these figures .
Considerations Relating to Laboratory Analysis—
The costs of laboratory analyses are particularly sensitive to two factors:
turnaround time and the level of quality control required. A rush request may
incur a surcharge on the cost of the analysis of 50 percent. Alternatively, an
hourly surcharge may be made; $75.00 per hour is typical.
21
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TABLE 2. EXAMPLES OF COSTS FOR FREQUENTLY MENTIONED METHODS
Costs of Sampling
(assume 4 hours for air sampling, except for detector tube methods)
Sample Matrix
Air
(Charcoal)
Soil
Water
Time Instrument
$27.00 - 47.00
n*
n
Supplies
$1.00
n($18-30)**
n($18-30)**
Total
$28.00 - 48.00
n($18-30)**
n($18-30)**
Costs of Laboratory Analyses
Method
ICP
GC/FID
HPLC/UV
Matrix
soil/sediment
water
air
e-g<
air
e-g-
bromoform
Preparation
$10.00
$10.00 (desorption)
Analysis
$10.00
$10.00
$60.00-
80.00
polycyclic $20.00-45.00
aromatic (Soxhlet extraction)
hydrocarbons $10.00-15.00 $100.00
(solvent exchange)
Total
$20.00
$10.00
$70.00-
90.00
$130.00-
160.00
Costs of Field Analyses
Method
Detector
Tube
Matrix
Time
Instrument
Supplies
Total
air $10.00-18.00
Test Stick water $3.00-5.00
$2.00-3.00 $12.00-21.00
n $3.00-5.00
* n = negligible
** If the cost of sampling containers is not included in the analytical cost
charged by the laboratory, the cost given in parentheses applies.
22
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Quality control is included to some degree in most commercial analyses,
and is generally a requirement in government contracts. To determine quality
control costs, it is necessary to determine what quality control procedures are
included in the cost of the analysis. If more standard, duplicate, or forti-
fied samples are desired, they will be analyzed as additional samples, with
commensurate charges. Texts are available that describe sampling plans to
ensure a constant level of risk to either the producer or consumer and thus
maintain a consistent level of quality in the product (analysis). However,
most quality control dictated in the methods located does not use such an
approach."
23
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RESULTS
BACKGROUND
General
The evaluation of a release of a hazardous substance will include both
determination of the occurrence of a release and characterization of the
release. Characterization of the release is the concern in this report and
can involve both identification of the hazardous substance involved and measure-
ment of the magnitude and distribution of the release. Identification of the
hazardous substances released is very release-specific, and is largely deter-
mined by the sample matrix characteristics, the particular substances released,
and the degree of knowledge of the nature of the released materials. Timely
and specific identification of hazardous substances of unknown origin in a
complex mixture released into a difficult matrix can be beyond the capabilities
of modern analytical technology. This is due to limitations in time, database,
and technology. In addition, in the instance of a compound that reacts with or
dissociates in water, only analysis for the products of the process is possible,
and such an analysis can never specifically identify the compound from which
the analyte(s) came. Such element-specific analyses give the best information
that can be obtained, but are not specific methods for individual compounds.
If it is known that a strong, exothermic reaction will occur when the substance
of interest contacts water, and that only decomposition products will be
present in the water sample, the phrase "reacts with water" is placed under the
Appendix A water sample headings. The Appendix B methods that apply to such
compounds are, accordingly, only used to determine reaction products; to avoid
any presumption that analysis is for a substance never actually present in its
original chemical state, the Method Description describes the analysis as for
ions, not for compounds. The substances in question may react with moisutre in
water or soil as well.
Measurement of the distribution of contamination from a release involves
collection and analysis of air, water, and soil/sediment samples in the
vicinity of the release. Sample collection requires physical collection of a
representative sample, while sample analysis involves two phases: sample
preparation and analyte determination. The sample preparation process involves
removal of potential interferences and transfer of the analyte into a state
amenable to the chosen method of analysis, and the determinative process then
involves the ultimate analysis of a suitably prepared sample. A weakness in
any of these three steps will result in a faulty measurement. Sample collec-
tion methods and their sophistication frequently depend upon the matrix being
sampled - air, soil, or water - and, to a lesser extent, upon the compounds of
interest. Sample preparation procedures, such as digestion, extraction, or
hot-water leaching, depend upon both the sample matrix and the determinative
24
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method(s) to be used, while the choice of a determinative method is largely
dictated by the analyte, and is frequently the same for all three sample
matrices. For many air analyses, the sample collection step and part of the
sample preparation process are combined in that the analyte is removed from the
air sample matrix into a solution or onto a stationary sorbent. Because of the
dependence of each section of the overall measurement process on these differ-
ent factors, consideration is made of the factors involved in sampling each
type of sample matrix, in sample preparation, and in determination of the
compounds of interest before specific discussion begins.
Sampling
Sampling of air differs substantially from sampling of water or soil-
With air sampling devices, substances in two physical states can be collected -
particulates and gases. Collection of particulates involves mechanically
trapping particles on a filter medium with pores smaller than the size of the
particles. This procedure is straightforward and does not involve rapid diffu-
sion, chemisorption, or other physical/ chemical processes. When gases are to
be collected from air, the compound of interest must have a significant vapor
pressure to be collected at any appreciable distance from the source of the
vapors. Non-volatile hazardous substances, such as inorganic salts, metals,
and organic compounds like dioxin, have negligible vapor pressures. Such com-
pounds exist as particulate substances in air only if very finely divided.
Low-volatility substances would slowly bleed into the atmosphere and the sampl-
ing system. In such a steady-state situation, collection of a cumulative
sample is ideal. Cumulative sampling utilizes the accumulation of an analyte
on some stationary phase, and is usually used in air sampling, due to the large
sample volumes which must be processed in order to obtain a reasonable amount
of analyte. For substances of high vapor pressure, such as hydrogen fluoride,
a release would have to be slow and steady to create a situation amenable to
composite sampling. If a rapid discharge of such a substance occurred, any
composite sample taken would only be a dilution of an instantaneous sample.
Due to the open nature of the atmospheric system, rapid releases of highly
volatile compounds could be dissipated before sampling begins. The well-mixed,
open-system characteristics of the atmosphere create special problems in samp-
ling. The variability in chemical properties and vapor pressures of the
approximately 617 hazardous substances under the purview of CERCLA requires
several techniques for sampling from air.
Many organic compounds and a few inorganic substances have sufficiently
high vapor pressures to be sampled as vapors. Such sampling usually involves
passage of air past a stationary solid phase, or through a liquid. The analyte
is thus either adsorbed on the solid or chemically fixed by the liquid.
Removal of the analyte from the solid or liquid can then be carried out by
standard techniques for analysis of solid or liquid samples.
Water bodies can be considered to be closed systems in the short term, and
are frequently not well mixed. When a water body is not well mixed, sampling
is not straightforward, particularly in the instance of insoluble or immiscible
substances. The difficulty associated with sampling in such an instance is due
to problems associated with obtaining a representative sample that truly
reflects the condition of the water body. Due to the vastly smaller volumes of
25
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water that are collected in comparison to air samples, sample collection times
are greatly decreased. Since the system is essentially closed, the only com-
pounds that will not be collected when in contact with a body of water will be
those that are insoluble, forming a separate phase or layer, and those that
degrade in water to become different substances.
Soil and sediment can also be considered to approximate a closed system
that is not well mixed. Due to the virtual lack of mixing, variations between
samples are expected to be large, and the contaminated soil near a release will
not be homogeneous. Since smaller volumes of soil than air are needed for
sampling, it can be sampled more quickly and easily. For sampling of both soil
and water, the sample is usually placed in a container for subsequent sample
preparation steps, in contrast to air sampling, which is done by removal of the
analyte from the (air) sample matrix. In some instances, soil sampling may not
be appropriate. For example, the release of a gas with a density less than
that of air would usually not be expected to contaminate nearby soil.
Sample Preparation
Sample preparation techniques usually involve the elimination of potential-
ly interfering substances from the sample. For example, this is done by total
oxidation of organic matter in the sample in the case of metals analyses, or by
column cleanup to eliminate certain interferences in organic analyses. In
addition, sample preparation can include modification of the analyte to make it
amenable to the determinative steps to follow. For example, metals in water
samples are oxidized so that all of the metal present is in the same oxidation
state, and certain organic compounds are often esterified to make them suitable
for gas chromatography. These techniques will depend on both the analyte of
interest and on the sample matrix, because the analyte must not be destroyed,
and because the potential interferences which must be removed are specific for
particular sample matrices.
Analyte Determination
The determinative procedures used on a suitably prepared sample are
usually dictated by the identity of the analyte. This is because a character-
istic of the analyte must ultimately be measured. In organic compounds this is
often a characteristic imparted by the presence of a certain functional group,
and, less frequently, the presence of a certain element such as nitrogen or
phosphorus. These characteristics may be measured by an appropriate detector
after chromatographic separation. On the other hand, in metal-containing
compounds, use is usually made of the high sensitivity and specificity possible
in determination of the metal content of samples by atomic spectrometry- The
place of element-specific inorganic analyses in the CERCLA program is discussed
in the sub-section of this report "Inorganic Listings - General Considerations.'
TECHNICAL RESULTS
This report gives Method Descriptions for 749 analytical procedures
applicable to CERCLA hazardous substances. Field methods comprise 167 of the
methods, and 582 laboratory methods are described. The cost of laboratory
analyses ranges from approximately $15.00 to $300.00 per sample in lots of six,
26
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and that of field analyses is from about $5.00 to $40.00 per sample in lots of
six. Sampling costs are not included in the costs given for laboratory anal-
yses, due to their extremely variable nature.
Of the 582 analytical procedures classified as laboratory methods, 153
cite an EPA-published reference, 178 describe a National Institute for
Occupational Safety and Health (NIOSH) or Occupational Safety and Health
Administration (OSHA) method, and 251 cite non-NIOSH/OSHA non-EPA publications.
NIOSH/OSHA references are singled out here because of the large amount of work
done by the Department of Health, Education, and Welfare (later Department of
Health and Human Services) in air analytical technology. It is also appropri-
ate to point out that these methods are intended for use in work place appli-
cations, where high levels of known target compounds are anticipated in the
absence of comparable levels of interfering compounds.
Table 3 shows the numbers of substances for which single- or multi-
compound methods were located. Single-compound methods for laboratory (field)
analysis were located for 155(67), 13(3), and 22(12) CERCLA-hazardous sub-
stances in air, soil, and water samples, respectively. For the multicompound
methods, 326(214), 438(57), and 507(263) compounds had methods located for
air, soil, and water, respectively, in the laboratory (field).
TABLE 3. SUBSTANCES FOR WHICH SINGLE- OR MULTICOMPOUND
METHODS WERE LOCATED
Type of Analysis Number of Substances
Single-Compound Multicompound
(Appendix A) (Appendix B)
Methods Methods
Laboratory -
Air 155 326 (99)*
Soil/Sediment 13 438 (1)*
Water 22 507 (8)*
Field -
Air 67 214 (24)*
Soil/Sediment 3 57
Water 12 263 (1)*
* ( ) Number of additional compounds with a single-compound method in
Appendix A as well as a multicompound method.
27
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If all 6 compound/matrix/level-of-sophistication combinations were located
for each inorganic compound, 1242 would be compiled. The actual number found
was 942, or 75 percent of the total. For organic compounds, 2460 entries are
possible, and 1134, or 46 percent of the total possible, were located. The
overall percentage of methods located was 57 percent. Table 4 shows the
number and percent of total possible compound methods located for field and
laboratory levels of sophistication for all three sample matrices. These
figures do not include duplicate compound/matrix/level-of-sophistication
entries. No methods were located for any matrix/level-of-sophistication for 31
organic substances; a method was found for at least one matrix/level-of-sophis-
tication for each inorganic substance.
TABLE 4. NUMBER OF SUBSTANCES FOR WHICH METHODS WERE LOCATED
Number for Which Percent of
Substances Method(s) Located Total Possible
Inorganic (207)
Field
Air 133 64
Soil/Sediment 45 22
Water 168 81
Laboratory
Air 203 98
Soil/Sediment 190 92
Water 203 98
Organics (410)
Field
Air 137 33
Soil/Sediment 15 4
Water 107 26
Laboratory
Air 278 68
Soil/Sediment 261 64
Water 336 82
28
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Organic Listings
General Considerations—
Organic compounds are characterized by the presence of carbon-carhon
bonds, which are nonpolar. Many organic compounds have similar physical and
chemical properties, due to structural similarities. Minor differences between
them exist due to the presence or absence of various functional groups, but in
general their solubilities, reactivity, and miscibility are similar. Since
these compounds are so numerous and many are so similar, detection by func-
tional group is possible, but compound-specific detection or measurement is
very difficult. Currently, mass spectrometry and Fourier transform infrared
spectrometry are the only detection/measurement methods with which as organic
compounds can usually be identified at trace levels; however, both of these
techniques require separation of the compound of interest from other compounds
present in the sample. Usually, this separation is performed by gas chromato-
graphy, a technique which requires that the analyte of interest be sufficiently
volatile and separable from other compounds in the sample. Novel methods of
sample introduction are being explored to attempt to make high performance
liquid chromatography (HPLC) a suitable separation step preceding mass spectrom-
etry. This would obviate the requirement that exists with gas chromatography
that the analyte by volatile or semi-volatile. Modifications of the HPLC
apparatus to encompass microbore columns are also being explored. Mass spec-
trometry frequently cannot differentiate between isomers, while Fourier trans-
form infrared spectrometry does not allow the analyst to differentiate between
homologs, or compounds that differ only in the length of a hydrocarbon chain.
In addition, for mass spectrometry to furnish completely unequivocal
compound identification, the mass spectrometer should be a high resolution
instrument, and certified pure compounds must be available or the database used
by the instrument computer must include a reference library of mass spectra
that contains information on the target compounds. The EPA/NIH database of
mass spectral data contains data for 38,971 compounds and their mass spectra,
and is usually furnished by the manufacturer when mass spectrometers are pur-
chased. However, of these compounds, only 348 are of concern under CERCLA.^
In order to generate such information, the compounds of interest must be avail-
able in pure form. The U.S. EPA Quality Assurance Reference Materials Project
(QARMP) has the responsibility of making such materials and their standard
solutions available to EPA and EPA-contractor laboratories. Of the 410 organic
compounds on the Comprehensive Hazardous Substances List, most should be amen-
able to mass spectrometric analysis for identification purposes. However,
many are currently unavailable through the QARMP-
The use of Fourier transform infrared spectrometry for environmental
analyses is still in the developmental stage. Unlike gas chromatography/mass
spectrometry (GC/MS), gas chromatography/Fourier transform infrared spectro-
metry (GC/FTIR) has not reached the stage of common use for environmental
analyses. A study by the U.S. EPA of the technique has been performed, and it
shows promise when used in conjunction with GC/MS.*° However, use of the
technique is currently limited by the size and quality of the database of
reference gas phase infrared spectra available.
29
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At higher concentrations than trace levels, more compound-specific methods
are available including nuclear magnetic resonance (NMR), (non-Fourier trans-
form) infrared spectrometry, and X-ray diffraction. However, for all of these
methods a nearly pure sample is required and, in analysis of environmental
samples, the presence of additional compounds could preclude their use. In
addition, no articles, books or other sources of information located mentioned
use of these methods in the CERCLA scenario. This report deals only with
techniques that have been shown to be somewhat applicable to use in analysis
of environmental samples: analysis of concentrated neat samples (e.g., drum or
tank residues) is not within the scope of this study.
Without compound-specific detection, analysis must rely even more heavily
upon separation procedures, to isolate the compounds of interest from other
interfering compounds present so that the signal from a non-specific detector
can be attributed to a single compound. This is particularly true for low
concentrations of analyte. Since the signal of an analytical instrument
usually results from monitoring a property that many organic compounds possess,
the analyte of interest must be removed from potentially interfering compounds.
Both gas chromatography and liquid chromatography are used extensively for this
purpose.
Other spectral techniques can provide less extensive information regarding
compound identity, but can be very useful as complementary techniques to each
other and/or to GC/MS. °>19 por exampie> ultraviolet-visible (uv-vis) spectro-
metry and fluorescence spectrometry yield information about electronic distri-
bution in a molecule, and can be quite valuable as ancillary techniques to mass
spectrometry. In addition, confirmation of tentative compound identification
can be accomplished by use of techniques including chemical derivatization, use
of dual GC columns or dual semi-specific GC detectors, thin layer chromato-
graphy (TLC), and others.
Air samples—
In the context of releases of CERCLA-hazardous substances into the air,
measurement of a wide range of concentrations, from 'ambient' levels to 'source'
levels, can be required. Ambient air is a complex and dynamic mixture with
very low levels of contaminants resulting in many potential physical/chemical
interactions. Airborne inorganic compounds can function as oxidants, water can
induce hydrolysis reactions, solid particles can act as catalytic surfaces for
reactions, and sunlight can promote photochemical transformations. In addi-
tion, organic species in air are difficult to sample and analyze because there
are a large number of compounds present in ambient air that can interfere with
measurements of typically low levels of other organic compounds. 'Source'
analytical procedures, as opposed to those for ambient air, are intended for
high levels of single, known contaminants without equivalently high levels of
interfering compounds.
Field monitoring for hazardous substances in air probably began with the
use of canaries in the mining industry. More recently, the Occupational Safety
and Health Administration (OSHA) has provided an impetus for development of
portable methods for measurement of levels of organic vapors in the workplace.
Semi-specific detector tubes, through which a known volume of air is pumped,
30
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are available for 78 of the 410 organic compounds on the Comprehensive Hazard-
ous Substances List. Table 5 lists the organic compounds on the List for which
gas detector tubes are available. In all, 137 of 410 possible methods were
located for field analysis of organics in air.
TABLE 5. ORGANIC COMPOUNDS FOR WHICH GAS DETECTOR TUBES ARE AVAILABLE
Acetaldehyde
Acetic Acid
Acetic Anhydride
Acetone
Acrolein
Acrylonitrile
Allyl Chloride
Amyl Acetate
Aniline
Aziridine
Benzene
Benzyl Chloride
Butyl Acetate
iso-Butyl Acetate
Butylamine
iso-Butyl Alcohol
n-Butyl Alcohol
Carbon Disulfide
Chlorobenzene
Chloroform
Cresol
m-Cresol
£-Cresol
£-Cresol
Cumene
Cyclohexane
Cyclohexanone
1,2-Dichlorobenzene
1,3-Dichlorobenzene
1,4-Dichlorobenzene
1,1-Dichloroethylene
1,2-trans-Dichloroethylene
1,2-Dichloropropane
Dichlorvos
Diethylamine
Dimethylamine
1,1-Dimethylhydrazine
1,2-Dimethylhydrazine
Dimethyl Sulfate
1,4-Dioxane
Epichlorohydrin
Ethyl Acetate
Ethyl Acrylate
Ethylbenzene
Ethylenediamine
Ethylene Oxide
Ethyl Ether
Formaldehyde
Formic Acid
Furfural
Methacrylonitrile
Methyl Bromide
Methylene Chloride
Methyl Ethyl Ketone
Methyl Isobutyl Ketone
Methyl Mercaptan
Methyl Methacrylate
Monoethylamine
Monomethylamine
Propionic Acid
Propylene Oxide
1,2-Propyleneimine
Pyridine
1,1,2,2-Tetrachloroethane
Tetrachloroethylene
Tetrahydrofuran
Toluene
Toluene Diisocyanate
1,2,1-Trichloroethane
Trichloroethylene
Triethylamine
Trimethylamine
Vinyl Acetate
Vinyl Chloride
Xylene
m-Xylene
o-Xylene
p-Xylene
For quantitative analysis of organic compounds in air, sampling and sample
preparation procedures become critical. The major obstacle in the development
of these procedures is the identification of a sampling process and medium
which, when combined, give quantitative recovery of the analyte from the air
volume sampled. The Environmental Monitoring Systems Laboratory, Research
Triangle Park, North Carolina, has demonstrated acceptable methods for the
determination of 43 volatile and semi-volatile organic compounds in air. If
the recovery of the analyte from the sampling medium is not quantitative,
questionable analytical results will be obtained (Mr. Steve Bromberg, Environ-
mental Monitoring Systems Laboratory, Research Triangle Park, North Carolina,
personal communication, 19 September 1982). However, partial recovery does not
rule out these media for qualitative identification. Laboratory procedures for
the determination of 278 of 410 organic compounds in air were located.
31
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The limitations of laboratory determinations of organic compounds in air
are very closely related to the weaknesses in sampling and sample preparation
steps mentioned above. For the vast majority of organic compounds on the List,
no sampling medium/preparation has been devised that has been shown" to give
quantitative absorption and desorption of analyte. Once an efficient process
has been demonstrated for both removal of the analyte from air onto or into a
sampling medium and for quantitative recovery from that medium, standard
organic determinative methods will usually be applicable. Development of such
a sampling process is difficult for environmental, or low-level, samples since
laborious cleanup procedures to control blank problems are often required for
current solid-phase collection systems.^ However, for many compounds, such
sampling methods could be devised and validated readily, with some research and
development work. One alternative method to current sampling procedures is to
concentrate organic gases into liquids at low temperature, obviating unwanted
reactions and artifacts.^ The most notable problem associated with sampling
air is that the large volumes of air needed for sampling in such instances can
often exceed the breakthrough volume for a given analyte and sampling medium,
which is the volume of air that will move the analyte completely through the
sampling system. Other problems associated with the sampling process are
irreversible sorption, vaporization, and potential decomposition or reaction of
the analyte caused by other atmospheric constituents during sampling.20
The limitations of field analytical techniques for the determination of
organics in air are related to the similarity in physical/chemical properties
of these substances. Since field equipment usually does not have the sophisti-
cated chromatographic or detection/measurement capabilities of laboratory
equipment, it frequently cannot differentiate between similar organic compounds.
For this reason, most of the field methods located for organic compounds in air
detect/measure more than one compound without differentiating between them.
Field-portable gas chromatographs, which can differentiate between
compounds, are available commercially with a wide variety of detectors and have
been used in emergency and remedial response actions.21 In addition, field-
portable infrared spectrometers are available and have been evaluated for field
use in spill responses.22
Water Samples—
Without the use of sophisticated laboratory instrumentation, field measure-
ment of organic compounds in water is not a well-developed technology. Due to
the much greater concentration of contaminants in and higher chemical activity
of water compared to air and to the complications posed by the presence of more
molecules/ions in solution, matrix interferences are much more prevalent in
water than in air. Because of the level of sophistication needed to separate
and detect or measure organics, the development of field methods for these
compounds has only recently been pursued. 3 Thin-layer chromatographic (TLC)
methods have been devised that are amenable to field use and successful use
of portable gas chromatographs has been demonstrated for a few compounds, but
the major thrust in field analysis for such analytes has been in the develop-
ment of mobile laboratories.^ Some progress could probably be made in the
development and testing of methods to remove the analyte from the problematic
water matrix and to utilize existing technology for actual analysis.25
32
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In addition, gas chromatographic static-headspace analytical methods, which
offer a large savings in analysis time compared to dynamic-headspace or purge-
and-trap methods,26'27 could be useful for initial site-characterization
efforts. Microextraction analytical techniques,28,29 wnich minimize the time
spent in sample preparation, could be valuable methods in conjunction with
field-portable instruments. In all, 107 organic compounds of 410 can be
detected or determined in water samples by the field methods located in the
appendices of this report.
Laboratory methods for the determination of organic substances in water
use separation and detection/measurement techniques which are more sophisti-
cated than those usually used for field analyses. Analytical methods for water
samples have been developed due to both the emphasis on water pollution,
through the Clean Water Act, and the fact that the water matrix presents less
of a sampling problem than air. Currently, laboratory analysis for organics in
water in the CERCLA Contractor Laboratory Program is carried out for approxi-
mately 130 compounds. Methods for the measurement of 336 of 410 organics were
located for water samples at the laboratory level of sophistication. Without
the use of GC/MS, unequivocal identification for the majority of compounds
would be almost impossible, and complementary identification data would have to
be obtained by other methods. Future progress should be expected in the
development of a combined GC/MS-GC/FTIR instrument, which could utilize the
strengths of each of these powerful techniques.
The major limitation for field methods is the lack of sophistication in
available separation and detection methods. However, by development of novel
sample preparation procedures, use could be made of existing field technologies,
like high-performance thin layer chromatography (HPTLC), paper chromatography,
and other techniques.^ Demonstration of applicability of various portable
instruments to field use and/or use of air field methods with modified sample
preparation techniques could expand field capabilities. On the other hand, the
technology-intensive laboratory is limited by reference data: the certified
standards, the pure materials needed to obtain reference mass spectra, and
computer data-handling capabilities. Progress on these fronts could come from
the EPA QARMP, the EPA/NIH mass spectral database, the GIFTS commercial FTIR
database, ^ and from instrument manufacturers.
Soil/Sediment Samples—
Field methods for only 15 organic compounds in soil/sediment samples were
located. This is probably at least partially due to the complexity and varia-
bility of the soil/sediment matrix, and the commensurate difficulties in
removal of interferences during sample preparation. However, methods for
laboratory analysis of soil/sediment samples exist, and the sample preparation
steps from these should usually be suitable for field use in combination with
existing field methods.
The technology for laboratory analysis of soil/sediment samples is the
same as that for analysis of water samples, except that the procedures used to
isolate the analyte from the matrix usually consist of a liquid-solid extrac-
tion step to dissolve the analyte in a liquid phase. The soil/sediment matrix
is more complex and variable than the water matrix, so that in most instances
additional cleanup steps are required for soil/sediment sample extracts.
33
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However, the determinative procedures carried out on a prepared sample are the
same. The same 130 compounds currently measured in water samples under CERCLA
are also measured in soil/sediment samples. Methods for 261 of 410 organics in
soil/sediment samples at the laboratory level of sophistication were located.
Inorganic Listings
General Considerations—
The List contains 207 entries which are classified as inorganic substances
in this report. Several of these compounds are organometallic compounds or
metal salts of organic acids, and a sizeable part of the molecule is organic in
nature. However, frequently the metallic part of the compound is the more
readily identified and measured one.
Laboratory methods for inorganic compounds can use sophisticated labora-
tory instrumentation to obtain better precision, accuracy, limits of detection
and certainty of identification of various ions than field methods provide.
Unfortunately, identification and measurement of a given ion often does not
satisfy the requirement of CERCLA that a particular CERCLA-hazardous substance
be identified. However, the Comprehensive Hazardous Substances List contains
14 inorganic species, with all compounds containing that moiety included. At
this time, no reportable quantity is being assigned to such listings, although,
if one were assigned, a significant diminution of the technological burden of
analysis would be removed. This is because many of the inorganic entries on
the Comprehensive Hazardous Substances List are salts that will dissociate or
hydrolyze in water or can undergo oxidation/reduction, acid/base, or complex
formation reactions quite readily in aqueous solution or in soil/sediment.
In such an instance, the CERCLA-hazardous substance is transformed into another
chemical species, the history of which cannot be known. Several of the mole-
cules and/or ions which are parts of CERCLA-hazardous substances can be indig-
enous to the sample collection area (e.g., sodium and phosphate in water, iron
and sulfides in soil/sediment).
Air Samples—
Field methods for the determination of inorganics in air are limited.
Methods were located for 133 of the 207 inorganics on the List. One limitation
is that many of these inorganic compounds are salts, with negligible vapor
pressures. Such compounds would be present in air only as particulates, and
such contaminations of air should be short-lived. The Occupational Safety and
Health Administration (OSHA) has been a major force in the development of port-
able sensing devices. These are directed at monitoring workplace air, to
ensure worker safety. The U.S. EPA Municipal Environmental Research Laboratory
in Edison, New Jersey, has not yet performed extensive air monitoring for
inorganics, except for analysis for hydrogen cyanide, hydrogen sulfide, and
ammonia for personnel safety. It has been suggested that humans smell the
vapors emanating from the ground at release sites, in order to gauge the con-
centration of the vapors. This method does not seem acceptable and, hope-
fully, development of responsible field methods for gases will continue. For
17 of the 207 inorganic entries on the Comprehensive Hazardous Substances List,
gas detector tubes are available (see Table 6). However, several of these
actually detect hydrolysis products of salts and not the hazardous substance
itself. Field air analysis capabilities for particulate inorganic compounds
34
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TABLE 6. INORGANIC SUBSTANCES FOR WHICH GAS DETECTOR TUBES ARE AVAILABLE
Ammonia Hydrogen Cyanide Nitrogen Dioxide
Chlorine Hydrogen Fluoride Phenol
Cyanogen Bromide Hydrogen Sulfide Phosgene
Cyanogen Chloride Mercury Phosphine
Hydrazine Nickel Tetracarbonyl Potassium Cyanide
Hydrochloric Acid Nitric Acid Sodium Cyanide
are mostly X-ray fluorescence methods, which are element-specific and do not
identify the particular compound containing the metal detected. Table 7 lists
the substances that are determined by field X-ray fluorescence. Use of the
same sampling procedures as for laboratory air analyses, with minor modifica-
tions of the sample preparation procedures used, combined with the use of
developed field methods for the analysis of water samples could give more
specific information about the prepared sample in the field air analyses.
TABLE 7. ELEMENTS DETERMINED
BY X-RAY FLUORESCENCE
Analyte Number of Compounds
Silicon 1
Antimony 7
Barium 1
Cadmium 4
Calcium 7
Chromium 14
Copper 10
Iron 10
Lead 14
Nickel 7
Manganese 1
Selenium 7
Zinc 16
Total 99
The National Institute for Occupational Safety and Health has developed
and validated a large number of analytical methods for inorganic compounds in
air. These are mainly element-specific methods, and they have been validated
over a specified concentration range. Laboratory methods that are applicable
to at least one portion of inorganic salts and compounds in air have been
located for 203 of the 207 inorganic substances on the Comprehensive Hazardous
Substances List. These methods do not give any information at all about the
identity of the compound containing the element determined.
35
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Many field and laboratory analytical methods for inorganic substances in
air lack specificity. Differentiation between valence states is, in the case
of chromium, possible but difficult, while unequivocal identification of the
particular metal-containing compound in a sample is beyond the reach of current
technology. X-ray diffraction methods could be applicable to such situations,
but no references citing demonstration of applicability were located in this
study- Field analytical methods for particulates in air are especially weak,
and validation of sampling/sample preparation procedures to allow use of field
water analysis determinative technology for air samples would improve this
situation greatly.
Water Samples—
Field analysis for inorganic substances in water are the best developed of
any of the field methods considered in this report. Methods were located for
168 of the 207 substances of interest. A major impetus for the development of
this technology came from the National Pollutant Discharge Elimination System,
and the need for field effluent testing it created. Analytical methods are
readily developed for inorganics in water, since water is an ideal solvent for
most inorganic substances. Methods for salts typically focus on one of the
constituents of the salt, so that methods frequently do not identify the parti-
cular compound present. Field kits exist for most heavy metal ions and, there-
fore, for their compounds, for ammonia and ammonium salts, and for cyanides,
inorganic acids, and fluorides. An EPA study found that a kit put together
from commercially available field test modules could detect most of the inor-
ganics listed in Federal Register, Vol. 40, No. 250, December, 1975.25 This
study relied very heavily upon highly non-specific methods like conductivity.
A field kit has been made available based on the results of this study, and it
is claimed to detect "over 300 compounds" in waterways. CERCLA requires
specific identification of substances from the List, so that non-specific
measurements are of limited use under the Act. However, such methods are use-
ful in field analyses, in order to gauge the extent of migration of a release
and thereby to plan a thorough and efficient sampling plan. Field kits,
including test papers, are available for the substances listed in Table 8.
Laboratory analytical methods for water samples have been located for all
but 9 of the 207 inorganic entries on the Comprehensive Hazardous Substances
List. However, most of these methods are applicable to only one portion of
the inorganic compound and are therefore of limited utility under CERCLA, since
they do not specifically identify a CERCLA compound. Table 9 lists the inor-
ganic species for which water and soil/sediment samples are analyzed in the
current CERCLA program."
Soil/Sediment Samples—
Field methods for 45 of the 207 inorganic substances on the Comprehensive
Hazardous Substances List have been located for the soil/sediment matrix.
Unfortunately, most of the methods located were elemental methods, which detect
or measure one element present in the compound.
36
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TABLE 8. ANALYTES THAT CAN BE DETERMINED IN WATER
SAMPLES USING TEST KITS
Analyte Number of Compounds
Aluminum 2
Aluminum (P) 2
Ammonia 31
Antimony (P) 7
Cadmium 4
Chromates 6
Chromium(VI) 12
Chromium (P) 19
Chromium 14
Copper 10
Copper (P) 10
Fluorides and others 17
Halides, cyanides, and others* 44
Hydrazines* 3
Lead 14
Lead (P) 14
Mercury 7
Nickel ions (P) 8
Nitrate ions 14
Potassium (P) 10
Selenium 7
Silver 4
Sulfite ions (P) 3
Zinc (P) 16
Zinc 16
Zirconium 4
Total 298
by field kit: 209
by test paper: 89
(P) Test Paper method
* 10 of the 47 compounds measured by these tests are
organics
Analytical capabilities for inorganics in soil/sediment at the laboratory
level of sophistication are nearly as well developed as for water, with 190 of
the possible 207 entries accounted for. Table 9 shows the inorganic species
for which analysis of water and soil/sediment samples are performed under
current CERCLA contracts. As with determinations of inorganic substances in
air and water samples, specific identification of compounds is difficult to
impossible.
37
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TABLE 9. INORGANICS MEASURED IN WATER AND SOIL SAMPLES UNDER CERCLA
Aluminum
Antimony
Arsenic
Barium
Beryllium
Boron
Cadmium
Chromium
Cobalt
Copper
Iron
Lead
Manganese
Mercury
Nickel
Selenium
Silver
Thallium
Tin
Vanadium
Zinc
Ammonia
Cyanide
Sulfide
FINANCIAL RESULTS
Specific cost information is included as part of each Method Description
in the appendices. Average costs for analysis by each method are shown in
Table 10. Cost averages for miscellaneous instrumental methods are not
included, because the cost figures have a wide range and the average is not
very meaningful. For the same reasons, overall cost averages have not been
compiled. Laboratory instrumental analysis for organic compounds is substan-
tially more expensive than other types of analysis. Readers should keep in mind
that prices for analysis can vary widely, depending upon current economic
conditions, laboratory equipment and specialty, and other factors. For that
reason, the contents of this report should not be considered a rigid price
list.
TABLE 10. METHOD- AND COST-SEARCH RESULTS
Laboratory Methods
AA or ICP
X-Ray fluorescence
Colorimetry
IR
Wet methods
Miscellaneous instrumental
GC
GC/MS
HPLC
Other
Non-NIOSH
Non-EPA
3
17
31
60
6
30
83
7
13
1
NIOSH
13
1
26
2
13
107
1
15
EPA
75
14
5
37
10
11
1
Average Cost
$ 20.00
32.00
35.00
70.00
25.00
90.00
285.00
130.00
TOTAL 251
178
153
Field Methods
X-Ray fluorescence
Test sticks/indicator papers
Wet methods/colorimetry
Miscellaneous instrumental
Detector tubes
TOTAL
Number of Methods
19
18
48
10
64
Average Cost
$32.00
4.50
20.00
- 16.50
159
38
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MOBILE LABORATORY SURVEY RESULTS
Instrumentation
The appendices of this report describe laboratory and field analyses, but
the definition of neither classification incorporates the special cases of
analyses by mobile laboratories. Therefore, a study was undertaken to explore
this topic. The following information is from the resulting report.
A commercial mobile laboratory is typically a vehicle with appropriate
support systems and a selection of sophisticated instruments that varies with
the needs of a particular situation. Table 11 is a list of instruments used in
selected commercial mobile laboratories. Gas chromatographs in mobile labora-
tories employ one or more of a variety of detectors: flame ionization detector
(FID), thermal conductivity detector (TCD), photoionization detector (PID),
electron-capture detector (ECD), flame photometric detector (FPD), and Hall
electrolytic conductivity detector (HECD). Brands and models of gas chroraato-
graph identified as having been used in commercial mobile laboratories are the
Hewlett-Packard HP5840, Perkin-Elmer P-E 3920, HNU, and Tracor Instruments Inc.
Model 560. Many smaller instruments and pieces of equipment, such as the
Miran® IR or bomb calorimeter, are also used routinely. The U.S. Coast Guard
has successfully used a Fourier transform infrared spectrometer (FTIR) in a
mobile laboratory in response to an environmental incident.
A Canadian firm, Sciex Ltd., has developed instruments with mass spectro-
metric detector systems that can sample air directly, and has begun manufactur-
ing a mobile laboratory equipped with them. The mobile laboratory is available
with either a TAGA™ 3000 GC/MS or a TAGA™ 6000 (GC) MS/MS system. Demonstrated
uses of TAGA™ systems include the following: tracing the chlorine from a train
derailment; determining PCB's in cement kiln stack gas, ambient air, and soil;
air monitoring at landfills for 20 compounds and in the workplace for bis-
(chloromethyl)ether; analyzing hazardous waste barrel contents; direct soil
surface sniffing; hazardous waste emission monitoring; and continuous on-line
monitoring of combustion gases and automobile engine exhausts. » Direct
MS/MS analysis cannot be used alone when certain interferences are present.
In such instances, flash gas chromatography is used before MS/MS as a gross
cleanup step. " The ionization sources for the TAGA™ 6000 are not completely
effective in all situations, but the instrument has significant applications
in many instances."
Procedures
The U.S. EPA Municipal Environmental Research Laboratory, Oil and Hazard-
ous Materials Spills Branch, Edison, New Jersey (MERL-Edison or MERL-OHMSB) has
pioneered EPA efforts to provide rapid on-site mobile laboratory analytical
capabilities. Table 12 lists past MERL-Edison mobile laboratory responses and
the principal analytes measured at each site.
In order to process the potentially large number of samples expected at
release sites and/or to obtain timely results, many of MERL-Edison!s mobile
laboratory analytical procedures attempt to save time by modifying traditional
sample workup procedures (e.g., APHA, ASTM, EPA) and/or through use of more
39
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TABLE 11. INSTRUMENTS USED IN SELECTED COMMERCIAL MOBILE LABORATORIES
Chemi-
lumin-
X-Ray escence UV/VIS
Fluor- NOx Spec-
Firm* GC GC/MS AA HPLC VOC TOX TOC escence Analyzer trometer
Alert x
EAL x
ES
ESE
GCA
IT x
OHM x
Radian x
RTS x
SCA x
x
X
X
XXX
XXX
**
X
* = Acronyms refer to the following companies:
EAL = EAL Corporation, Richmond, California.
ES = Engineering-Science, Arcadia, California.
ESE = Environmental Science and Engineering, Inc., Gainesville, Florida.
GCA = GCA Corporation, Bedford, Massachusetts.
IT = IT Corporation, Wilmington, California.
OHM = 0. H. Materials, Findlay, Ohio.
RTS = Resource Technology Service, Inc., Devon, Pennsylvania.
SCA = SCA Waste Chemical Co., Inc., Cheektowaga, New York.
** = Will be used in a pending job.
t = Finnigan OWA GC/MS.
ft = Usage has been limited, but capability is present.
rapid instrumental determinative steps. The procedures at MERL-Edison are
designed to minimize losses in precision and accuracy, to use less space, and
to generate less waste.
Traditional methods developed for lower levels of contamination in environ-
mental matrices are often tedious and time consuming. Such procedures fre-
quently involve extraction, evaporative concentration, chromatographic cleanup,
40
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TABLE 12. MERL-EDISON MOBILE LABORATORY RESPONSES AND ANALYTES
Location
Date
Analyte(s)
Haverford, Pennsylvania
Dittmer, Missouri
Oswego, New York
Niagara, New York
Elizabeth, New Jersey
Pittston, Pennsylvania
Crosby, Texas
Moira, New York
Seymour, Indiana
Kingston, New Hampshire
La Marque, Texas
Nov. 1976
Apr. 1977
Oct. 1977
Oct. 1978
May 1979
Aug. 1979
Feb. 1980
Oct. 1980
Nov. 1980
Jan. 1981
Sep. 1981
Pentachlorophenol
PCB's
PCB's
Chlorinated benzenes
PCB's
£-Dichlorobenzene
PCB's
PCB's
Priority pollutants
PCB's, pesticides
Purgeable compounds
BHC, PCB's
and other steps to remove interferences and concentrate the analyte in order
to obtain a reliable instrumental response for the analyte of interest. In
spill responses, however, the analyte-to-interference concentration ratio is
much higher, and the sample preparation procedure is usually not so critical.
In addition, the identity of the spilled material is often known, so that use
of more rapid and direct sample preparation procedures and analytical methods
is possible. For example, MERL-Edison has developed procedures for organics
with a rapid extraction step, such as simply spinning the sample with the
extraction solvent.3'~^2 por certain situations, the extraction step has been
completely omitted.^3 Streamlined cleanup techniques and use of positive dis-
placement micropipets to eliminate multiple dilutions of samples and standards
have also been adopted.39,40
MERL-Edison has not yet been requested to perform analyses with the
results to be used in litigation but has always concentrated on site character-
ization and the monitoring of remedial response efforts. However, standard
analytical procedures are performed in the mobile laboratory when it is located
in Edison, New Jersey- This indicates that the laboratory is capable of gener-
ating high-quality analytical data that can be used in litigation activities,
provided support systems equivalent to those in Edison are available on site.
It is expected that this situation applies to all mobile laboratories now in
use.
MERL-Edison is currently assembling a manual of their tested analytical
protocols for mobile-laboratory use that will be applicable to approximately
240 of the CERCLA hazardous substances in air, water, or soil. Table 13 lists
those substances on the CERCLA Comprehensive Hazardous Substances List that
MERL-Edison has measured in the field with a mobile laboratory, and for which
protocols are being prepared. The instrumentation required to perform the
analyses for the substances listed in Table 13 include GC/MS, GC/ECD or GC/HECD,
GC/NPD, GC/FID, spectrofluorometers, infrared spectrometers, emission spectrom-
eters, carbon analyzers, inductively coupled atomic plasma emission
41
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TABLE 13. HAZARDOUS COMPOUNDS ANALYZED BY THE MERL-EDISON MOBILE LABORATORY
Compound Name CAS No. Compound Name CAS No.
Acenaphthene
Acenaphthylene
Acrolein
Aldrin
Aluminum Sulfate
Aniline
Anthracene
Ant imony
Aroclor 1016
Aroclor 1221
Aroclor 1232
Aroclor 1242
Aroclor 1248
Aroclor 1254
Aroclor 1260
Arsenic
Benzal Chloride
Benzene
Benzidine
Benzo[ajanthracene
Benzo[a]pyrene
Benzo[b]fluoranthene
Benzo[k]fluoranthene
Benzo[ghi]perylene
Benzoic Acid
Benzonitrile
Benzotrichloride
Benzyl Chloride
Beryllium (and
Compounds)
a-BHC
8-BHC
Bromoform
Cadmium (and
Compounds)
Carbon Tetrachloride
Chlordane
Chlorobenzene
Chloroethane
Chloroform
£-Chloro-m-cresol
83-32-9 2-Chloronaphthalene 91-58-7
208-96-8 Chlorophenol (all Isomers) 25167-80-0
107-02-8 2-Chlorophenol 95-57-8
309-00-2 Chromium (and 7440-47-3
10043-01-3 Compounds)
62-53-3 Chrysene 218-01-9
120-12-7 Copper (and Compounds) 7440-50-8
7440-36-0 Cresol 1319-77-3
12674-11-2 Cyclohexane 110-82-7
11104-28-2 ODD 72-54-8
11141-16-5 DDE 72-55-9
53469-21-9 DDT (and Metabolites) 50-29-3
12672-29-6 Dibenz[a,h]anthracene 53-70-3
11097-69-1 Dibenz[a,i]pyrene 189-55-9
11096-82-5 Dichlorobenzene 25321-22-6
7440-38-2 (Mixed)
98-87-3 1,2-Dichlorobenzene 95-50-1
71-43-2 1,3-Dichlorobenzene 541-73-1
92-87-5 1,4-Dichlorobenzene 106-46-7
56-55-3 Dichlorobromomethane 75-27-4
50-32-8 Dichloroethane 1300-21-6
205-99-2 1,1-Dichloroethane 75-34-3
207-08-9 1,2-Dichloroethane 107-06-2
191-24-2 Dichloroethylene (all 25323-30-2
65-85-0 Isomers)
100-47-0 1,1-Dichloroethylene 75-35-4
98-07-7 1,2-Dichloroethylene 156-60-5
100-44-7 2,4-Dichlorophenol 120-83-2
7440-41-7 2,6-Dichlorophenol 87-65-0
Dichloropropane (all 26638-19-7
319-84-6 Isomers)
319-85-7 1,2-Dichloropropane 78-87-5
75-25-2 Dieldrin 60-57-1
7440-43-9 Diethyl Phthalate 84-66-2
2,4-Dimethylphenol 105-67-9
56-23-5 Dimethyl Phthalate 131-11-3
57-74-9 Di-n-butyl Phthalate 84-74-2
108-90-7 Dinitrobenzene (all 25154-54-5
75-00-3 Isomers)
67-66-3 4,6-Dinitro-o-cresol 534-52-1
59-50-7 Dinitrophenol (all 25550-58-7
Isomers)
2,4-Dinitrophenol 51-28-5
(continued)
42
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Compound Name
TABLE 13,
CAS No.
(Continued)
Compound Name
CAS No,
Dinitrotoluene (all 25321-14-6
Isomers)
2,4-Dinitrotoluene 121-14-2
2,6-Dinitrotoluene 606-20-2
Endosulfan 115-29-7
Endrin (and Metabolites) 72-20-8
Ethylacetate 141-78-6
Ethylbenzene 100-41-4
Ethylene Dibromide 106-93-4
Fluoranthene 206-44-0
Fluorene 86-73-7
Halomethanes
Heptachlor 76-44-8
Heptachlor Epoxide 1024-57-3
Hexachlorobenzene 118-74-1
Hexachlorobutadiene 87-68-3
Hexachloroethane 67-72-1
Kepone 143-50-0
Lead Acetate 301-04-2
Lead (and Compounds) 7439-92-1
Lindane 58-89-9
Malathion 121-75-5
Mercury (and Compounds) 7439-97-6
Methanol 67-56-1
Methoxychlor 72-43-5
Methyl Bromide 74-83-9
Methyl Chloride 74-87-3
Methyl Parathion 298-00-0
Methylene Bromide 74-95-3
Methylene Chloride 75-09-2
Naphthalene 91-20-3
Nickel (and Compounds) 7440-02-0
Nitrobenzene 98-95-3
Nitrophenol (all 25154-55-6
Isomers)
2-Nitrophenol 88-75-5
4-Nitrophenol 100-02-7
Nitrotoluene 1321-12-6
Parathion 56-
Pentachlorobenzene 608-
Pentachloroethane 76-
Pentachloronitrobenzene 82-
Pentachlorophenol 87-
Phenanthrene 85-
Phenol 108-
Polynuclear Aromatic
Hydrocarbons
Pyrene 129-
Pyridine 110-
Quinoline 91-
Resorcinol 108-
Selenium (and Compounds) 7782-
Silver (and Compounds) 7440-
Sodium 7440-
Sodium Hydroxide 1310-
1,2,4,5-Tetrachlorobenzene 95-
1,1,1,2-Tetrachloroethane 630-
1,1,2,2-Tetrachloroethane 79-
2,3,4,6-Tetrachlorophenol 58-
Thallium (and Compounds) 7440-
Toluene 108-
Toxaphene 8001-
1,2,4-Trichlorobenzene 120-
1,1,1-Trichloroethane 71-
1,1,2-Trichloroethane 79-
Trichloroethylene 79-
Trichloromonofluoro- 75-
methane
Trichlorophenol 25167-
2,4,5-Trichlorophenol 95-
2,4,6-Trichlorophenol 88-
sym-Trinitrobenzene 99-
XyTene 1330-
Xylenol 1300-
Zinc (and Compounds) 7440-
•38-2
•93-5
•01-7
•68-8
•86-5
•01-8
•95-2
00-0
86-1
22-5
46-3
49-2
22-4
23-5
73-2
94-3
20-6
34-5
90-2
28-0
88-3
35-2
82-1
55-6
00-5
01-6
69-4
82-2
95-4
06-2
35-4
•20-7
•71-6
•66-6
43
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spectrometers (ICP), and atomic absorption spectrometers (AA). In addition to
providing field operation guidance for the instruments listed, each protocol
provides guidance on sample isolation, fractionation, screening, and the use of
appropriate safety devices.
The MERL OHMSB mobile laboratory has developed specific quality assurance
protocols for use in mobile laboratory responses. Several QA/QC protocols
are designed to generate method validation data concurrently with sample
results in order to give the on-site coordinator real-time feedback on
analytical quality.^" Use of a single standard to define the linear dynamic
calibration range for a large number of compounds eliminates the need for ex-
tensive preanalysis instrument calibration. "»40 ^ series of complementary
QA protocols that describe the preparation of synthetic samples for method
validation have been prepared. These make use of aqueous, non-aqueous, or
sediment media that resemble the site samples and include detailed instructions
for fortification of samples with water-soluble, partially water-soluble,
water-insoluble, and volatile materials.
Several commercial firms have designed their own mobile laboratory sampl-
ing, sample work-up, and analytical methods, but most firms use procedures
designed for standard laboratory analyses, or make minor modifications.
Typically, the same quality assurance procedures that are employed in the main
laboratory are employed in the field units.
Cost Factors
According to one firm that provides both mobile and fixed-site laboratory
services, the first two factors considered in setting a price for a mobile
laboratory activation are how rapid a response is required and how many samples
per day will be processed. If the mobile laboratory support effort is of suffi-
cient magnitude, analytical costs may be lower than those incurred at a fixed-
site laboratory. For example, an on-site compatibility screening (PCB, oxidant,
reductant, cyanide, and sulfide) of up to 200 samples per day was performed at
a cost of approximately $15.00 per sample. Such large numbers of samples can
help distribute the capital costs of mobilization. A 2-day job would have
prohibitive mobilization costs, while a stay of 1 to 2 weeks could be cost
-effective. If laboratory trailers were located in several areas of the
country, mobilization costs could be greatly reduced. For nearly all on-site
analytical programs, costs are determined on the basis of outfitting a mobile
laboratory with men and equipment. Normally, for the use of a mobile labora-
tory, a fixed daily rate is charged that includes glassware, extractors, and
miscellaneous supplies. Any reagents or supplies that must be expended are
charged. Major equipment such as a gas chromatograph is charged at a daily
rate with discounts according to the duration of the job. Besides the probabil-
ity of lower charges when a sufficient number of samples is processed per day,
an added benefit of on-site analysis is quick turnaround time that may signifi-
cantly lower the costs of other contractors on the site.
44
-------
REFERENCES
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Hazardous Substances; EPA-600/X-82-016, U.S. Environmental Protection
Agency: Las Vegas, 1982.
3. Gruenfeld, M.; Frank, U.; Remeta, D. "Rapid Methods of Chemical Analysis
Used in Emergency Response Mobile Laboratory Activities" Proc. U.S. EPA
Nat. Conf. on Management of Uncontrolled Hazardous Waste Sites, 1980;
Hazardous Materials Control Research Institute: Silver Spring, Maryland,
pp. 165-172.
4. Engels, J. L.; Kerfoot, H. B.; Arnold, D. F. Survey of Mobile Laboratory
Capabilities and Configurations; EPA 600/X-84-170, U.S. Environmental
Protection Agency: Las Vegas, 1984.
5. Besterfield, D. H. Quality Control; Prentice Hall: Englewood Cliffs,
New Jersey, 1979.
6. U.S. Environmental Protection Agency, Handbook for Analytical Quality
Control in Water and Wastewater Laboratories; EPA-600/4-79-019, U.S. EPA:
Cincinnati, 1979.
7. U.S. Environmenal Protection Agency, Organics Analysis, Multi-Media,
Multi-Concentration, GC/MS with Medium-Level GC Screen, Exhibit D: Invita-
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15, 1984.
8. U.S. Environmental Protection Agency, Chemical Analytical Services for Low
and Medium Concentration Inorganics in All Media, Exhibit D; Invitation
for Bid (Solicitation Number WA82-A072), U.S. EPA: Washington, April 23,
1982.
9. U.S. Environmenal Protection Agency, Test Methods for Evaluating Solid
Waste; Physical/ Chemical Methods, 2nd ed.; SW-846, U.S. EPA: Washington,
July 1982.
10. U.S. Environmental Protection Agency, Methods for Chemical Analysis of
Water and Wastes; EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979.
Technical Additions to Methods for Chemical Analysis of Water and Wastes:
EPA-600/4-82-055; U.S. EPA: Cincinnati, 1982.
45
-------
11. U.S. Environmental Protection Agency. Methods for Organic Analysis of
Municipal and Industrial Wastewater; J. E. Longbottom and J. J. Litchenberg,
Eds.; EPA-600/4-82-057, U.S. EPA: Cincinnati, 1982.
12. U.S. Department of Health and Human Services (U.S. Department of Health,
Education, and Welfare), NIOSH Manual of Analytical Methods, Vol. 1-7; U.S.
DHHS (U.S. DHEW): Cincinnati, 1974-1981.
13. American Society for Testing and Materials, ASTM Standards on Chromato-
graphy. 1st ed.; ASTM: Philadelphia, 1981.
14. American Society for Testing and Materials, 1983 Annual Book of ASTM
Standards, Section 11 (Water); ASTM: Philadelphia, 1983.
15. American Public Health Association, Methods of Air Sampling and Analysis,
2nd ed., M. Katz, Ed.; APHA: Washington, 1977.
16. Bendix Environmental and Process Instruments Division, Largo, Florida;
Chemtech Consulting Group, Inc., New York, New York; Draegerwerk AG,
Lubeck, Germany; Energy Resources Co., Inc., Environmental Resources
Division, Cambridge, Massachusetts; Gallard-Schlesinger Chemical Mfg.
Corp., Carle Place, New York; Hach Chemical Company, Ames, Iowa; Hazelton
Laboratories of America, Inc., Madison, Wisconsin; Rocky Mountain Analytical
Laboratory, Arvada, Colorado; IT Analytical Services, Cerritos, California;
Woodward-Clyde Consultants, Oakland, California.
17. "CLP Analytical Laboratories Costing and Deliverables", October 7, 1983,
Environmental Protection Agency. "Preliminary Assessment of the Impact
of Waste Disposal Sites on Ground Water and on the Niagara River in Western
New York," February 12, 1982, United States Department of the Interior.
18. Gurka, D. G. Applications of GC/FTIR and GC/MS Techniques for Total
Analysis of Volatile Toxic Substances in Hazardous Wastes; EPA-600/X-82-
029, U.S. Environmental Protection Agency: Las Vegas, 1982.
19. Shafer, K. H.; Cooke M.; DeRoos F.; Jakobsen R. J.; Rosario 0.; Mulik,
J.D. "WCOT Capillary Column GC/FT-IR and GC/MS for Identifying Toxic
Organic Pollutants, Appl. Spect., 35., 1981, pp. 469-472. See also Anal.
Chem., 54_(11), 1982, pp. 1819-1824, and Appl. Spect. Rev., L5(2), 1979^
pp. 261-325.
20. Hauser, T. R.; Scott, D. R.; Midgett, M. R. "EPA Methods Development
Needs for Regulatory Air Pollution Monitoring" In Identification and
Analysis of Organic Pollutants, L. H. Keith, Ed.; Butterworth: Boston,
1984.
21. Spittler, T. M. "Field Measurement of PCB's in Soil and Sediment Using a
Portable Gas Chromatograph" In Proceedings of the Fourth National Confer-
ence on Management of Uncontrolled Hazardous Waste Sites; Hazardous
Materials Control Research Institute: Silver Spring, Maryland, 1983.
46
-------
22. Denton, M. S.: Walker, M. H. "Portable Infrared Field Monitor for PCB's:
Phase II" In Proceedings; 1983 PCS Seminar, Electric Power Research
Institute: Palo Alto, California, EPRI EL-3581 (Project 2028), 1984.
23. Jacot, B. J. "OVA Field Screening at a Hazardous Waste Site" In Proceedings
of the Fourth National Conference on Management of Uncontrolled Hazardous
Waste Sites; Hazardous Materials Control Research Institute:Silver
Spring, Maryland, 1983.
24. Sherma, J. "Sample Preparation for Quantitative TLC" In Thin Layer
Chromatography; Quantitative Environmental and Clinical Applications,
J. C. Touchstone and D. Rogers, Eds.; Wiley-Interscience: New York, 1982,
pp. 17-35.
25. U.S. Environmental Protection Agency "Development of a Kit for Detecting
Hazardous Materials Spills in Waterways"; EPA-600/2-78-055, U.S. EPA:
Cincinnati, March, 1978.
26. Cowen, W. F.; Baynes, R. K. "Estimated Application of Gas Chromatographic
Headspace Analysis to Priority Pollutants:, J. Environ. Sci. Health,
A15(5), 1980, pp. 413-427.
27. Umbreit, G. R.; Grob, R.L. "Experimental Application of Gas Chromatographic
Headspace Analysis to Priority Pollutants'1, J. Environ. Sci. Health,
A15(5), 1980, pp. 429-466.
28. Rhoades, J. W.; Nulton, C. P. "Priority Pollutant Analyses of Industrial
Wastewaters Using a Microextraction Approach", J. Environ. Sci. Health,
A15(5), 1980, pp. 467-484.
29. Thrum, K. E.; Simmons, K. E.; Oberholtzer, J. E. "An Evaluation of Factors
Affecting the Microextraction of Benzene, Toluene, Ethylbenzene, and o-
Xylene into Pentane" J. Environ. Sci. Health, A15(5), 1980, pp. 485-501.
30. GIFTS Operators Manual, M091-0128; Digilab, Cambridge, Massachusetts,
1981, and Hanna, A.; Marshall, J. C.; Isenhour T. L. J. Chromatogr.
Sci., 17_, 1979, p. 434-440.
31. Skoog, D. A.; West, D. M. Fundamentals of Analytical Chemistry, 3rd ed.:
Holt, Rinehart and Winston: New York, 1981.
32. Astle, A. D.; Duffee R. A.; Stankunas A. R.; "Estimating Vapor and Odor
Emission Rates from Hazardous Waste Sites", Proc. of Nat. Conf. on Manage-
ment of Uncontrolled Hazardous Waste Sites; Hazardous Materials Control
Research Institute, Silver Spring, Maryland, 1982.
33. Hach Company, Loveland, Colorado.
34. Literature supplied by Sciex Ltd., Thornhill, Ontario, Canada.
47
-------
35. French, J. G.; Davidson, W. R.; Reid, N. M.; Buckley, J. A.
In Tandem Mass Spectrometry, Chapter 18; F. W. McLafferty, Ed.; John Wiley
and Sons: New York, 1983, pp. 353-370.
36. Tanner, S.; Ngo, A.; Davidson, W. "Optimizing Productivity for the Trace
Analysis of Real-Life Samples Using Flash Gas Chromatography MS/MS."
Extended Abstract, ASMS Conference, Boston, 1983.
37. Frank, U.; Gruenfeld, M.; Losche, R; Lafornara, J. Mobile Laboratory
Safety and Analysis Protocols Used at Abandoned Chemical Waste Dump Sites
and Oil and Hazardous Chemical Spills, 1980 National Conference on Control
of Hazardous Materials Spills, Louisville, Kentucky. Copyright held by
Vanderbilt University, Nashville, Tennessee.
38. Gruenfeld, M. "Extraction of Dispersed Oils from Water for Quantitative
Analysis by Infrared Spectrophotometry," Environ. Sci. Technol., 1_, 1973,
pp. 636-639.
39. Gruenfeld, M. ; Frank, U.; Remeta, D. "Rapid Methods of Chemical Analysis
Used in Emergency Response Mobile Laboratory Activities," from Proc. U.S.
EPA Nat. Conf. on Management of Unc. Haz. Waste Sites, October 15-17,
1980; Hazardous Materials Control Research Institute: Silver Spring,
Maryland, pp. 165-172.
40. Gruenfeld, M.; Frank, U.; Remeta, D. Specialized Methodology and Quality
Assurance Procedures Used Aboard Mobile Laboratories for the Analysis of
Hazardous Wastes, 185th National Meeting of the American Chemical Society,
March 28-April 21, 1983; American Chemical Society: Washington, DC,
Abstr. Div. Environmental Chemistry.
41. Frank, U.; Pernell, L. "Synchronous Excitation Fluorescence Spectroscopy,"
Analytical Quality Control Newsletter, No. 31; U.S. EPA: Cincinnati,
Ohio, 1976.
42. Frank, U.; Remeta, D. "Rapid Quantification of Hazardous Materials in
Sediments by Synchronous Excitation Fluorescence Spectroscopy," EPA Quality
Assurance Newletter, 1:4; U.S. EPA: Cincinnati, Ohio, 1978.
43. Losche, R.; Frederick, R: Frank, U. "Analysis of Oil and PCB's in Sedi-
ments," EPA Quality Assurance Newsletter, 3; U.S. EPA: Cincinnati, Ohio,
April 1980.
44. Literature supplied by 0. H. Materials Company, Findlay, Ohio.
48
-------
Index and Table of Contents for Appendix A
49
-------
CAUTION
The following information is presented in each volume containing the
appendices to the report. These facts are presented to ensure that the infor-
mation presented in the appendices is clearly defined and that what is not
intended to be included is outlined.
The Method Descriptions presented in Appendix A and Appendix B are not
intended to be critical reviews of analytical methods, but comprise an anno-
tated bibliography. The Method Descriptions are only a brief summary of the
information contained in the reference(s) being described. Efforts were pur-
posely made to avoid speculation about applications of methods to analytes or
sample matrices not documented by a reference. There is an Index/Table of
Contents which tells the name for each substance used throughout the report.
See the text of the report for a detailed description of the contents of the
Method Descriptions and for the reasons for preparation of the appendices and
report.
The cost figures furnished for each method are presented following the
Method Descriptions, and should not be used as a price list. For a discussion
of the factors involved in figuring the cost figures cited, see the text of the
report.
50
-------
Use of this Index
This Index contains each regulatory synonym for specific hazardous sub-
stances designated under the Federal Water Pollution Control Act (Clean Water
Act), the Clean Air Act, and the Resource Conservation and Recovery Act. To
the right of each entry is the Chemical Abstracts Service (CAS) Registry
Number, to aid in unequivocal identification of the substance. To the right of
the CAS number is the consensual name, or the synonym chosen for use throughout
this report, followed by the page in Appendix A where method descriptions
and/or references to Appendix B can be found.
51
-------
Hazardous Substance
CAS No.
Consensual Name
Page
Acenaphthene
Acenaphthylene
Acetaldehyde
Acetaldehyde, Chloro-
Acetaldehyde, Trichloro-
Acet amide, N-(Aninothioxomethyl)-
Acet amide, N-(4-Ethoxyphenyl)-
Acetamide , N-9H-Fluoren-2-yl-
Acet amide, 2 -Fluor o-
Acetlc Add
Acetic Acid, Ethyl Ester
Acetic Acid, Fluoro-, Sodium Salt
Acetic Acid, Lead Salt
Acetic Acid, Thallium(I) Salt
Acetic Anhydride
Acetimldic Acid, N-[(aethylcar-
bamoyl)ozy]thio-, Methyl Ester
Acetone
Acetone Cyanohydrln
Acetonltrile
3- (a -Acetonylbenzy 1 )-4-
Hydrozycounarin and Salts
Acetophenone
2-Acetylaminofluorene
Acetyl Bromide
Acetyl Chloride
l-Acetyl-2-Thlourea
Acrolein
Acrylamlde
Acrylic Acid
Acrylonitrile
Adlplc Acid
Alanlne, 3-[j>-bls(2-chloroethyl)-
aml no ] pheny 1- , L-
Aldlcarb
Aldrin
Allyl Alcohol
Allyl Chloride
Aluminum Phosphide
Aluminum Sulfate
5-(Amlnomethyl)-3-lsoxazolol
4-Amlnopyridlne
Ami t role
Ammonia
Ammonium Acetate
Ammonium Benzoate
Ammonium Bicarbonate
Ammonium Bichromate
Ammonium Bifluorlde
Ammonium Bisulfite
Ammonium Carbamate
Ammonium Carbonate
Ammonium Chloride
Ammonium Chromate
Ammonium Citrate, Dibasic
83-32-9
208-96-8
75-07-0
107-20-0
75-87-6
591-08-2
62-44-2
53-96-3
640-19-7
64-19-7
141-78-6
62-74-8
301-04-2
563-68-8
108-24-7
16752-77-5
67-64-1
75-86-5
75-05-8
81-81-2
98-86-2
53-96-3
506-96-7
75-36-5
591-08-2
107-02-8
79-06-1
79-10-7
107-13-1
124-04-9
148-82-3
116-06-3
309-00-2
107-18-6
107-05-1
20859-73-8
10043-01-3
2763-96-4
504-24-5
61-82-5
7664-41-7
631-61-8
1863-63-4
1066-33-7
7789-09-5
1341-49-7
10192-30-0
1111-78-0
506-87-6
12125-02-9
7788-98-9
3012-65-5
Chloroacetaldehyde
Chloral
l-Acetyl-2-thlourea
Phenacetln
2-Acetylamlnofluorene
Fluoroacet amide
Ethyl Acetate
Fluoroacetlc Acid, Sodium Salt
Lead Acetate
Thalllum(I) Acetate
Methomyl
Warfarin
Melphalan
Ammonium Dlchromate
A-287
A-288
A-289
A-437
A-433
A-310
A-819
A-307
A-656
A-293
A-621
A-657
A-135
A-254
A-296
A-716
A-298
A-301
A-303
A-951
A-306
A-307
A-308
A-309
A-310
A-311
A-315
A-316
A-318
A-322
A-708
A-323
A-324
A-326
A-328
A-3
A-4
A-331
A-332
A-333
A- 5
A-334
A-335
A-9
A-15
A-10
A-ll
A-336
A-12
A-13
A-14
A-337
52
(continued)
-------
Hazardous Substance
CAS No.
Consensual Name
Page
Ammonium Dichronate
Ammonium Fluoborate
Ammonium Fluoride
Ammonium Hydroxide
Ammonium Oxalate
Ammonium Picrate
Ammonium Sllicofluorlde
Ammonium Sulfamate
Ammonium Sulfide
Ammonium Sulfite
Ammonium Tartrate
Ammonium Thiocyanate
Ammonium Thiosulfate
Ammonium Vanadate
Amyl Acetate
iso-Amyl Acetate
sec-Amy 1 Acetate
tert-Amyl Acetate
Aniline iS*-i.-
Anthracene
Antimony
Antimony Pentachloride
Antimony Potassium Tartrate
Antimony Tribromide
Antimony Trichloride
Antimony Trlfluorlde
Antimony Trioxide
Aroclor 1016
Aroclor 1221
Aroclor 1232
Aroclor 1242
Aroclor 1248
Aroclor 1254
Aroclor 1260
Arsenic
Arsenic Acid
Arsenic Dlsulfide
Arsenlc(III) Oxide
Arsenlc(V) Oxide
Arsenic Pentoxlde
Arsenic Trichloride
Arsenic Trioxide
Arsenic Trisulflde
Arslne. Diethyl-
Asbestos
Auramlne
Azaserine
Azirldine
Azirino(2',3':3,4)pyrrolo(l,2-a)-
lndole-4,7-dlone ,6-«mlno-8-
[((aminocarbonyl)oxy)«ethyl]-
l.la,2,8,8a,8b-hexahydro-8a-
»ethoxy-5-»ethyl-
7789-09-5
13826-83-0
12125-01-8
1336-21-6
6009-70-7
5972-73-6
14258-49-2
131-74-8
16919-19-0
7773-06-0
12135-76-1
10196-04-0
14307-43-8
3164-29-2
1762-95-4
7783-18-8
7803-55-6
628-63-7
123-92-2
626-38-0
625-16-1
62-53-3
120-12-7
7440-36-0
7647-18-9
28300-74-5
7789-61-9
10025-91-9
7783-56-4
1309-64-4
12674-11-2
11104-28-2
11141-16-5
53469-21-9
12672-29-6
11097-69-1
11096-82-5
7440-38-2
1327-52-2
7778-39-4
1303-32-8
1327-53-3
1303-28-2
1303-28-2
7784-34-1
1327-53-3
1303-33-9
692-42-2
1332-21-4
492-80-8
115-02-6
151-56-4
50-07-7
Polychlorinated Blphenyls
Polychlorinated Biphenyls
Polychlorinated Biphenyls
Polychlorinated Biphenyls
Polychlorlnated Biphenyls
Polychlorinated Biphenyls
Polychlorinated Biphenyls
Arsenic Trioxide
Arsenic Pentoxlde
Diethylarslne
Mltomycln C
i
A-15
A-16
A-17
A-18
A-338
A-339
A-19
A-22
A-23
A-24
A-340
A-25
A-26
A-27
A-341
A-344
A-345
A-346
A-347
A-350
A-28
A-29
A-30
A-31
A-32
A-33
A-34
A-832
A-832
A-832
A-832
A-832
A-832
A-832
A-35
A-37
A-38
A-41
A-39
A-39
A-40
A-41
A-42
A-104
A-43
A-351
A-352
A-353
A-760
oon r i mi
53
-------
Hazardous Substance
CAS No.
Consensual Name
Page
Barium Cyanide
Bent [ j ] aceanthrylene , 1 ,2-Dlhydro-
3-nethyl
Benz[c]acridine
3 , 4-Benzacr idine
Benzal Chloride
Benz [a]anthracene
1 ,2-Benzanthracene
1,2-Benanthracene, 7,12-Dimethyl-
Benzenanine
Benzenamine, 4,4'-CarboniBldoylbis-
(N.N-dimethyl-
Benzenamlne , 4-Chloro
Benzenamine, 4-Chloro-2-»ethyl-,
Hydrochlorlde
Benzenamine, N,N-Dlmethyl-4-phenylazo-
Benzenamlne, 4,4'-Methylenebi8(2-
chloro-
Benzenamlne, 2-Methyl-, Hydrochlorlde
Benzenamine, 2-Methyl-5-nitro-
Benzenamine, 4-Nitro-
Benzene
Benzeneacetlc Acid, 4-Chloro-alpha-
(4-chlorophenyl)-alpha-hydroxy-, Ethyl
Ester
Benzene , l-Bromo-4-phenoxy-
1,2-Benzenedlcarboxylic Acid Anhydride
1,2-Benzenedicarboxyllc Acld,[bis(2-
ethylhexyl)] Ester
1,2-Benzenedicarboxyllc Acid, Dl butyl
Ester
1,2-Benzenedicarboxylic Acid, Dlethyl
Ester
1,2-Benzenedicarboxylic Acid, Dimethyl
Ester
1,2-Benzenedicarboxyllc Acid, Di-n-
octyl Ester ~
Benzene, Chloro-
Benzene, Chloromethyl-
Benzene, 1,2-Dichloro-
Benzene, 1,3-Dlchloro-
Benzene, 1,4-Dlchloro-
Benzene , Dl chloromethy 1-
Benzene, 2,4-Dllsocyanatomethyl-
Benzene, Dimethyl
•-
o-
i~
1,3-Benzenedlol
1,2-Benzenedlol, 4-[l-hydroxy-2-
(methylamlno)ethyl]-
Benzene, Hexachloro-
Benzene, Bexahydro-
Benzene, Hydroxy-
542-62-1
56-49-5
225-51-4
225-51-4
98-87-3
56-55-3
56-55-3
57-97-6
62-53-3
492-80-8
106-47-8
3165-93-3
60-11-7
101-14-4
636-21-5
99-55-8
100-01-6
71-43-2
510-15-6
101-55-3
85-44-9
117-81-7
84-74-2
84-66-2
131-11-3
117-84-0
108-90-7
100-44-7
95-50-1
541-73-1
106-46-7
98-87-3
584-84-9
1330-20-7
108-38-3
95-47-6
106-42-3
108-46-3
51-43-3
118-74-1
110-82-7
108-95-2
3-Methylcholanthrene
Benz[c]acrldlne
Benzo [ a ] anthracene
Benzo [ a ] anthracene
7,12-Dimethylbenr[a]-
•nthracene
Aniline
Auramine
p-Chloroanlllne
4"-Chloro-o-toluldlne ,
Hydrochloride
Dlmethylamlnoazobenzene
4,4'-Methylenebls-
( 2-chloroani line )
o-Toluidine Hydrochloride
5-Nitro-o-Toluldine
p-Nltroanillne
Ethyl 4,4' -Dichlorobenz-
llate
4-Bromophenyl Phenyl Ether
Phthallc Anhydride
Bis ( 2-ethy Ihexy 1 )Phthalat e
Di-n-butyl Phthalate
Dlethyl Phthalate
Dimethyl Phthalate
Dl-ii-octyl Phthalate
Chlorobenzene
Benzyl Chloride
1,2-Dlchlorobenzene
1 , 3-D! chlorobenzene
1 ,4-Dl chlorobenzene
Benzal Chloride
Toluene Dilsocyanate
Xylene
•-Xylene
o-Xylene
£-Xylene
Resorclnol
Eplnephrlne
Hexachlorobenzene
Cyclohexane
Phenol
A-47
A-727
A-354
A-354
A-356
A-365
A-365
A-564
A-347
A-351
A-438
A-457
A-562
A-728
A-910
A-805
A-778
A-357
A-632
A-398
A-829
A-392
A-493
A-551
A-574
A-592
A-439
A-379
A-500
A-503
A-505
A-356
A-906
A-953
A-954
A-955
A-956
A-857
A-619
A-677
A-470
A-821
(continued)
54
-------
Hazardous Substance
CAS No.
Consensual Name
Page
Benzene, Methyl-
Benzene, l-Methyl-2,4-dlnitro-
Benzene, l-Methyl-2,6-dlnitro-
Benzene, l,2-Methylenedloxy-4-allyl-
Benzene, l,2-Methylenedioxy-4-
propenyl-
Benzene , 1 , 2-Methy lenedioxy-4-pr opy 1-
Benzene, 1-Methylethyl-
Benzene, Nitro-
Benzene, Pentachloro—
Benzene , Pentachloronltro-
Benzenesulfonic Acid Chloride
Benzenesulfonyl Chloride
Benzene, 1,2,4,5-Tetrachloro-
Benzenethlol
Benzene, 1,3,5-trinitro-
Benzldlne
1 , 2-Benzlsothlazolln~3-one ,1,1,-
dioxlde, and Salts
Benzo [ a ] anthracene
Benz o [ b ] f luor anthene
Benzo (k)fluoranthene
Benzo [ j ,k] f luorene
Benzole Acid
Benzonltrlle
Benzo [ ghl ] perylene
Benzo [a] pyretic
3 , 4-Benzopyrene
p-Benzoquinone
Benzotrichlorlde
Benzoyl Chloride
1 , 2-Benzphenanthrene
Benzyl Chloride
Beryllium
Beryllium Chloride
Beryllium Dust
Beryllium Fluoride
Beryllium Nitrate
o-BHC
6-BHC
Tf-BHC
6-BRC
2,2'-Bioxirane
( 1 , 1 ' -Blpheny l)-4 ,4 ' dlamlne
(l,l'-Biphenyl)-4,4'dlamine,
3,3'-dlchloro-
( 1 , 1 '-Blphenyl)-4 ,4 ' dlamlne
3,3'dlmethoxy-
(l,l'-Blphenyl)-4,4'diamlne
3,3'-dlmethyl-
Bls(2-chloroethoxy) Methane
Bis(2-chloroethyl) Ether
Bls(2-chlorolsopropyl) Ether
Bls(chloromethyl) Ether
108-88-3
121-14-2
606-20-2
94-59-7
120-58-1
94-58-6
98-82-8
98-95-3
608-93-5
82-68-8
98-09-9
98-09-9
95-94-3
108-98-5
99-35-4
92-87-5
81-07-2
56-55-3
205-99-2
207-08-9
206-44-0
65-85-0
100-47-0
191-24-2
50-32-8
50-32-8
106-51-4
98-07-7
98-88-4
218-01-9
100-44-7
7440-41-7
7787-47-5
7440-41-7
7787-49-7
13597-99-4
7787-55-5
319-84-6
319-85-7
58-89-9
319-86-8
1464-53-5
92-87-5
91-94-1
119-90-4
119-93-7
111-91-1
111-44-4
108-60-1
542-88-1
Toluene
2 ,4-Dinltrotoluene
2,6-Dlnltrotoluene
Safrole
Isosafrole
Dlhydrosafrole
Cumene
Nitrobenzene
Pentachlorobenzene
Pentachloronltrobenzene
Benzenesulfonyl Chloride
1,2,4, 5-Tetrachlorobenzene
Thlophenol
syjD-Trinitrobenzene
Saccharin and Salts
Fluoranthene
Benzo [ajpyrene
Chrysene
Beryllium
Llndane
1,2:3, 4-Dlepoxybutane
Benzldlne
3,3' -Dichlorobenzldlne
3,3'-Dlmethoxybenzldlne
3 , 3 '-Dlmethylbenzidlne
A-901
A-589
A-590
A-860
A-694
A-556
A-468
A-779
A-811
A-814
A-361
A-361
A-871
A-895
A-940
A-362
A-858
A-365
A-366
A-367
A-654
A-368
A-370
A-371
A-372
A-372
A-375
A-377
A-378
A-459
A-379
A-54
A-55
A-54
A-56
A-57
A-381
A-382
A-700
A-383
A-543
A-362
A-508
A-559
A-565
A-384
An p c
-385
A4 Q Q
-388
A-389
(continued)
55
-------
Hazardous Substance
CAS No.
Consensual Dane
Page
Bis(dlmethylthlocarbamoyl) Disulflde
Bis(2-Ethylhexyi)phthalate
Bromine Cyanide
Bromoacetone
Bromofom
4-Broaophenyl Phenyl Ether
Bruclne
1,3-Butadlene, 1,1,2,3,4,4,-
Bexachloro
1-Butanamlne , N-Butyl-N-nitroso-
Butanolc acid, 4-[bls(2-chloroethyl)-
amino] benzene-
1-Butanol
2-Butanone
2-Butanone Peroxide
2-Butenal
2-Butene, 1,4-Dichloro
Butyl Acetate
iso-Butyl Acetate
sec-Butyl Acetate
tert-Butyl Acetate
iso-Butyl Alcohol
n-Butyl Alcohol
Butylamine
JBo-Butylamlne
sec-Butylamine
tert-Butylamine
Butyl Benzyl Phthalate
n-Butyl Phthalate
Butyric Acid
Iso-Butyric Acid
Cacodylic Acid
Cadmium
Cadmium Acetate
Cadmium Bromide
Cadmium Chloride
Calcium Arsenate
Calcium Arsenlte
Calcium Carbide
Calcium Chromate
Calcium Cyanide
Calcium Dodecylbenzene Sulfonate
Calcium Hypochlorlte
Camphene, Octachloro-
Captan
Carbamlc Acid, Ethyl Ester
Carbamlc Acid, Methylnitroso-. Ethyl
Ester
Carbamide, N-Ethyl-N-nitroso-
Carbamide. N-Methyl-N-nltroso
Carbamide, Thlo-
Carbamlmidoselenolc Acid
137-26-8
117-81-7
506-68-3
598-31-2
75-25-2
101-55-3
357-57-3
87-68-3
924-16-3
305-03-3
71-36-3
78-93-3
1338-23-4
123-73-9
4170-30-3
764-41-0
123-86-4
110-19-0
105-46-4
540-88-5
78-83-1
71-36-3
109-73-9
78-81-9
513-49-5
13952-84-6
75-64-9
85-68-7
84-74-2
107-92-6
79-31-2
75-60-5
7440-43-9
543-90-8
7789-42-6
10108-64-2
7778-44-1
52740-16-6
75-20-7
13765-19-0
592-01-8
26264-06-2
7778-54-3
8001-35-2
133-06-2
51-79-6
615-53-2
759-73-9
684-93-5
62-56-6
630-10-4
Thlram
Cyanogen Bromide
Hexachlorobutadlene
N-Nltrosodl-n-butylamlne
Chlorambucil"
n-Butyl Alcohol
Methyl Ethyl Ketone
Methyl Ethyl Ketone
Peroxide
Crotonaldehyde
1 ,4-Dichloro-2-butene
Dl-n-butyl Phthalate
Toxaphene
Ethyl Carbamate (Drethan)
N-Nitroso-N-methylurethane
N-Nitroso-N-ethylurea
N-Nltroso-N-»ethylurea
Thlourea
Selenourea
A-899
A-392
A-98
A-394
A-396
A-398
A-399
A-678
A-790
A-434
A-407
A-736
A-739
A-467
A-511
A-400
A-401
A-402
A-404
A-405
A-407
A-410
A-413
A-414
A-415
A-416
A-493
A-417
A-418
A-58
A-59
A-61
A-62
A-63
A-64
A-65
A-66
A-67
A-68
A-69
A-70
A-911
A-419
A-631
A-799
A-797
A-798
A-897
A-217
(continued)
56
-------
Hazardous Substance
CAS No.
Consensual Name
Page
Carbamoyl Chloride. Dime thy 1-
Carbaryl
Carbofuran
Carbon Bisulfide
Carbon Bisulfide
Carbonic Acid, Dithalllum (I) Salt
Carbonochloridlc Acid, Methyl Ester
Carbon Oxyfluorlde
Carbon Tetrachlorlde
Carbonyl Chloride
Carbonyl Fluoride
Chloral
Chlorambucll
Chlordane
Chlordane , Technical
Chlorine
Chlorine Cyanide
Chlornaphazlne
Chloroacetaldehyde
£-Chloroaniline
Chlorobenzene
4-Chloro-tt-cresol
£-Chloro-«-cre8ol
Chlorodibromone thane
1-Chlor o-2 , 3-epoxypropane
Chloroethane
2-Chloroethyl Vinyl Ether
Chloroform
Chloromethyl Methyl Ether
6-Chloronaphthalene
2-Chloronaphthalene
2-Chlorophenol
o-Chlorophenol
4-Chlorophenyl Phenyl Ether
l-(o-Chlorophenyl)thiourea
3-Chloropropionitrile
Chlorosulfonic Acid
4-Chloro-o-toluidine Hydrochloride
Chlorpyri?os
Chromic Acetate
Chromic Acid
Chromic Acid, Calcium Salt
Chromic Sulfate
Chromium
Chromous Chloride
Chrysene
Cobaltous Bromide
Cobaltous Formate
Cobaltous Sulfamate
Copper
Copper Cyanides
Coumaphos
Creosote
Cresol(s)
•—Cresol
o-Cresol
£-Cresol
79-44-7
63-25-2
1563-66-2
75-15-0
75-15-0
6533-73-9
79-22-1
353-50-4
56-23-5
75-44-5
353-50-4
75-87-6
305-03-3
57-74-9
57-74-9
7782-50-5
506-77-4
494-03-1
107-20-0
106-47-8
108-90-7
59-50-7
59-50-7
124-48-1
106-89-8
75-00-3
110-75-8
67-66-3
107-30-2
91-58-7
91-58-7
95-57-8
95-57-8
7005-72-3
5344-82-1
542-76-7
7790-94-5
3165-93-3
2921-88-2
1066-30-4
11115-74-5
13765-19-0
10101-53-8
7440-47-3
10049-05-5
218-01-9
7789-43-7
544-18-3
14017-41-5
7440-50-8
544-92-3
56-72-4
8001-58-9
1319-77-3
108-39-4
95-48-7
106-44-5
Dlmethylcarbaaoyl Chloride
Carbon Bisulfide
Thallium (I) Carbonate
Methyl Chlorocarbonate
Carbonyl Fluoride
Phosgene
Chlordane
Cyanogen Chloride
£-Chloro-m-cresol
Eplchlorohydrin
2-Chloronaphthalene
2-Chlorophenol
Calcium Chromate
A-567
A-421
A-423
A-424
A-424
A-255
A-726
A-432
A-429
A-825
A-432
A-433
A-434
A-435
A-435
A-71
A-100
A-436
A-437
A-438
A-439
A-442
A-442
A-443
A-615
A-4A4
A-445
A-446
A-450
A-452
A-452
A-453
A-453
A-454
A-455
A-456
A-76
A-457
A-458
A-77
A-78
A-67
A-80
A-81
A-82
A-459
A-83
A-84
A-85
A-86
A-87
A-460
A-461
A-462
A-463
A-464
A-466
(continued)
57
-------
Hazardous Substance
CAS No.
Consensual Kane
Page
Cresyllc Acid
•-Cresyllc Acid
o-Cresylic Acid
£-Cresylic Acid
Crotonaldehyde
Cumene
Cuprlc Acetate
Cuprlc Acetoarsenlte
Cupric Chloride
Cupric Nitrate
Cuprlc Oxalate
Cuprlc Sulfate
Cuprlc Sulfate Auonlated
Cuprlc Tartrate
Cyanides (soluble cyanide salts),
not elsewhere specified.
Cyanogen
Cyanogen Bronlde
Cyanogen Chloride
1 ,4-Cyclohexadienedione
Cyclohexane
Cyclohexanone
1 , 3-Cy clopentadlene , 1,2,3,4,5,5-
Hexachloro-
Cyclophosphaolde
2,4-D Acid
Daunooycln
ODD
4, 4 '-ODD
DDE
4, 4 '-DDE
DDT
4, 4 'DDT
2,4-D Esters
Decachlorooctahydro-1 , 3 , 4-«etheno-2H-
cyclobuta [ c , d ] -pentalen-2-one
Dlallate
Dlamlne
Dlamlnotoluene
Dlazlnon
Dibenz [ a ,h ] anthracene
1,2:5, 6-Dlbenzanthracene
Dlbenzo[ a, h] anthracene
1,2:7, 8-Dlbenzopyr ene
Dibenz [ a , 1 ] pyr ene
1 , 2-Dlbr ono-3-chloropropane
1319-77-3
108-39-4
95-48-7
106-44-5
123-73-9
4170-30-3
98-82-8
142-71-2
12002-03-8
7447-39-4
3251-23-8
5893-66-3
7758-98-7
10380-29-7
815-82-7
57-12-5
460-19-5
506-68-3
506-77-4
106-51-4
110-82-7
108-94-1
77-47-4
50-18-0
94-75-7
20830-81-3
72-54-8
72-54-8
72-55-9
72-55-9
50-29-3
50-29-3
94-11-1
94-79-1
94-80-4
1320-18-9
1928-38-7
1928-61-6
1929-73-3
2971-38-2
25168-26-7
53467-11-1
143-50-0
2303-16-4
302-01-2
95-80-7
333-41-5
53-70-3
53-70-3
53-70-3
189-55-9
189-55-9
96-12-8
Cresol(s)
•-Cresol
o-Cresol
£-Cresol
p-Benzoqulnone
Hexachlorocyclopentadlene
ODD
DDE
DDT
Kepone
Hydrazlne
Toluenedlanine
Dibenz [ a, hj anthracene
Dibenz j a , h ] anthracene
Dibenz [a , 1 ] pyrene
A-462
A-463
A-464
A-466
A-467
A-468
A-88
A-89
A-90
A-91
A-92
A-93
A-94
A-95
A-96
A-97
A-98
A-100
A-375
A-470
A-473
A-679
A-475
A-476
A-478
A-479
A-479
A-480
A-480
A-481
A-481
A-483
A-696
A-484
A-117
A-904
A-486
A-488
A-488
A-488
A-489
A-489
A-490
58
(continued)
-------
Hazardous Substance
CAS No.
Consensual Name
Page
Dlbutyl Phthalate
Di-n-butyl Phthalate
Dlcamba
Dichlobenll
Dlchlone
S- ( 2 , 3-Dichloroal lyl ) Diisopropy 1-
thiocarbamate
Dichlorobenzene (mixed)
1 , 2-Dichlorobenrene
1 , 3-Dichloro benzene
1 ,4-Dichlorobenzene
B-Dlchlorobenzene
o-Dlchlorobenrene
§ "-Dichlorobenzene
, 3 ' -Dichlorobenzidine
Dichlorobromomethane
l,4-Dichloro-2-butene
Dichlorodif luoromethane
3 , 5-Dichloro-N- ( 1 , 1-dimethy 1-2-
propynyl)benzamide
Dichlorodiphenyl Dichloroethane
Dichlorodiphenyl Trichloroethane
1 , 1-Dichloroethane
1 , 2-Dichloroethane
1 , 1-Dichloroethylene
1 , 2-trans-Dichloroethylene
Dichloroethyl Ether
2 , 4-Dichlorophenol
2,6-Dichlorophenol
2,4-Dichlorophenoxyacetlc Acid,
Salts and Esters
Dichlorophenylarsine
Dichloropropane
1 , 2-Dichloropr opane
Dichloropropane - Dichloropropene
Mixture
Dichloropropene
1 , 3-Dichloropropene
2,2-Dichloropropionic Acid
Dichlorvos
Dieldrin
1,2:3, 4-Diepoxybutane
Dlethylamlne
Diethylarsine
1,4-Diethylene Dioxide
0,0-Diethyl-S-[2-(ethylthio)ethyl)]-
phosphorodithioate
N.N'-Diethylhydrazine
0,0-Diethyl S-Methyl Dithiophosphate
Diethyl-£-nitrophenyl Phosphate
Diethyl Phthalate
0,0-Diethyl 0-Pyrazlnyl Phosphoro-
thloate
Diethylstllbestrol
l,2-Dlhydro-3,6-pyridazinedione
84-74-2
84-74-2
1918-00-9
1194-65-6
117-80-6
2303-16-4
25321-22-6
95-50-1
541-73-1
106-46-7
541-73-1
95-50-1
106-46-7
91-94-1
75-27-4
764-41-0
75-71-8
23950-58-5
72-54-8
50-29-3
75-34-3
107-06-2
75-35-4
156-60-5
111-44-4
120-83-2
87-65-0
94-75-7
696-28-6
26638-19-7
78-87-5
8003-19-8
26952-23-8
542-75-6
75-99-0
62-73-7
60-57-1
1464-53-5
109-89-7
692-42-2
123-91-1
298-04-4
1615-80-1
3288-58-2
311-45-5
84-66-2
297-97-2
56-53-1
123-33-1
Dl-n-butyl Phthalate
Dial late
1 ,3-Dlchlorobenrene
1 , 2-Dichlorobenrene
1,4-Dlchlorobenzene
Pronamide
DDD
DDT
Bis(2-chloroethyl) Ether
2,4-D Acid
1,4-Dioxane
Disulfoton
Malelc Hydrazlde
A-493
A-493
A-495
A-496
A-498
A-484
A-499
A-500
A-503
A-505
A-503
A-500
A-505
A-508
A-510
A-511
A-512
A-835
A-479
A-481
A-515
A-518
A-521
A-524
A-385
A-527
A-528
A-476
A-103
A-529
A-530
A-534
A-535
A-536
A-537
A-539
A-541
A-543
A-544
A-104
A-593
A-600
A-547
Aft Q
-548
A-549
A-551
A-553
A-555
A-705
(continued)
59
-------
Hazardous Substance
CAS No.
Consensual Name
Page
Dlhydrosafrole
Dllsopropyl Fluorophosphate
Dlmethoate
3 , 3 '-Dlmethoxybenzidine
Dimethylaaine
Dlmethylamlnoazobenzene
7,12-DiBethylbenz[a]anthracene
3.3'-Dimethylbenzldlne
a ,o -Dlmethylbenzy Ihydroperoxlde
Dimethylcarbamoyl Chloride
1 , 1-Dlmethylhydrazlne
1 ,2-Dlmethylhydrazlne
3,3-Dlmethyl-l-(methylthlo)-2-
butanone , 0-[ (raethylamlno)carbonyl)
Oxlme
0,0-Dlmethyl 0-p_-Nitrophenylphos-
phorothioate
Dimethylnltrosamlne
a,o-Dlmethylphenethylamlne
2 , 4-Dlmethylphenol
Dimethyl Phthalate
Dimethyl Sulfate
Dinltrobenzene (mixed)
m-Dlnltrobenzene
o-Dlnltrobenzene
jr-Dinltrobenzene
4,6-Dinltro-o-cresol and Salts
4 ,6-Dinltro-o-cyclohexylphenol
Dlnltrophenol
2,4-Dlnltrophenol
2 , 5-Dlnl tropheno 1
2 , 6-Dlnl trophenol
Dlnltrotoluene
2 ,4-Dlnltrotoluene
2 , 6-Dlnl tro toluene
Dlnoseb
Dl-n-octyl Phthalate
1,4-Dioxane
1 ,2-Dlphenylhydrazlne
Dlphosphoramlde, Octamethyl-
Dlpropylamlne
Dl-n-propylnltrosamlne
Dlquat
Dlsulfoton
2,4-Dithlobluret
Dlthlopyrophosphorlc Acld.Tetraethyl
Ester
Dluron
Dodecylbenzenesulfonlc Acid
2,4-D Salts and Esters
Endosulfan
o-Endosulfan
6-Endosulfan
Endosulfan Sulfate
94-58-6
55-91-4
60-51-5
119-90-4
124-40-3
60-11-7
57-97-6
119-93-7
80-15-9
79-44-7
57-14-7
540-73-8
39196-18-4
298-00-0
62-75-9
122-09-8
105-67-9
131-11-3
77-78-1
25154-54-5
99-65-0
528-29-0
100-25-4
534-52-1
131-89-5
25550-58-7
51-28-5
329-71-5
573-56-8
25321-14-6
121-14-2
606-20-2
88-85-7
117-84-0
123-91-1
122-66-7
152-16-9
142-84-7
621-64-7
85-00-7
2764-72-9
298-04-4
541-53-7
3689-24-5
330-54-1
27176-87-0
94-75-7
115-29-7
959-98-9
33213-65-9
1031-07-8
Thlofanox
Methyl Farathlon
N-Nltrosodlmethylamlne
Octaoethylpyrophosphoramlde
N-Nitrosodl-n-propylamlne
Tetraethyldlthiopyro-
phosphate
2,4-D Acid
A-556
A-557
A-558
A-559
A-560
A-562
A-564
A-565
A-566
A-567
A-569
A-571
A-893
A-755
A-793
A-572
A-573
A-574
A-575
A-577
A-578
A-579
A-580
A-581
A-582
A-583
A-584
A-585
A-586
A-587
A-589
A-590
A-591
A-592
A-593
A-596
A-806
A-597
A-796
A-598
A-600
A-601
A-884
A-602
A-605
A-476
A-606
A-607
A-608
A-609
60
(continued)
-------
Hazardous Substance
CAS No.
Consensual Name
Page
Endothall
Endrin
Endrin Aldehyde
Epichlorohydrin
Eplnephrlne
Ethanal
Ethanamine, l,l-Dlmethyl-2-phenyl-
Ethanamlne, N-Ethyl-N-nltroso-
Echane, 1,2,-Dibromo-
Ethane, 1,1-Dlchloro-
Ethane , 1 , 2-Dlchloro-
Ethane, l,l'-[Methylenebis(oxy)]bls
[2-chloro-
Ethanenltrile
Ethane, l,l'-0xybis-
Ethane, l,l'-0xybls[2-chloro-
Ethane , Pentachloro-
Ethane, 1 ,1,1,2-Tetrachloro-
Ethane, 1,1,2,2-Tetrachloro-
Ethanethioaolde
Ethane, 1,1,2-Trichloro-
Ethane, l,l,l-Trichloro-2,2-bis-
(£-«ethoxyphenyl )
1 , 2-Ethanedly Ibiscarbamodithlolc Acid
Ethanol, 2,2'-(NitroBolmino)bis-
Ethanooe, 1-Phenyl-
Ethanoyl Chloride
Ethenamlne, N-Methyl-N-nltroso
Ethene, Chloro-
Ethene, 2-Chloroethoxy-
Ethene, 1,1-Dlchloro-
Ethene, 1,1,2,2-Tetrachloro-
Ethene , trans-1 , 2-Dichloro-
Ethlon
Ethyl Acetate
Ethyl Acrylate
Ethylbenrene
Ethyl Carbamate (Drethan)
Ethyl Cyanide
Ethyl 4.4'-Dichlorobenzllate
Ethylenebls(Dlthlocarbamic Acid)
Ethylened lamlne
Ethylenedlamlne Tetraacetlc Acid
(EDTA)
Ethylene Dlbroalde
Ethylene Dlchlorlde
Ethylene Oxide
Ethylenethlourea
Ethylenlmlne
Ethyl Ether
Ethylldene Dlchlorlde
Ethyl Methacrylate
Ethyl Methanesulfonate
145-73-3
72-20-8
7421-93-4
106-89-8
51-43-4
75-07-0
122-09-8
55-18-5
106-93-4
75-34-3
107-06-2
67-72-1
111-91-1
75-05-8
60-29-7
111-44-4
76-01-7
630-20-6
79-34-5
62-55-5
79-00-5
72-34-5
111-54-6
1116-54-7
98-86-2
75-36-5
4549-40-0
75-01-4
110-75-8
75-35-4
127-18-4
156-60-5
563-12-2
141-78-6
140-88-5
100-41-4
51-79-6
107-12-0
510-15-6
111-54-6
107-15-3
60-00-4
106-93-4
107-06-2
75-21-8
96-45-7
151-56-4
$0-29-7
75-34-3
97-68-2
62-50-0
Acetaldehyde
0,0 -Dime thy Iphenethy lamlne
N-Nltrosodlethylamlne
Ethylene Dlbromide
1 , 1-Dlchloroethane
1 , 2-Dlchloroethane
Hexachloroe thane
Bls(2-chloroethoxy) Methane
Acetonltrlle
Ethyl Ether
Bis (2-chloroethyl) Ether
Pentachloroethane
1,1,1, 2-Tetrachloroethane
1,1,2, 2-Tetrachloroethane
Thloacetamlde
1,1, 2-Trichloroethane
Methoxychlor
EthyleneblsCDlthlocarbamlc
Acid)
N-Nltrosodlethanolamlne
Acetophenone
Acetyl Chloride
N-Ni t roBomethylvinylamlne
Vinyl Chloride
2-Chloroethyl Vinyl Ether
1 , 1-Dlchloroethylene
Tetrachloroethylene
1 , 2-trans-Dichloroethylene
Propanenltrlle
1 , 2-Dlchloroethane
Azlrldlne
1 , 1-Dichloroethane
A-610
A-612
A-614
A-615
A-619
A-289
A-572
A-792
A-639
A-515
A-518
A-681
A-384
A-303
A-649
A-385
A-812
A-876
A-877
A-892
A-921
A-717
A-633
A-791
A-306
A-309
A-800
A-947
A-445
A-521
A-879
A-524
A-620
A-621
A-625
• too
A— O/o
A £11
-631
A-837
A-632
A-633
A-634
A-637
A-639
A-518
A-6A3
A-646
A-353
A-649
A-515
A-651
A-652
61
(continued)
-------
Hazardous Substance
CAS No.
Consensual Have
Page
Famphur
Ferric Ammonium Citrate
Ferric Ammonium Oxalate
Ferric Chloride
Ferric Dextran
Ferric Fluoride
Ferric Nitrate
Ferric Sulfate
Ferrous Ammonium Sulfate
Ferrous Chloride
Ferrous Sulfate
Fluoranthene
Fluorene
Fluorine
Fluoroacet amide
Fluoroacetlc Acid, Sodium Salt
Formaldehyde
Formic Acid
Fulmlnlc Acid, Mercury (II )Salt
Fumarlc Acid
Furan
2-Furancarboxaldehyde
-2 , 5-Furandlone
•Furan, Tetrahydro-
Furfural
Furfuran
D-Glucopyranose , 2-Deoxy-2(3-
methyl-3-nltrosoureldo)-
Glycldylaldehyde
Guanldine, N-Nitroso-N-nethyl-N'-
nitro-
Guthlon
Heptachlor
Heptachlor Epozide
Hexachlorobenzene
Hexachlorobutadlene
Bexachlorocyclohexane (gamma iaomers)
Bexachlorocyclopentadlene
l,2,3,4,10,10-Hexachloro-6,7-epoxy-
l,4,4a,5,6,7,8, 8a-oc tahydro-endo ,
endo-l,4:5,8-dlaethanonaphthalene
1 , 2 , 3 , 4 , 10 , 10-Hexachloro-6 , 7-epoxy-
l,4,4a,5,6,7,8, 8a-oc tahydro-endo , exo-
1 ,4:5,8-dlnethanonaphthalene
Hexachloroethane
Hexachlorohexahydro-endo,endo-
dioethanonaphthalene
l,2,3,4,10,10-Hexachloro-l,4,4a,5,
8 , 8a-hexahydro-l ,4,5, 8-endo , endo-
diaethanonaphthalene
l,2,3,4,10,10-Hexachloro-l,4,4a,5,
8 , 8a-hexahydro-l ,4:5, 8-endo , exo-
dlmethanonaphthalene
52-85-7
1185-57-5
2944-67-4
55488-87-4
7705-08-0
9004-66-4
7783-50-8
10421-48-4
10028-22-5
10045-89-3
7758-94-3
7720-78-7
7782-63-0
206-44-0
86-73-7
7782-41-4
640-19-7
62-74-8
50-00-0
64-18-6
628-86-4
110-17-8
110-00-9
98-01-1
108-31-6
109-99-9
98-01-1
110-00-9
18883-66-4
765-34-4
70-25-7
86-50-0
76-44-8
1024-57-3
118-74-1
87-68-3
58-89-9
77-47-4
72-20-8
60-57-1
67-72-1
465-73-6
465-73-6
309-00-2
'
Mercury Fulminate
Furfural
Maleic Anhydride
Tetrahydrofuran
Furan
Streptozotocin
N-Methyl-N'-nltro-N-nitroso-
guanldine
Llndane
Endrin
Dieldrln
Hexachlorohexahydro-endo ,
endo-dimethanonaphthalene
Aldrln
A-653
A-105
A-106
A-107
A-108
A-109
A-110
A-lll
A-112
A-113
A-114
A-654
A-655
A-115
A-656
A-657
A-658
A-665
A-162
A-668
A-669
A-690
A-705
A-887
A-670
A-669
A-861
A-673
A-754
A-674
A-675
A-676
A-677
A-678
A-700
A-679
A-612
A-541
A-681
A-683
A-683
A-324
62
(continued)
-------
Hazardous Substance
Hexachlorophene
Hexachloropropene
Hexaethyl Tecraphosphate
By d ratine
Hydrazinecarbothloamide
Hydrazine, 1,2-Dlethyl-
Hydrazine, 1,1-Dlnethyl-
Hydrazlne, 1,2-Dlmethyl-
Hydrazloe , 1 , 2-Diphenyl-
Hydrazine, Methyl-
Hydrochloric Acid
Hydrocyanic Acid
Hydrofluoric Acid
Hydrogen Cyanide
Hydrogen Fluoride
Hydrogen Phosphide
Hydrogen Sulfide
Hydroperoxide, 1-Methyl-l-phenyl-
ethyl-
Hydroxydinethylarsine Oxide
2-Imidazolidinethione
Indeno [1,2, 3-cd Jpyrene
Iron Dextran
Isobutyl Alcohol
Isocyanic Acid, Methyl Ester
•Isophorone
Isoprene
Isopropanolaffllne Docecylbenzene-
sulfonate
Isosafrole
3(2H)-Isoxazolone, 5-(Aminomethyl)-
Kelthane
Kepone
Laslocarpine
Lead
Lead Acetate
Lead Araenate
Lead Chloride
Lead Fluoborate
Lead Fluoride
Lead Iodide
Lead Nitrate
Lead Phosphate
Lead Stearate
Lead Subacetate
Lead Sulfate
Lead Sulfide
Lead Thiocyanate
Lindane
Lithium Chrooate
CAS No.
70-30-4
1888-71-7
757-56-4
302-01-2
79-19-6
1615-80-1
57-14-7
540-73-8
122-66-7
60-34-4
7647-01-0
74-90-8
7664-39-3
74-90-8
7664-39-3
78036-51-2
7783-06-4
80-15-9
75-60-5
96-45-7
193-39-5
9004-66-4
78-83-1
624-83-9
78-59-1
78-79-5
42504-46-1
120-58-1
2763-96-4
115-32-2
143-50-0
303-34-4
7439-92-1
301-04-2
7784-40-9
7645-25-2
10102-48-4
7758-95-4
13814-96-5
7783-46-2
10101-63-0
10099-74-8
7446-27-7
7428-48-0
1072-35-1
56189-09-4
1335-32-6
15739-80-7
7446-14-2
1314-87-0
592-87-0
58-89-9
14307-35-8
Consensual Nane
Thlosemicarbazlde
N.N'-Diethylhydrazine
1 , 1-Dlmethylhydrazine
1 , 2-Dimethy Ihydrar ine
1 , 2-Diphenylhydrazlne
Methyl Hydrazine
Hydrogen Cyanide
Hydrogen Fluoride
Phoephine
o, a-Dimethylbenzyl-
Hydroperoxlde
Cacodylic Acid
Ethylenethiourea
Ferric Dextran
iso-Butyl Alcohol
Methyl Isocyanate
5-(Aminomethyl)-3-lBoxazolol
Page
A-684
A-686
A-687
A-117
A-896
A-547
A-569
A-571
A-596
A-741
A-120
A-123
A-127
A-123
A-127
A-189
A-130
A-566
A-58
A-646
A-688
A-108
A-405
A-748
A-689
A-691
A-693
A-694
A-331
A-695
A-696
A-698
A-134
A-135
A-136
A-137
A-138
A-142
A-143
A-144
A-145
A-146
A-147
A-148
A-149
A-151
A- 7 00
A-152
(continued)
63
-------
Hazardous Substance
CAS No.
Consensual Name
Page
Malathion
Malelc Acid
Halelc Anhydride
Malelc Hydraiide
Malononicrile
Melphalan
Mercaptodlmethur
Mercuric Cyanide
Mercuric Nitrate
Mercuric Sulfate
Mercuric Thlocyanate
Mercurous Nitrate
Mercury
Mercury, (acetato-O)phenyl-
Mercury Fulminate
Methacrylonitrile
Methanamlne, N-Methyl-
Me thane, Bromo-
Me thane, Chloro-
Methane, Chloromethoxy-
Methane, Dlbromo-
Me thane , Dichlor o-
Me thane, Dichlorodlf luoro-
Me thane, lodo-
Methane, Oxybis(chloro-
Methanesulfenyl Chloride, Trlchloro
Methanesulfonic Acid, Ethyl Ester
Methane , Tetrachloro-
Methane, Tetranltro-
Methanethlol
Methane, Tribroao
Methane, Trlchloro-
Me thane, Trlchlorof luoro-
4,7-Methano-lH-indene,l,4,5,6,7,8,8-
Hepta£bJg£g£J|p4 ^Z^Ja-tetrahydr o-
Methanoic Acid
4,7-Methanolndan-l,2,4,5,6,7,8,8-
Octachloro-3a ,4,7, 7a-tetrahydro-
Methanol
Methapyrllene
Me thorny 1
Methoxychlor
Methyl Alcohol
2-Methylazlridlne
Methyl Bromide
1-Methylbutadlene
Methyl Chloride
Methyl Chlorocarbonate
Methyl Chloroform
3-Methylcholanthrene
4 , 4 '-Methylenebls ( 2-chloroanl line )
2,2' -Methylenbis ( 3,4, 6-trlchloro-
phenol)
121-75-5
110-16-7
108-31-6
123-33-1
109-77-3
148-82-3
2032-65-7
592-04-1
10045-94-0
7783-35-9
592-85-8
10415-75-5
7782-86-7
7439-97-6
62-38-4
628-86-4
126-98-7
124-40-3
74-83-9
74-87-3
107-30-2
74-95-3
75-09-2
75-71-8
74-88-4
542-88-1
594-42-3
62-50-0
56-23-5
509-14-8
74-93-1
75-25-2
67-66-3
75-69-4
76-44-8
64-18-6
57-74-9
67-56-1
91-80-5
16752-77-5
72-43-5
67-56-1
75-55-8
74-83-9
504-60-9
74-87T3
79-22-1
71-55-6
56-49-5
101-14-4
70-30-4
Propanedlnitrlle
Phenylmercurlc Acetate
Dlmethylamlne
Methyl Bromide
Methyl Chloride
Chloromethyl Methyl Ether
Methylene Bromide
Methylene Chloride
Dichlorodlf luoromethane
Methyl Iodide
Bis(chloromethyl) Ether
Trlchloromethanesulfenyl
Chloride
Ethyl Methanesulfonate
Carbon Tetrachlorlde
Tetranltromethane
Methylmercaptan
BroBoform
Chloroform
Trlchloromonof luoromethane
Heptachlor
Formic Acid
Chlordane
Methanol
1,3-Pentadiene
1,1, 1-Trlchloroethane
Hezachlorophene
A-702
A-704
A-705
A-706
A-836
A-708
A-709
A-154
A-155
A-156
A-157
A-158
A-159
A-188
A-162
A-710
A-560
A-719
A-723
A-450
A-730
A-732
A-512
A-743
A-389
A-928
A-652
A-429
A-890
A-749
A-396
A-446
A-929
A-675
A-665
A-435
A-712
A-715
A-716
A-717
A-712
A-718
-719
-818
-723
-726
-918
-727
-728
-684
(continued)
64
-------
Hazardous Substance
CAS No.
Consensual Name
Page
Methylene Bromide
Methylene Chloride
Methylene Oxide
Methyl Ethyl Ketone
Methyl Ethyl Ketone Peroxide
Methyl Hydrazlne
Methyl Iodide
Methyl Isobutyl Ketone
Methyl Isocyanate
2-Methyllactonltrile
Methylmercaptan
Methyl Methacrylate
N-Methyl-N'-nltro-N-nitrosoguanidine
Methyl Parathion
4-Methyl-2-pentanone
Methylthiouracll
Mevinphos
Mexacarbate
Mitomycin C
Monoethylamine
Monomethylamlne
Naled
5,12-Naphthacenedione, (8s-cis)-8-
acety 1-10- [ 3-amino-2 , 3 , 6-trldeoxy-
alpha-L-lyxo-hexopyranosyl )oxy 1-
7,8,9,10-tetrahydro-6,8,ll-
trihydroxy-1-methoxy-
Naphthalene
Naphthalene, 2-Chloro-
1 ,4-Naphthalenedlone
2,7-Naphthalenedisulfonic Acid, 3,3'-
[3,3'-dlmethyl-(l,l'-biphenyl)-4,4'-
diyl)-biB(azo)]bls(5-amino-4-
hydroxy) .Tetraeodium Salt
Naphthenlc Acid
1 ,4-Naphthoquinone
1-Naphtlfiylamine
2-Naphthylamlne
a-Naphthylamine
B-Naphthylamlne
2-Naphthylamine , N,N-bls(2-chloro-
ethyl)-
o-Naphthylthlourea
Nickel
Nickel Ammonium Sulfate
Nickel Carbonyl
Nickel Chloride
Nickel Cyanide
Nlckel(II) Cyanide
Nickel Hydroxide
Nickel Nitrate
Nickel Sulfate
Nickel Tetracarbonyl
Nicotine and Salts
74-95-3
75-09-2
50-00-0
78-93-3
1338-23-4
60-34-4
74-88-4
108-10-1
624-83-9
75-86-5
74-93-1
80-62-6
70-25-7
298-00-0
108-10-1
56-04-2
7786-34-7
315-18-4
50-07-7
75-04-7
74-89-5
300-76-5
20830-81-3
91-20-3
91-58-7
130-15-4
72-57-1
1338-24-5
130-15-4
134-32-7
91-59-8
134-32-7
91-59-8
494-03-1
86-88-4
7440-02-0
15699-18-0
13463-39-3
7718-54-9
37211-05-5
557-19-7
557-19-7
12054-48-7
14216-75-2
7786-81-4
13463-39-3
54-11-5
Formaldehyde
Acetone Cyanohydrin
Methyl Isobutyl Ketone
Daunomycln
2-Chloronaphthalene
1 ,4-Naphthoquinone
Trypan Blue
1-Naphthylamlne
2-Naphthylamine
Chlornaphazlne
Nickel Tetracarbonyl
Nickel Cyanide
A-730
A-732
A-658
A-736
A-739
A-741
A-743
A-745
A-748
A-301
A-749
A-751
A-754
A-755
A-745
A-756
A-757
A-759
A-760
A-761
A-763
A-765
A-478
A-766
A-452
A-770
A-942
A-769
A-770
A-771
A-772
A-771
A-772
A-436
A-773
A-163
A-164
A-170
A-165
A-166
A-166
AT AT
-167
A-168
A-169
A-170
A-775
(continued)
65
-------
Hazardous Substance
CAS Mo.
Consensual Name
Page
Nitric Acid
Nitric Oxide
D-Nitroanlline
Nitrobenzene
Nitrogen Dioxide
Nltrogen(II) Oxide
Nitrogen (IV) Oxide
Nitroglycerine
Nltrophenol (Mixed)
•-Ni 1 rophenol
o-Nitrophenol
£-Ni t r opheno 1
2-Nitrophenol
3-Nltrophenol
4-Ni tr ophenol
2-Nitropropane
N-Nltrosodi-n-butylamlne
N-Nltrosodiethanolamlne
N-Nitrosodlethylamlne
N-Nitrosodimethylamine
N-Nitrosodiphenylamlne
N-NitroBodi-n-propylamine
N-Nitroso-N-e"thylurea
N-Nltroso-N-methylurea
N-Nitroso-N-methylure thane
-N-Nltrosomethylvinylamlne
N-Nitrosopiperldine
N-Nltrosopyrrolldine
Nitro toluene
5-Nitro-o-Toluidine
5-Norbornene-2,3-dimethanol,l,4,5,
6>7,7-hexachloro,Cyclic Sulflte
Octane thy Ipyrophosphoraaide
Osmium Oxide
Osmium Tetroxlde
7-Oxablcyclo[2.2.1]heptane-2.3-
dlcarboxyllc Acid
1,2-Oxathiolane, 2,2-Dloxlde
2H-1 , 3 , 2-Oxazaphosphorlne , 2- [bis (2-
chloroethyl ) ami no ] tetrahydro-2-
oxlde
Oxirane
Oxlrane, 2-(Chloromethyl)-
Paraformaldehyde
Paraldehyde
Parathlon
Pentachlorobenzene
Pentachloroethane
Pentachloronltrobenzene
Pentachlorophenol
1,3-Pentadlene
Phenacetln
Phenanthrene
Phenol
Phenol , 2-Chloro-
7697-37-2
10102-43-9
100-01-6
98-95-3
10102-44-0
10102-43-9
10102-44-0
55-63-0
25154-55-6
554-84-7
88-75-5
100-02-7
88-75-5
554-84-7
100-02-7
79-46-9
924-16-3
1116-54-7
55-18-5
62-75-9
86-30-6
621-64-7
759-73-9
684-93-5
615-53-2
4549-40-0
100-75-4
930-55-2
1321-12-6
99-55-8
115-29-7
152-16-9
20816-12-0
20816-12-0
145-73-3
1120-71-4
50-18-0
75-21-8
106-89-8
30525-89-4
123-63-7
56-38-2
608-93-5
76-01-7
82-68-8
87-86-5
504-60-9
62-44-2
85-01-8
108-95-2
95-57x8
Nitric Oxide
Nitrogen Dioxide
3-Nitrophenol
2-Nltrophenol
4-Nltrophenol
Endosulfan
Osmium Tetroxlde
Endothall
1,3-Propane Sultone
Cyclophosphamide
Ethylene Oxide
Eplchlorohydrin
2-Chlorophenol
A-173
A-177
A-778
A-779
A-180
A-177
A-180
A-781
A-783
A-785
A-784
A-786
A-784
A-785
A-786
A-787
A-790
A-791
A-792
A-793
A-795
A-796
A-797
A-798
A-799
A-eoo
A-801
A-802
A-803
A-805
A-606
A-806
A-185
A-185
A-610
A-838
A-475
A-643
A-615
A-807
A-808
A-809
A-811
A-812
A-814
A-815
A-818
A-819
A-820
A-B21
A-453
66
(continued)
-------
Hazardous Substance
CAS No.
Consensual Name
Page
Phenol, 4-Chloro-3-«ethyl- 59-50-7
Phenol, 2-Cyclohexyl-4,6-dinitro- 131-89-5
Phenol, 2,4-Dichloro- 120-83-2
Phenol, 2,6,-Chloro- 87-65-0
Phenol, 2,4-Dimethyl- 105-67-9
Phenol, 2,4-Dinltro- 51-28-5
Phenol, 2,4-Dlnitro-6-(l-»ethyl- 88-85-7
propyl)-
Phenol, 2,4-Dinltro-6-methyl-, 534-52-1
and Salts
Phenol, 4-Nltro- 100-02-7
Phenol, Pentachloro- 87-86-5
Phenol, 2,3,4,6-Tetrachloro- 58-90-2
Phenol, 2,4,5-Trichloro- 95-95-4
Phenol, 2,4,6-Trichloro 88-06-2
Phenol, 2,4,6-Trtnltro-, Ammonium 131-74-8
Salt
Phenyl Dichloroarslne 696-28-6
1,10-(1,2-Phenylene)pyrene 193-39-5
Fhenylmercurlc Acetate 62-38-4
N-Phenylthiourea 103-85-5
Phorate 298-02-2
Phosgene 75-44-5
Phosphine 7803-51-2
-Phosphoric Acid 7664-38-2
Phosphoric Acid, Diethyl 311-45-5
p-nitrophenyl Ester
Phosphoric Acid, Lead Salt 7446-27-7
Phosphorodlthloic Acid, 0,0-Diethyl 3288-58-2
S-Methyl Ester
Phosphorodithioic Acid, 0,0-Diethyl-S 298-02-2
(ethylthio)Methyl Ester
Phosphorodithioic Acid, 0,0-Diethyl 60-51-5
S-l2(methylamino)-2-oxoethyl] Ester
Phosphorofluoridic Acid, bis(l-»ethyl- 55-91-4
ethyl) Ester
Phosphorothloic Acid, 0,0-Diethyl 56-38-2
0-(p-nitrophenyl) Ester
Phosphorothoic Acid, 0,0-Diethyl 297-97-2
0-pyrazlnyl Ester
Phosphorothioic Acid, 0,0-Dimethyl 52-85-7
0-[£-(dl»ethylamino)-«ulfonyl)
phenyl] Ester
Phosphorus 7723-14-0
Phosphorus Oxychlorlde 10025-87-3
Phosphorus Pentasulfide 1314-80-3
Phosphorus Sulfide 1314-80-3
Phosphorus Trichloride 7719-12-2
Phthallc Anhydride 85-44-9"
2-Plcoline 109-06-8
Plumbane, Tetraethyl- 78-00-2
POLYCHLORINATED BIPHENYLS (PCB's) 1336-36-3
Potassium Arsenate 7784-41-0
Potassium Arsenlte 10124-50-2
£-Chloro-*-cresol
4,6-Dinltro-o-cyclohexyl-
phenol
2,4-Dichlorophenol
2,6-Dlchlorophenol
2,4-DinethyIphenol
2,4-Dinitrophenol
Dinoseb
4,6-Dlnltro-o-cresol and
Salts
4-Nitrophenol
Pentachlorophenol
2,3,4,6-Tetrachlorophenol
2,4,5-Trichlorophenol
2,4,6-Trichlorophenol
Ammonium Plcrate
Dlchlorophenylarslne
Indeno(1,2,3-cd)pyrene
Dlethyl-p_-Nitrophenyl
Phosphate
Lead Phosphate
0,0-Diethyl S-Methyl
Dlthiophosphate
Phorate
Dinethoate
Dlisopropyl Fluorophosphate
Parathlon
0,0-Diethyl 0-Pyrazinyl
Phosphorothioate
Famphur
Phosphorus Pentasulfide
Tetraethyl Lead
A-442
A-582
A-527
A-528
A-573
A-584
A-591
A-581
A-786
A-815
A-883
A-932
A-933
A-339
A-103
A-688
A-188
A-823
A-824
A-825
A-189
A-192
A-549
A-145
A-548
A-824
A-558
A-557
A-809
A-553
A-653
A-194
A-196
A-197
A-197
A-199
A-829
A-831
A-250
A-832
A-200
A-201
(continued)
67
-------
Hazardous Substance
CAS No.
Consensual Name
Page
Potassium Bichromate
Potassium Chromate
Potassium Cyanide
Potassium Dlchromate
Potassium Hydroxide
Potassium Permanganate
Potassium Silver Cyanide
Pronamlde
1-Propanal, 2,3-Epoxy-
Propanal , 2-Methyl-2-(methylthlo)-
0-((methylamlno) carbonyljoxime
1-Propanamlne
1-Propanamlne, N-Propyl-
Propane, l,2-Dibromo-3-chloro
Propanedlnltrlle
Propanenltrile
Propanenitrlle, 3-Chloro-
Propanenitrlle , 2-Hydroxy-2-methyl-
Propane, 2,2'-Oxybls[2-chloro-
Propane , 2-Nitro-
1,3-Propane Sultone
1,2,3-Fropanetrlol, Trlnltrate
1-Propanol, 2,3-Dlbromo-, Phosphate
(3:1)
1-Propanol, 2-Methyl-
2-Propaaone
2-Propanone , 1-Bromo-
Proparglte
Propargyl Alcohol
2-Propenal
2-Propenaolde
Propene, 1 , 3-Dlchloro-
1-Propene , 1,1,2,3,3, 3-Hexachloro-
2-Propenenltrlle
2-Propenenltrlle, 2-Methyl-
2-Propenoic Acid
2-Propenolc Acl*; Ethyl Ester
2-Propenolc Acid, 2-Methyl-, Ethyl
Ester
2-Propenolc Acid, 2-Methyl-, Methyl
Ester
2-Propen-l-ol
Proplonlc Acid
Proplonlc Acid, 2-(2,4,5-Trlchloro-
phenoxy)-
Proplonlc Anhydride
n-Propylamlne
Propylene Bichloride
Propylene Oxide
1 , 2-Propy lenimine
2-Propyn-l-ol
Pyrene
Pyrethrlns
4-Pyrldlnamlne
7778-50-9
7789-00-6
151-50-8
7778-50-9
1310-58-3
7722-64-7
506-61-6
23950-58-5
765-34-4
116-06-3
107-10-8
142-84-7
96-12-8
109-77-3
107-12-0
542-76-7
75-86-5
108-60-1
79-46-9
1120-71-4
55-63-0
126-72-7
78-83-1
67-64-1
598-31-2
2312-35-8
107-91-7
107-02-8
79-06-1
542-75-6
1888-71-7
107-13-1
126-98-7
79-10-7
140-88-5
97-63-2
80-62-6
107-18-6
79-09-4
93-72-1
123-62-6
107-10-8
78-87-5
75-56-9
75-55-8
107-19-7
129-00-0
121-29-9
121-21-1
504-24-5
Potassium Dlchromate
Glycldylaldehyde
Aldlcarb
n-Propylamlne
Dlpropylamlne
l,2-Dlbromo-3-chloropropane
3-Chloroproplonltrlle
Acetone Cyanohydrln
A-204
A-202
A-203
A-204
A-205
A-206
A-212
A-835
A-673
A-323
A-842
A-597
A-490
A-836
A-837
A-456
A-301
Bls(2-chloroisopropyl) Ether A-388
2-Nltropropane
Nitroglycerine
Trls(2,3-dlbromopropyl)
Phosphate
Iso-Butyl Alcohol
Acetone
Bromoacetone
2-Propyn-l-ol
Acroleln
Acrylamlde
1 , 3-Dlchloropropene
Hexachloropropene
Acrylonltrile
Methacrylonltrlle
Acrylic Acid
Ethyl Acrylate
Ethyl Methacrylate
Methyl Methacrylate
Allyl Alcohol
2,4.5-TP Acid
1 ,2-Dlchloropropane
2-Methylazlrldlne
4-Ami nopyrldlne
A-787
A-838
A-781
A-941
A-405
A-298
A-394
A-839
A-846
A-311
A-315
A-536
A-686
A-318
A-710
A-316
A-625
A-651
A-751
A-326
A-840
A-914
A-841
A-842
A-530
A-843
A-718
A-846
A-847
A-B48
A-332
(continued)
68
-------
Hazardous Substance
CAS No.
Consensual Name
Page
Pyridlne
Pyrldine, 2-[ (2-Dlmethylamino-
ethy 1 )-2-thenylamino J
Pyridlne, Hexahydro-N-nitroso-
Pyridine, 2-Methyl-
Pyrldine, (S)-3-(l-Methyl-2-
pyrrolidinyl)- and Salts
4(lH)-Pyrimidlnone, 2,3-Dihydro-6-
•ethyl-2-thioxo-
Pyrophosphorlc Acid, Tetraethyl Ester
Pyrrole, Tetrahydro-N-nitroso-
Quinoline
Reserpine
Resorcinol
Saccharin and Salts
Safrole
Selenlous Acid
Selenium
Selenium Dioxide
Selenium Dlsulfide
Selenium Oxide
Selenourea
L-Serine, Dlazoacetate (ester)
Silver
Silver Cyanide
-Silver Nitrate
Silvex
Sodium
Sodium Arsenate
Sodium Arsenite
Sodium Azide
Sodium Bichromate
Sodium Bifluorlde
Sodium Bisulfite
Sodium Chronate
Sodium Cyanide
Sodium Dichromate
Sodium Dodecylbenzene Sulfonate
Sodium Fluoride
Sodium Hydrosulfide
Sodium Hydroxide
Sodium Hypochlorite
Sodium Methylate
Sodium Nitrite
Sodium Phosphate. Dibasic
Sodium Phosphate, Tribaslc
110-86-1
91-80-5
100-75-4
109-06-8
54-11-5
56-0402
107-49-3
930-55-2
91-22-5
50-55-5
108-46-3
81-07-2
94-59-7
7783-00-8
7782-49-2
7446-08-4
7488-56-4
7446-08-4
630-10-4
115-02-6
7440-22-4
506-64-9
7761-88-8
93-72-1
7440-23-5
7631-89-2
7784-46-5
26628-22-8
10588-01-9
1333-83-1
7631-90-5
7775-11-3
143-33-9
10588-01-9
25155-30-0
7681-49-4
16721-80-5
1310-73-2
7681-52-9
10022-70-5
124-41-4
7632-00-0
7558-79-4
10039-32-4
10028-24-7
10140-65-5
7601-54-9
7785-84-4
10101-89-0
10361-89-4
7758-29-^4
10124-56-8
Methapyrilene
N-Nitrosoplperldlne
2-Picollne
Nicotine and Salts
Methylthiouracll
Tetraethyl Pyrophosphate
N-Nltrosopyrrolldine
Selenium Dioxide
Azaserlne
2,4,5-TP Acid
Sodium Dichromate
A-850
A-715
A-801
A-831
A-775
A-756
A-885
A-802
A-854
A-856
A-857
A-858
A-860
A-213
A-214
A-215
A-216
A-215
A-217
A-352
A-218
A-219
A-220
A-914
A-221
A-222
A-223
A-224
A-230
A-226
A-227
A-228
A-229
A-230
A-231
A-232
A-233
A-234
A-236
A-237
A-238
A-239
A-240
(continued)
69
-------
EUtardoue Substance
Sodium Selenlte
4,4'-Stilbenediol, a.o-Dlethyl
Streptototocln
Strontiua Chr ornate
Strontium Sulfide
Strychnldln-10-one. and Salts
Strychnldln-10-one , 2 , 3-Dlmethoxy-
Strychnine and Salts
Styrene
Sulfurlc Acid
Sulfuric Acid, Dimethyl Ester
Sulfur Hydride
Sulfur Monochlorlde
Sulfur Phosphide
Sulfur Selenlde
Sulfuric Acid, Thalllum(I) Salt
2,4,5-T
2,4, 5-T Acid
2,4,5-T Amines
2, 4, 5-T Esters ^5-
TDE
1,2,4, S-Tetrachlorobenzene
2,3,7, 8-Tetrachlorodibenzo-
£-dioxin(TCDD)
1,1,1, 2-Tet rachloroethane
1,1,2, 2-Tetrachloroethane
Tetrachloroethylene
2,3,4, 6-Tetrachlorophenol
Tetraethyldlthlopyrophosphate
Tetraethyl Lead
Tetraethyl Pyrophosphate
Tetrahydrofuran
Tetranltrome thane
Tetraphosphoric Acid, Hezaethyl Ester
Thalllc Oxide
Thallium
Thallium(I) Acetate
Thalllum(I) Carbonate
Thalllum(I) Chloride
Thalllum(I) Nitrate
Thallium(III) Oxide
Thalllum(l) Selenlde
Thalllum(I) Sulfate
Thloacetamide
Thiofanox
Thlolmldodicarbonlc Dlamlde
Thlooethanol
Thlophenol
Thlosemlcarbazlde
Thlourea
CAS No.
10102-18-8
7782-82-3
56-53-1
18883-66-4
7789-06-2
1314-96-1
57-24-9
357-57-3
57-24-9
100-42-5
7664-93-9
77-78-1
7783-06-4
12771-08-3
1314-80-3
7488-56-4
7446-18-6
93-76-5
93-76-5
2008-46-0
93-79-8
2545-59-7
61792-07-2
1928-47-8
25168-15-4
72-54-8
95-94-3
1746-01-6
630-20-6
79-34-5
127-18-4
58-90-2
3689-24-5
78-00-2
107-49-3
109-99-9
509-14-8
757-58-4
1314-32-5
7440-28-0
563-68-8
6533-73-9
7791-12-0
10102-45-1
1314-32-5
12039-52-0
7446-18-6
62-55-5
39196-18-4
541-53-7
74-93-1
108-98-5
79-19-6
62-56-6
Consensual Name
Diethylstllbestrol
Strychnine and Salts
Bruclne
Dimethyl Sulfate
Hydrogen Sulfide
Phosphorus Pentasulfide
Selenium Disulflde
Thallium(I) Sulfate
2,4,5-T Acid
ODD
Hexaethyl Tetraphosphate
Thallic Oxide
2,4-Dlthlobluret
Methylmercaptan
Page
A-241
A-555
A-861
A-242
A-243
A-862
A-399
A-862
A-863
A-244
A-575
A-130
A-248
A-197
A-216
A-259
A-867
A-867
A-869
A-870
A-479
A-871
A-872
A-876
A-877
-879
-883
-884
-250
-885
-887
-890
-687
-252
-253
-254
A-255
A-256
A-257
A-252
A-258
A-259
A-892
A-893
A-601
A-749
A-895
A-896
A-897
(continued)
70
-------
Hazardous Substance
CAS No.
Consensual Naae
Page
Thlourea, (2-Chlorophenyl)-
Thiourea , 1-Naphthalenyl-
Thiourea, Phenyl-
Thiram
Toluene
Toluenediamlne
Toluene Dlisocyanate
o-Toluidlne Hydrochloride
Toxaphene
2.4,5-TP Acid
2,4,5-TP Acid Esters
1H-1 ,2,4-Triazol-3-anlne
Trichlorfon
1,2, 4-Trichlorobenr ene
1,1, 1-Trichloroethane
1,1, 2-Trichlorethane
Trichloroethene
Trichloroethylene
Trichloromethanesulfonyl Chloride
Trichloromonofluorome thane
Trichlorophenol
2,4, 5-Trichlorophenol
2,4, 6-Tr ichlorophenol
2,4,5-Trichlorophenoxyacetlc Acid
Trlethanolamine Dodecylbenzene
Sulfonate
Triethylamine
Trimethylamine
sya-Tr Initrobenzene
1,3,5-Trioxane, 2,4,6-Trimethyl-
Tris(2,3-dlbromopropyl) Phosphate
Trypan Blue
2,4,5-T Salts
Dracil, 5-[bis(2-chloroethyl)aainol-
Uracil Mustard
Uranyl Acetate
Uranyl Nitrate
Vanadlc Acid, Aomonium Salt
Vanadlua(V) Oxide
Vanadium Pentoxlde
Vanadyl Sulfate
Vinyl Acetate
Vinyl Chloride
Vinylldene Chloride
Warfarin
Xylene
•-Xylene
o-Xylene
p_-Xylene
Xylenol
Yohlmban-16-carboxyllc Acid, 11,17-
Dimethoxy-18- [(3,4, 5-trimethoxy-
benzoyl)oxy]-»ethyl Ester
Zinc
5344-82-1
86-88-4
103-85-5
137-26-8
108-88-3
95-80-7
584-84-9
636-21-5
8001-35-2
93-72-1
32534-95-5
61-82-5
52-68-6
120-82-1
71-55-6
79-00-5
79-01-6
79-01-6
594-42-3
75-69-4
25167-82-2
95-95-4
88-06-2
93-76-5
27323-41-7
121-44-8
75-50-3
99-35-4
123-63-7
126-72-7
72-57-1
13560-99-1
66-75-1
66-75-1
541-09-3
10102-06-4
36478-76-9
7803-55-6
1314-62-1
1314-62-1
27774-13-6
108-05-4
75-01-4
75-34-5
81-81-2
1330-20-7
108-38-3
95-47-6
106-42-3
1300-71-6
50-55-5
7440-66-6
l-( o-Chloropheny 1 ) thlourea
a-Naphthylthiourea
N-Phenylthlourea
Anltrole
Trichloroethylene
2,4,5-T Acid
Paraldehyde
Dracil Mustard
Ammonium Vanadate
Vanadium Pentoxide
1 , 1-Dichloroethylene
Reserplne
A-455
A-773
A-823
A-899
A-901
A-904
A-906
A-910
A-911
A-914
A-915
A-333
A-916
A-917
A-918
A-921
A-924
A-924
A-928
A-929
A-931
A-932
A-933
A-867
A-934
A-935
A-937
A-940
A-808
A-941
A-942
A-943
A-944
» A/ /
A— 94*
A-260
A-261
A-27
A-262
A-262
A-264
A-945
A-947
A-521
A-951
A-953
A-954
A-955
A-956
A-957
A-856
A-265
(contined)
71
-------
Hazardous Substance
CAS No.
Consensual Nane
Page
Zinc Acetate
Zinc Ammonium Chloride
Zinc Borate
Zinc Bromide
Zinc Carbonate
Zinc Chloride
Zinc Cyanide
Zinc Fluoride
Zinc Formate
Zinc Hydrosulfite
Zinc Nitrate
Zinc Phenolsulfonate
Zinc Phosphide
Zinc Sllicofluoride
Zinc Sulfate
Zirconium Nitrate
Zirconium Potassium Fluoride
Zirconium Sulfate
Zirconium Tetrachloride
557-34-6
52628-25-8
14639-97-5
14639-98-6
1332-07-6
7699-45-8
3486-35-9
7646-85-7
557-21-1
7783-49-5
557-41-5
7779-86-4
7779-88-6
127-88-2
1314-84-7
16871-71-9
7733-02-0
1374-89-9
16923-95-8
14644-61-2
10026-11-6
A-266
A-267
A-268
A-269
A-270
A-271
A-272
A-273
A-274
A-275
A-276
A-277
A-278
A-280
A-281
A-282
A-283
A-284
A-285
72
-------
Appendix A
Analytical Methods Available
A-l
-------
Part I: Inorganic Compounds
A-2
-------
ALUMINUM PHOSPHIDE (CAS Number 20859-73-8)
RQ: 45.4 kg
SAFETY INFORMATION; Liberates phosphine on contact with water- Toxic (inhala-
tion). Flammable.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Aluminum," Appendix B.
Air Samples
Laboratory Method
See "Aluminum," Appendix B.
See "Phosphorus," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Aluminum," Appendix B.
See "Phosphorus," Appendix B.
Water Samples
Laboratory Method
See "Aluminum," Appendix B.
See "Phosphorus," Appendix B,
A-3
-------
ALUMINUM SULFATE (CAS Number 10043-01-3)
RQ: 2270 kg
SAFETY INFORMATION:
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Aluminum," Appendix B.
See "Fluorides and Other Compounds," Appendix B.
Air Samples
Laboratory Method
See "Aluminum," Appendix B.
See "Nitrates and Sulfates," Appendix B.
See "Sulfates (Particulate)." Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Aluminum," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Aluminum," Appendix B.
See "Sulfates," Appendix B.
A-4
-------
AMMONIA (CAS Number 7664-41-7)
RQ: 45.4 kg
SAFETY INFORMATION; Toxic gas.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
METHOD SUMMARY;
Analysis for ammonia in air may be performed by use of a detector tube. A
0.1 to 1 liter sample is collected and analyzed with a hand-operated bellows
pump (Bendix/Gastec®, Draeger®, or equivalent) and an ammonia gas-detector tube
(Bendix/Gastec® No. 3H, 3M, or 3L, Draeger® No. CH20501, 25501, or 31901, or
equivalent). A positive result is indicated by a change in color in the tube
(purple to yellow, purple to yellow, pink to yellow, orange to dark blue,
yellow to grey, or yellow to violet, respectively). The color change is from
an acid-base reaction and an acid-base indicator in all cases but one (Draeger®
CH25501) where formation of the millon base nitrate produces the grey color.
INTERFERENCES;
Aliphatic amines produce positive results, but with lower sensitivity.
Hydrazines react with the same sensitivity as ammonia.
QUALITY CONTROL;
No quality control procedures are given.
SENSITIVITY;
This method is sensitive to concentration levels of ammonia of approxi-
mately 200 to 200,000 milligrams per cubic meter (3H and CH31901), 1 to 100
milligrams per cubic meter (3M and CH 25501), and 0.1 to 4 milligrams per cubic
meter (3L and CH 20501) with the above sample sizes in the absence of interfer-
ences .
REFERENCES;
National Draeger, Inc., Detector Tube Handbook, 4th ed.; K. Leichnitz, Ed.;
National Draeger, Inc.: Pittsburgh, 1979, pp. 35-37.
Bendix Corporation, Bendix Gastec Precision Gas Detector System Manual, Blue
Book; Bendix Corporation: Largo, Florida, no date, pp. 21-23.
A-5
-------
COST INFORMATION;
Cost per sample for analysis by this method is approximately $13-20
(list).
See also; "Hydrazines and Other Compounds," Appendix B.
See also: "Organic Vapors," Appendix B.
See also; "Volatile Species," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
Air Samples
Laboratory Method 1
METHOD SUMMARY:
Ammonia in air samples may be measured colorimetrically. The ammonia is
collected from a known volume of air in a midget impinger containing dilute
sulfuric acid. Nessler reagent is added to produce a yellow-brown complex,
which is measured at 440 nm on a spectrophotometer.
INTERFERENCES;
Ammonium salts will react with the reagent to give a false high reading,
but filtration of the air before its passage into the impinger will remove
them.
QUALITY CONTROL:
A blank should be processed with the samples.
EPA/TECHNICAL STATUS;
This method is classified as tentative by the National Institute of
Occupational Safety and Health (NIOSH) for use over the range of 14 to 94
milligrams per cubic meter of air with a 10-liter sample. Precision and
accuracy information is not furnished. The method is applicable to concentra-
tion of 10 to 80 milligrams of ammonia per cubic meter according to the APHA.
REFERENCES;
U.S. Department of Health, Education and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 205; Publication No. 77-157-A, U.S.
DHEW:Cincinnati, 1977.
A-6
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American Public Health Association Methods of Air Sampling and Analyses, 2nd ed,
Method 801; APHA: Washington 1977.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $25-30
(list), plus sampling costs.
See also: "Ammonia," Appendix B.
Air Samples
Laboratory Method 2
METHOD SUMMARY;
Infrared absorption spectrometry can be used to determine the concentra-
tion of ammonia in air samples. The absorbance at 10770 nm (929 cm"~l) is
measured, using a 10-meter path length cell. Air can be sampled in a Saran® or
Mylar® plastic bag and approximately 5 liters of the sample drawn into an
evacuated cell. Continuous monitoring of air flowing through the cell is
possible if the spectrometer is set to one particular wavelength. Some vapors
can be adsorbed on silica gel and quantitatively desorbed into the absorption
cell later. Tentative qualitative identification of compounds can be made
based on a full infrared absorption spectrum.
INTERFERENCES;
Compounds present in the sample which absorb infrared radiation at the
wavelength of interest will interfere.
QUALITY CONTROL;
No quality control procedures are given.
EPA/TECHNICAL STATUS;
This method is not EPA-approved. The sensitivity of the method, using
a 10-meter path-length cell, is 17 milligrams per cubic meter. No precision
or accuracy information is furnished.
REFERENCE;
American Public Health Association "Infrared Absorption Spectroscopy" In
Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington,
B.C., 1977, pp. 79-84.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $75-85
(list).
A-7
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Note: NIOSH Method S347 (ion specific electrode analysis) is applicable.
(Reference provided by reviewer.)
See also; "Ammonia," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
Water Samples
Laboratory Method
See "Ammonia," Appendix B.
A-8
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AMMONIUM BICARBONATE (CAS Number 1066-33-7)
RQ: 2270 kg
SAFETY INFORMATION:
Air Samples
Field Method
Soil/Sediment
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Ammonia," Appendix B.
A-9
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AMMONIUM BIFLUORIDE (CAS Number 1341-49-7)
RQ: 2270 kg
SAFETY INFORMATION: Toxic (inhalation).
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Fluorides," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Fluorides," Appendix B.
See "Fluorides and Other Compounds," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Fluorides," Appendix B.
See "Fluorides and Hydrogen Fluoride," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
Water Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Fluoride Compounds," Appendix B.
See "Fluoride Ions," Appendix B.
See "Fluorides," Appendix B.
A-10
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AMMONIUM BISULFITE (CAS Number 10192-30-0)
RQ: 2270 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Sulfite Ions," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
Water Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Sulfites," Appendix B.
A-ll
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AMMONIUM CARBONATE (CAS Number 506-87-6)
RQ: 2270 kg
SAFETY INFORMATION:
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Ammonia," Appendix B.
A-12
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AMMONIUM CHLORIDE (CAS Number 12125-02-9
RQ: 2270 kg
SAFETY INFORMATION:
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Halides. Cyanides, and Other Compounds," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Chlorides," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
Water Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Chlorides," Appendix B.
A-13
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AMMONIUM CHROMATE (CAS Number 7788-98-9)
RQ: 454 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Chromium," Appendix B.
Soil/Sediment Samples
Field Method
See "Chromium," Appendix B.
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Chromates," Appendix B.
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Chromic Acid and Chromates," Appendix B.
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
Water Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Chromium," Appendix B.
See "Chromium, Trivalent," Appendix B.
See "Hexavalent Chromium," Appendix B.
A-14
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AMMONIUM DICHROMATE (CAS Number 7789-09-5)
RQ: 454 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Chromium," Appendix B.
Soil/Sediment Samples
Field Method
See "Chromium," Appendix B.
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Chromic Acid and Chromates," Appendix B.
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
Water Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
A-15
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AMMONIUM FLUOBORATE (CAS Number 13826-83-0)
RQ: 2270 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
Water Samples
Laboratory Method
See "Ammonia," Appendix B.
A-16
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AMMONIUM FLUORIDE (CAS Number 12125-01-8)
RQ: 45.4 kg
SAFETY INFORMATION; Exhibits chronic toxicity.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Fluorides," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Fluorides and Other Compounds," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Fluorides," Appendix B.
See "Fluorides and Hydrogen Fluoride," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Amines," Appendix B.
See "Ammonia," Appendix B.
See "Fluorides," Appendix B.
A-17
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AMMONIUM HYDROXIDE (CAS Number 1336-21-6)
RQ: 454 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Hydroxides," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
Water Samples
Laboratory Method
See "Ammonia," Appendix B.
A-18
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AMMONIUM SILICOFLUORIDE (CAS Number 16919-19-0)
RQ: 454 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
METHOD SUMMARY:
Analysis for ammonium silicofluoride in air can be performed by filtration
of air, followed by X-ray fluorescence analysis of the filter for silicon,
using a portable X-ray fluorescence spectrometer with a radioisotope excitation
source. Sampling time may be up to 8 hours, but analysis may be performed in
approximately 1 minute. This method is non-destructive, so that further
analysis of the filtered material may be undertaken following this measurement.
This method is not specific for ammonium silicofluoride, but measures the total
silicon content of the sample.
INTERFERENCES:
Polyvinyl chloride filters are unacceptable for sampling, and silica
quartz filter materials contain silicon, aluminum, and phosphorus. Cellulose
membrane or fiber filters and polycarbonate or fluorocarbon membrane filters
are acceptable, while glass fiber filters are satisfactory for sampling only if
of the highest purity.
QUALITY CONTROL:
No quality control procedures are given.
SENSITIVITY;
The method is sensitive to amounts of ammonium silicofluoride over 150
micrograms, or approximately 0.1 to 10.0 micrograms per cubic meter, depending
on the volume of air sampled.
REFERENCES:
Rhodes, J. R. ; Stout, J. C.; Schindler, J. S.; Piorek, S. "Portable X-ray
Survey Meters for in Situ Trace Element Monitoring of Air Particulates," In
Toxic Materials in~the Atmosphere, STP-786; American Society for Testing and
Materials: Philadelphia, 1981, pp. 70-82.
Rhodes, J. R.; Pradzynski, A. H.; Hunter, C. B.; Payne, J. S.; Lindgren, J. L.
"Energy Dispersive X-ray Fluorescence Analysis of Air Particulates in Texas,"
Environ. Sci. Technol.. 6(10), 1972, pp. 922-927.
A-19
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COST INFORMATION;
Cost per sample for analysis by this method is approximately $30 (list),
plus sampling costs.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Fluorides and Other Compounds," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
METHOD SUMMARY;
Analysis for ammonium silicofluoride in air can be performed by filtration
of air, followed by X-ray fluorescence analysis of the filter for silicon,
using an X-ray fluorescence spectrometer. This method is not specific for
ammonium silicofluoride, but measures the total silicon content of the sample.
Sampling time may be up to 8 hours, but analysis may be performed in approxi-
mately 1 minute. This method is non-destructive, so that further analysis of
the filtered material may be undertaken following this measurement.
INTERFERENCES;
Polyvinyl chloride filters are unacceptable for sampling, and silica
quartz filter materials contain silicon, aluminum, and phosphorus. Cellulose
membrane or fiber filters and polycarbonate or fluorocarbon membrane filters
are acceptable. This method is not specific for ammonium silicofluoride, but
measures silicon.
QUALITY CONTROL;
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision information is furnished. The
method is used to measure silicon only, and is sensitive to amounts of ammonium
silicofluoride over 150 micrograms, or approximately 0.1 to 10.0 microgram per
cubic meter, depending on the volume of air sampled.
A-20
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REFERENCES;
Rhodes, J. R.; Stout, J. C.; Schindler, J. S.; Piorek, S. "Portable X-ray
Survey Meters for in Situ Trace Element Monitoring of Air Particulates," In
Toxic Materials in the Atmosphere, STP-786; American Society for Testing and
Materials: Philadelphia, 1981, pp. 70-82.
Rhodes, J. R.; Pradzynski, A. H.; Hunter, C. B.; Payne, J. S.; Lindgren, J. L.
"Energy Dispersive X-ray Fluorescence Analysis of Air Particulates in Texas,"
Environ. Sci. Technol., £(10), 1972, pp. 922-927-
COST INFORMATION:
Cost per sample for analysis by this method is approximately $30 (list),
$20 (bid), plus sampling costs.
Note: NIOSH Method S348 (analysis by ion chromatography) is applicable.
(Reference furnished by reviewer.)
See also: "Ammonia," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
Water Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Fluorides," Appendix B.
A-21
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AMMONIUM SULFAMATE (CAS Number 7773-06-0)
RQ: 2270 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Sulfur Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Ammonia," Appendix B.
A-22
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AMMONIUM SULFIDE (CAS Number 12135-76-1)
RQ: 45.4 kg
SAFETY INFORMATION: Exhibits oral toxicity. Flashpoint 72°C.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Sulfides," Appendix B.
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Halides, Cyanides, and Other Compounds," Appendix B.
See "Sulfides," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Sulfur Compounds (Particulate)." Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Sulfides," Appendix B.
Water Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Sulfides," Appendix B,
A-23
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AMMONIUM SULFITE (CAS Number 10196-04-0)
RQ: 2270 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Sulfite Ions," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Sulfur Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Ammonia," Appendix B.
See "Sulfites," Appendix B.
A-24
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AMMONIUM THIOCYANATE (CAS Number 1762-95-4)
RQ: 2270 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Ammonia," Appendix B.
See "Thiocyanates," Appendix B.
A-25
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AMMONIUM THIOSULFATE (CAS Number 7783-18-8)
RQ: 2270 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Sulfur Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Ammonia," Appendix B.
A-26
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AMMONIUM VANADATE (CAS Number 7803-55-6)
RQ: 454 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Vanadium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonium," Appendix B.
See "Vanadium," Appendix B.
Water Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Vanadium," Appendix B.
A-27
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ANTIMONY (CAS Number 7440-36-0)
RQ: 0.454 kg
SAFETY INFORMATION; Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Antimony," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Antimony," Appendix B.
Air Samples
Laboratory Method
Note: NIOSH Method P&CAM 351 (analysis by ICP) is applicable. (Reference
furnished by reviewer.)
See also; "Antimony," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Antimony," Appendix B.
Water Samples
Laboratory Method
See "Antimony," Appendix B.
A-28
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ANTIMONY PENTACHLORIDE (CAS Number 7647-18-9)
RQ: 454 kg
SAFETY INFORMATION; Reacts vigorously with water to form HC1.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Antimony," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Reacts with water.
See "Antimony," Appendix B.
See "Halides, Cyanides, and Other Compounds," Appendix B.
Air Samples
Laboratory Method
See "Antimony," Appendix B.
See "Chlorides," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Antimony," Appendix B.
Water Samples
Laboratory Method
Reacts with water.
See "Antimony," Appendix B.
See "Chlorides," Appendix B.
A-29
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ANTIMONY POTASSIUM TARTRATE (CAS Number 28300-74-5)
RQ: 45.4 kg
SAFETY INFORMATION; Exhibits chronic toxicity.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Antimony," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Antimony," Appendix B.
See "Potassium," Appendix B.
Air Samples
Laboratory Method
See "Antimony," Appendix B.
See "Potassium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Antimony," Appendix B.
See "Potassium," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Antimony," Appendix B.
See "Potassium," Appendix B.
A-30
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ANTIMONY TRIBROMIDE (CAS Number 7789-61-9)
RQ: 454 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Antimony," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Reacts with water.
See "Antimony," Appendix B.
See "Halides, Cyanides, and Other Compounds," Appendix B.
Air Samples
Laboratory Method
See "Antimony," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Antimony," Appendix B.
Water Samples
Laboratory Method
Reacts with water.
See "Antimony," Appendix B.
See "Iodides and Bromides," Appendix B.
A-31
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ANTIMONY TRICHLORIDE (CAS Number 10025-91-9)
RQ: 454 kg
SAFETY INFORMATION: Reacts vigorously with water to form HC1.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Antimony," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Reacts with water.
See "Antimony," Appendix B.
See "Chlorides," Appendix B.
See "Halides, Cyanides, and Other Compounds," Appendix B.
Air Samples
Laboratory Method
See "Antimony," Appendix B.
See "Chlorides," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Antimony," Appendix B.
Water Samples
Laboratory Method
Reacts with water.
See "Antimony," Appendix B.
See "Chlorides," Appendix B.
A-32
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ANTIMONY TRIFLUORIDE (CAS Number 7783-56-4)
RQ: 454 kg
SAFETY INFORMATION; Toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Antimony," Appendix B.
See "Fluorides," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Antimony," Appendix B.
See "Fluorides and Other Compounds," Appendix B.
Air Samples
Laboratory Method
See "Antimony," Appendix B.
See "Fluorides," Appendix B.
See "Fluorides and Hydrogen Fluoride," Appendix B,
Soil/Sediment Samples
Laboratory Method
See "Antimony," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Antimony," Appendix B.
See "Fluorides," Appendix B.
A-33
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ANTIMONY TRIOXIDE (CAS Number 1309-64-4)
RQ: 454 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Antimony," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Antimony," Appendix B.
Air Samples
Laboratory Method
See "Antimony," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Antimony," Appendix B.
Water Samples
Laboratory Method
See "Antimony," Appendix B.
A-34
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ARSENIC (CAS Number 7440-38-2)
RQ: 0.454 kg
SAFETY INFORMATION; Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
METHOD SUMMARY
Arsenic in air samples can be measured by spectrophotometry. The arsenic,
converted to arsine, is adsorbed on mercuric iodide crystals, eluted with
iodine solution, and reacted with molybdate reagent and hydrogen sulfate solu-
tion at 100°C. The color is read at 720 nm on a portable spectrophotometer and
the arsenic concentration is calculated from a standard curve. (This method is
described by Olivee, W.T.; Funnell, H. S. Anal. Chem. 31, 1959, p. 259, and is
summarized in the reference given below.)
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
SENSITIVITY:
This method is a source method only.
REFERENCE;
Quantitative Analysis of Gaseous Pollutants, W. Ruch, Ed.; Ann Arbor-Humphrey
Science: Ann Arbor, 1970, p. 35.
COST INFORMATION:
No cost information has been obtained.
Soil/Sediment Samples
Field Method
See "Arsenic," Appendix B.
A-35
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Water Samples
Field Method
Air Samples
Laboratory Method
Note: NIOSH Methods P&CAM 286 (analysis by furnace AA) and P&CAM 320 (ion
chromatography, hydride generation, analysis by quartz furnace AA) are
applicable. (References provided by reviewer.)
See also; "Arsenic," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Arsenic," Appendix B.
Water Samples
Laboratory Method
See "Arsenic," Appendix B.
A-36
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ARSENIC ACID (CAS Numbers 1327-52-2, 7778-39-4)
RQ: 0.454 kg
SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Arsenic," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Arsenic," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Arsenic," Appendix B.
Water Samples
Laboratory Method
See "Arsenic," Appendix B.
A-37
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ARSENIC BISULFIDE (CAS Number 1303-32-8)
RQ: 2270 kg
SAFETY INFORMATION; Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Arsenic," Appendix B.
See "Sulfides," Appendix B.
Water Samples
Field Method
See "Sulfides," Appendix B.
Air Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Sulfur Compounds (Particulate) ," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Sulfides," Appendix B.
Water Samples
Laboratory Method
Insoluble in water.
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ARSENIC PENTOXIDE (CAS Number 1303-28-2)
RQ: 2270 kg
SAFETY INFORMATION: Exhibits toxicity (oral).
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Arsenic," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Arsenic," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Arsenic," Appendix B.
Water Samples
Laboratory Method
See "Arsenic," Appendix B.
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ARSENIC TRICHLORIDE (CAS Number 7784-34-1)
RQ: 2270 kg
SAFETY INFORMATION; Reacts vigorously with water to form HC1.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Arsenic," Appendix B.
Water Samples
Field Method
Reacts with water.
See "Halides, Cyanides and Other Compounds," Appendix B.
Air Samples
Laboratory Method
See "Arsenic," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Arsenic," Appendix B.
Water Samples
Laboratory Method
Reacts with water.
See "Arsenic," Appendix B.
A-40
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ARSENIC TRIOXIDE (CAS Number 1327-53-3)
RQ: 2270 kg
SAFETY INFORMATION: Exhibits toxicity (oral). Potentially carcinogenic.
Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Arsenic," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Arsenic," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Arsenic," Appendix B.
Water Samples
Laboratory Method
See "Arsenic," Appendix B.
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ARSENIC TRISULFIDE (CAS Number 1303-33-9)
RQ: 2270 kg
SAFETY INFORMATION; Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Arsenic," Appendix B.
See "Sulfides," Appendix B.
Water Samples
Field Method
See "Sulfides," Appendix B.
Air Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Sulfur Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Sulfides," Appendix B.
Water Samples
Laboratory Method
See "Sulfides," Appendix B.
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ASBESTOS (CAS Number 1332-21-4)
RQ: 0.454 kg
SAFETY INFORMATION; Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
METHOD SUMMARY:
A colorimetric test may be used to detect the possible presence of asbes-
tos-bound magnesium and iron in soil/sediment samples. A 100-milligram sample
is treated with acid to remove any iron and/or magnesium present that is not
asbestos-bound, then reacted to release the asbestos-bound iron and magnesium.
A positive result is indicated by a color change from clear to red.
INTERFERENCES:
A few other compounds that contain similarly bound magnesium and iron will
produce false positive results.
QUALITY CONTROL;
Non-asbestos control samples for magnesium and non-asbestos control samples
for iron should also be analyzed.
SENSITIVITY;
This method is sensitive to concentration levels of asbestos as low as 1
percent can be detected.
REFERENCES:
E.G. Apparatus Corporation, Asbestest® Test Kit for Screening Sample Materials
for Possible Presence of Asbestos, EC Apparatus Bulletin No. 110, EC Apparatus
Corp., St. Petersburg, Florida.
Gorman, Jr., W. EC Apparatus Corp., St. Petersburg, Florida, personal
communication, April 1983.
A-43
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COST INFORMATION:
The cost per sample for analysis by this method is approximately $10-18
(list).
Water Samples
Field Method
Air Samples
Laboratory Method 1
METHOD SUMMARY:
Asbestos mineral particles in air samples can be measured by scanning
transmission electron microscopy (STEM). The intensity of the X-ray spectrum
obtained is compared to that of a standard. The analysis will differentiate
particles of the three asbestos minerals: chrysotile, amosite, and crocidolite.
INTERFERENCES:
Variations in the diameter of the asbestos fiber can affect the intensity
ratios under certain conditions.
QUALITY CONTROL;
No quality control procedures are given.
EPA/TECHNICAL STATUS;
This method is not EPA-approved. Precision and accuracy information is
not furnished.
REFERENCE:
Grasserbauer, M. In Analysis of Airborne Particles by Physical Methods, H.
Malissa, Ed.; CRC Press: West Palm Beach, 1978, pp. 125-178.
COST INFORMATION;
The cost per sample for analysis by this method is $250 and up, plus
sampling costs.
Air Samples
Laboratory Method 2
METHOD SUMMARY;
Asbestos fibers in air samples may be measured by microscopy. The sample
is collected on a cellulose ester membrane filter. The filter is dissolved
into a transparent, optically homogenous gel by treatment with a reagent
A-44
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containing dimethyl phthalate and diethyl oxalate. The asbestos fibers are
sized and counted using a phase-contrast microscope at 400-450x magnification.
INTERFERENCES;
All particulates with a length-to-diameter ratio of 3 to 1 or greater and
a length greater than 5 micrometers are, in the absence of other information,
considered to be asbestos if the atmosphere is known to contain asbestos.
QUALITY CONTROL:
A blind recount should be performed for about 1 in every 10 samples.
EPA/TECHNICAL STATUS:
This method is classified as operational by the National Institute for
Occupational Safety and Health (NIOSH). The lowest limit of reliable quantifi-
cation is 100,000 fibers per cubic meter (NIOSH). The test method is generally
applicable for the number-count determination of asbestiform particulates rang-
ing from 0.5 to 20 particulates per cubic centimeter of air (ASTM). Precision
and accuracy information is furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 239; Publication No. 77-157-A, U.S.
DHEW, 1977.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.03, Method D4240-83; ASTM: Philadelphia, 1983.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $30 (list).
Note; NIOSH Method P&CAM 309 (filter collection, redeposition on a silver
filter, analysis by X-ray diffraction) is applicable for chrysotile
asbestos.
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
A-45
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METHOD SUMMARY;
Analysis for asbestos in water may be performed by electron-microscopic
examination of a membrane filter after a known quantity of water has been
passed through it.
INTERFERENCES;
Misidentification of fibers as asbestos can cause incorrect results, and
obscuration by large amounts of extraneous material can also interfere.
QUALITY CONTROL;
No quality control procedures are given.
EPA/TECHNICAL STATUS;
This method is an EPA interim method, updating the 1967 EPA method, and is
approved for use under the Clean Water Act. No precision or accuracy informa-
tion is furnished.
REFERENCE:
Anderson, C. H.; Long, J. McA. Interim Method for Determining Asbestos in
Water; EPA-600/4-80-005, U.S. EPA: Athens, Georgia, 1980.
COST INFORMATION;
The cost per sample for analysis by this method is $250 and up.
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BARIUM CYANIDE (CAS Number 542-62-1)
RQ: 4.54 kg
SAFETY INFORMATION; Highly toxic (ingestion).
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
METHOD SUMMARY;
Analysis for barium cyanide in air can be performed by filtration of air,
followed by X-ray fluorescence analysis of the filter for barium, using a
portable X-ray fluorescence spectrometer and a radioisotope excitation source.
Sampling time may be up to 8 hours, but analysis may be performed in approxi-
mately 1 minute. This method is non-destructive, so that further analysis of
the filtered material may be undertaken following this measurement. The method
is not specific for barium cyanide, but measures the total barium content of
the sample.
INTERFERENCES:
Polyvinyl chloride filters are unacceptable for sampling, and silica
quartz filter materials contain silicon, aluminum, and phosphorus. Cellulose
membrane or fiber filters and polycarbonate or fluorocarbon membrane filters
are acceptable, while glass fiber filters are satisfactory for sampling only if
of the highest purity.
QUALITY CONTROL;
No quality control procedures are given.
SENSITIVITY;
The method is sensitive to amounts of barium cyanide over 280 micrograms,
or approximately 0.1 to 10.0 microgram per cubic meter, depending on the volume
of air sampled.
REFERENCES;
Rhodes, J. R.; Stout, J. C.; Schindler, J. S.; Piorek, S. "Portable X-ray
Survey Meters for in Situ Trace Element Monitoring of Air Particulates," In
Toxic Materials in the Atmosphere, STP-786; American Society for Testing and
Materials: Philadelphia, 1981, pp. 70-82.
Rhodes, J. R.; Pradzynski, A. H.; Hunter, C. B.; Payne, J. S.; Lindgren, J. L.
"Energy Dispersive X-ray Fluorescence Analysis of Air Particulates in Texas,"
Environ. Sci. Technol., 6(10), 1972, pp. 922-927-
A-47
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COST INFORMATION:
The cost per sample for analysis by this method is approximately $30, plus
sampling costs.
Soil/Sediment Samples
Field Method
See "Cyanides," Appendix B.
Water Samples
Field Method
METHOD SUMMARY;
Analysis for barium cyanide in water can be performed by turbidimetric
analysis for barium. A 25-milliliter water sample is treated with a reagent,
causing barium to precipitate as the sulfate. The precipitate is held in
suspension by a colloid, and the turbidity is analyzed with a portable spectro-
photometer. This method is not specific for barium cyanide, but measures the
total barium content of the sample.
INTERFERENCES;
Calcium concentrations over 100 milligrams per liter interfere. Strontium
interferes and is read as barium.
QUALITY CONTROL:
A barium standard solution can be used to check the accuracy of the test.
SENSITIVITY;
The method is sensitive to concentration levels of barium above approxi-
mately 25 milligrams per liter in the absence of interferences.
REFERENCE;
Hach Chemical Company, Procedures, Chemical Lists, and Glassware for Water and
Wastewater Analysis, Hach: Ames, IA, 1975, pp. 2-17, 2-18.
COST INFORMATION:
The cost per sample for analysis by this method is approximately $15-23
(list).
See also: "Cyanides," Appendix B.
See also; "Halides, Cyanides, and Other Compounds," Appendix B.
A-48
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Air Samples
Laboratory Method 1
METHOD SUMMARY:
Analysis for barium cyanide in air can be performed by filtration of air,
followed by X-ray fluorescence analysis of the filter for barium, using an
X-ray fluorescence spectrometer. Sampling time may be up to 8 hours, but
analysis may be performed in approximately 1 minute. This method is non-
destructive, so that further analysis of the filtered material may be under-
taken following this measurement. This method is not specific for barium
cyanide, but measures the total barium content of the sample.
INTERFERENCES:
Polyvinyl chloride filters are unacceptable for sampling, and silica
quartz filter materials contain silicon, aluminum, and phosphorus. Cellulose
membrane or fiber filters and polycarbonate or fluorocarbon membrane filters
are acceptable, while glass-fiber filters are satisfactory for sampling only if
of the highest purity.
QUALITY CONTROL:
No quality control procedure is given.
EPA/TECHNICAL STATUS;
This method is not EPA-approved. Precision information is furnished. The
method is sensitive to concentration levels of barium cyanide over 100 micro-
grams, or approximately 0.1 to 10.0 micrograms per cubic meter, depending on
the volume of air sampled.
REFERENCES:
Rhodes, J. R.; Stout, J. C.; Schindler, J. S.; Piorek, S. "Portable X-ray
Survey Meters for jln Situ Trace Element Monitoring of Air Particulates," In
Toxic Materials in the Atmosphere, STP-786; American Society for Testing and
Materials: Philadelphia, 1981, pp. 70-82.
Rhodes, J. R.; Pradzynski, A. H.; Hunter, C. B.; Payne, J. S.; Lindgren, J. L.
"Energy Dispersive X-ray Fluorescence Analysis of Air Particulates in Texas,"
Environ. Sci. Technol., 6(10), 1972, pp. 922-927.
COST INFORMATION;
The cost per sample for analysis by this method is approximately $30
(list), $20 (bid), plus sampling costs.
A-49
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Air Samples
Laboratory Method 2
METHOD SUMMARY:
Analysis for barium cyanide in air can be performed by cellulose-membrane
filtration of a known volume of air, followed by hot water leaching of soluble
compounds and subsequent analysis of the resulting solution for barium by
atomic absorption spectrometry (AA). The method is not specific for barium
cyanide, but measures all those barium compounds that are dissolved from the
collection filter in boiling water.
INTERFERENCES;
Addition of sodium chloride to the sample is required to suppress ioniza-
tion.
QUALITY CONTROL:
A method blank should be processed with each set of 10 samples and the
results used in the calculations.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH), and validated over the range of 0.281 to 1.084 milligrams
of barium per cubic meter for a 168-liter air sample. The method may be
extended to lower concentrations by longer sampling times or increased instru-
mental response. A method classified as operational by NIOSH is for use over
the range of 42 to 1.650 milligrams per cubic meter in a 240-liter air sample.
Precision and accuracy information is furnished.
REFERENCES;
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set N, Method S198; PB-258 433 (NTIS), U.S. DHEW: Cincinnati, 1976.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods. 2nd ed., Vol. 1, Method P&CAM 173; Publication No. 77-157-A, U.S.
DHEW: Cincinnati, 1977-
COST INFORMATION;
Cost per sample for analysis by this method is approximately $10-20
(list), plus sampling costs.
Note; NIOSH Method 351 (acid digestion, analyses for barium by ICP) is
applicable. (Reference provided by reviewer.)
See also; "Cyanides," Appendix B.
A-50
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Soil/Sediment Samples
Laboratory Methods
METHOD SUMMARY:
Analysis of soil/sediment samples for barium cyanide can be performed by
analysis for barium by atomic spectrometry. A 2-gram sample is digested with
nitric acid and hydrogen peroxide and analyzed by inductively coupled plasma
(ICP) or flame atomic absorption spectrometry (AA). These methods are not
specific for barium cyanide, but measure the total barium present in the sample.
INTERFERENCES;
Potassium chloride must be added to the sample and standards to suppress
the ionization of barium.
QUALITY CONTROL;
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods. A
reference standard should be run weekly and at least 10 percent of the samples
should be duplicates and/or standards.
EPA/TECHNICAL STATUS;
These methods are in use in the CERCLA program and are approved for the
National Pollutant Discharge Elimination System (NPDES). Precision and accuracy
information is furnished.
REFERENCES;
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes. Method 208.1; EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 7080, 7081; SW-846, U.S. EPA:
Washington, 1982.
Federal Register, 44 (233), December 3, 1979, pp. 69559-69564.
COST INFORMATION;
Cost per sample for analysis by flame AA is approximately $24 (list); by
ICP, it is approximately $20 (list).
See also; "Cyanides," Appendix B.
A-51
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Water Samples
Laboratory Methods
METHOD SUMMARY:
Analysis of water samples for barium cyanide can be performed by atomic
spectrometry. A 100-milliliter sample is digested with nitric acid and hydro-
gen peroxide and analyzed by inductively coupled plasma (ICP) or flame or
furnace atomic absorption (AA) spectrometry. This method is not specific for
barium cyanide, but measures the total barium content of the sample.
INTERFERENCES:
Potassium chloride must be added to the sample and standards to suppress
the ionization of barium.
QUALITY CONTROL;
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods. A
reference standard should be run weekly and at least 10 percent of the analyses
should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for the
National Pollutant Discharge Elimination System (NPDES) of the Clean Water Act.
Precision and accuracy information is furnished. Limits of detection are 0.1
milligram barium per liter for flame AA, and 2 micrograms barium per liter for
furnace AA or ICP (EPA). The working range for flame AA is 1 to 5 milligrams
per liter (ASTM).
REFERENCES;
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Methods 200.7, 208.1, 208.2, EPA-600/4-79-020, U.S. EPA:
Cincinnati, 1979.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste;
Physical/Chemical Methods, 2nd ed., Methods 7080, 7081; SW-846, U.S. EPA:
Washington, 1982.
Federal Register, 44 (233), December 3, 1979, pp. 69559-69564.
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.02, D3051-78, D5986-81; ASTM: Philadelphia, 1983.
A-52
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COST INFORMATION;
Cost per sample for analysis by flame AA is approximately $10-20 (list)-
by furnace AA, approximately $18-50 (list), by ICP, approximately $10 (list).
See also; "Acid Anions," Appendix B.
See also: "Cyanides," Appendix B.
A-53
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BERYLLIUM (CAS Number 7440-41-7)
RQ: 0.454 kg
SAFETY INFORMATION; Potentially carcinogenic. Potentially chronically toxic.
Exhibits toxicity (inhalation).
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Beryllium," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
Note: NIOSH METHOD 288 (graphite furnace analysis) is applicable. (Reference
furnished by reviewer.)
See also; "Beryllium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Beryllium," Appendix B.
Water Samples
Laboratory Method
See "Beryllium," Appendix B.
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BERYLLIUM CHLORIDE (CAS Number 7787-47-5)
RQ: 2270 kg
SAFETY INFORMATION; Potentially carcinogenic. Potentially chronically toxic.
Reacts vigorously with water to form HC1 and to evolve
heat.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Beryllium," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Halides, Cyanides, and Other Compounds," Appendix B.
Air Samples
Laboratory Method
See "Beryllium," Appendix B.
See "Chlorides," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Beryllium," Appendix B.
Water Samples
Laboratory Method
See "Beryllium," Appendix B.
See "Chlorides," Appendix B.
A-55
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BERYLLIUM FLUORIDE (CAS Number 7787-49-7)
RQ: 2270
SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Beryllium," Appendix B.
See "Fluorides," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Fluorides and Other Compounds," Appendix B.
Air Samples
Laboratory Method
See "Beryllium," Appendix B.
See "Fluorides," Appendix B.
See "Fluorides and Hydrogen Fluoride," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Beryllium," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Beryllium," Appendix B.
See "Fluorides," Appendix B.
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BERYLLIUM NITRATE (CAS Numbers 13597-99-4. 7787-55-5)
RQ: 2270 kg
SAFETY INFORMATION; Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Beryllium," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Nitrate Ions," Appendix B.
Air Samples
Laboratory Method
See "Beryllium," Appendix B.
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Beryllium," Appendix B.
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Beryllium," Appendix B.
See "Nitrates," Appendix B.
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CACODYLIC ACID (CAS Number 75-60-5)
RQ: 0.454 kg
SAFETY INFORMATION; Potentially carcinogenic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Arsenic," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Arsenic," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Arsenic," Appendix B.
Water Samples
Laboratory Method
See "Arsenic," Appendix B.
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CADMIUM (CAS Number 7440-43-9)
RQ: 0.454 kg
SAFETY INFORMATION; Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Cadmium," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Cadmium," Appendix B.
Air Samples
Laboratory Method
METHOD SUMMARY:
Atomic spectrometry may be used for the analysis of cadmium fumes in air
samples. Analysis is performed by membrane-filtration of 140 liters of air,
followed by acid digestion of the sample and sampling medium and flame atomic
absorption (AA) analysis of the resulting solution at 228.8 nm.
INTERFERENCES;
Silicon has been reported to interfere with the analysis. Cadmium dust
and other cadmium compounds interfere.
QUALITY CONTROL:
A method blank should be analyzed with each set of 10 or fewer samples.
The percent recovery should be determined and, if it is less than 95 percent,
results corrected accordingly. Duplicate determinations should agree within 5
percent.
EPA/TECHNICAL STATUS;
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH), and validated over the ranges of 0.04 to 0.175 milligrams
per cubic meter in a 140-liter air sample, and 0.122 to 0.175 milligrams per
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cubic meter in a 25-liter sample. Precision and accuracy information is
furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, Ten NIOSH Analytical Methods^
Set 1, Method S313; PB-271 712 (NTIS). U.S. DREW: Cincinnati, 1977.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods. 2nd ed., Vol. 3, Method S313; Publication No. 77-157-C, U.S. DREW:
Cincinnati, 1977.
Note; NIOSH Method P&CAM 345 (filter collection and analyses by X-ray
fluorescence) is applicable. (Reference provided by reviewer.)
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10-20
(list), plus sampling costs.
See also: "Cadmium," Appendix B.
See also; "Lead and Cadmium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Cadmium," Appendix B.
Water Samples
Laboratory Method
See "Cadmium," Appendix B.
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CADMIUM ACETATE (CAS Number 543-90-8)
RQ: 45.4 kg
SAFETY INFORMATION; Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Cadmium," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Cadmium," Appendix B.
Air Samples
Laboratory Method
See "Cadmium," Appendix B.
See "Lead and Cadmium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Cadmium," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B,
See "Cadmium," Appendix B.
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CADMIUM BROMIDE (CAS Number 7789-42-6)
RQ: 45.4 kg
SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Cadmium," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Cadmium," Appendix B.
See "Halides, Cyanides, and Other Compounds," Appendix B.
Air Samples
Laboratory Method
See "Cadmium," Appendix B.
See "Lead and Cadmium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Cadmium," Appendix B.
Water Samples
Laboratory Method
See "Cadmium," Appendix B.
See "Iodides and Bromides," Appendix B.
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CADMIUM CHLORIDE (CAS Number 10108-64-2)
RQ: 45.4 kg
SAFETY INFORMATION; Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Cadmium," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Cadmium," Appendix B.
See "Halides, Cyanides, and Other Compounds," Appendix B.
Air Samples
Laboratory Method
See "Cadmium," Appendix B.
See "Chlorides," Appendix B.
See "Lead and Cadmium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Cadmium," Appendix B.
Water Samples
Laboratory Method
See "Cadmium," Appendix B.
See "Chlorides," Appendix B.
A-63
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RQ: 454 kg
SAFETY INFORMATION:
CALCIUM ARSENATE (CAS Number 7778-44-1)
Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Calcium," Appendix B.
Soil/Sediment Samples
Field Method
See "Arsenic," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Calcium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Calcium," Appendix B.
Water Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Calcium," Appendix B.
A-64
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CALCIUM ARSENITE (CAS Number 52740-16-6)
RQ: 454 kg
SAFETY INFORMATION; Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Calcium," Appendix B.
Soil/Sediment Samples
Field Method
See "Arsenic," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Calcium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Calcium," Appendix B.
Water Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Calcium," Appendix B.
A-65
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CALCIUM CARBIDE (CAS Number 75-20-7)
RQ: 4.54 kg
SAFETY INFORMATION; Forms flammable and explosive gas on exposure to moisture.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Calcium," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Calcium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Calcium," Appendix B.
Water Samples
Laboratory Method
See "Calcium," Appendix B.
A-66
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CALCIUM CHROMATE (CAS Number 13765-19-0)
RQ: 454 kg
SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Calcium," Appendix B.
See "Chromium," Appendix B.
Soil/Sediment Samples
Field Method
See "Chromium," Appendix B.
Water Samples
Field Method
See "Chromium," Appendix B.
See "Chromates," Appendix B.
See "Hexavalent Chromium," Appendix B.
Air Samples
Laboratory Method
See "Calcium," Appendix B.
See "Chromic Acid and Chromates," Appendix B.
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Calcium," Appendix B.
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
Water Samples
Laboratory Method
See "Calcium," Appendix B.
See "Chromium," Appendix B.
See "Chromium, Trivalent," Appendix B.
See "Hexavalent Chromium," Appendix B.
A-67
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RQ: 4.54 kg
SAFETY INFORMATION:
CALCIUM CYANIDE (CAS Number 592-01-8)
Forms toxic cyanide in water. Evolves highly toxic
hydrogen cyanide on contact with acids. Fire risk if
exposed to moisture or combined with calcium carbide.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Calcium," Appendix B.
Soil/Sediment Samples
Field Method
See "Cyanides," Appendix B.
Water Samples
Field Method
See "Halides, Cyanides, and Other Compounds," Appendix B.
See "Cyanides," Appendix B.
Air Samples
Laboratory Method
See "Calcium," Appendix B.
See "Cyanides," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Calcium," Appendix B.
See "Cyanides," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Calcium," Appendix B.
See "Cyanides," Appendix B.
A-68
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CALCIUM DODECYLBENZENE SULFONATE (CAS Number 26264-06-2)
RQ: 454 kg
SAFETY INFORMATION:
Air Samples
Field Method
See "Calcium," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Anionic Detergents," Appendix B.
Air Samples
Laboratory Method
See "Calcium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Calcium," Appendix B.
Water Samples
Laboratory Method
See "Alkyl Benzene Sulfonates," Appendix B.
See "Calcium," Appendix B.
A-69
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CALCIUM HYPOCHLORITE (CAS Number 7778-54-3)
RQ: 4.54 kg
SAFETY INFORMATION; Strong oxidizer; can readily cause fires.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Calcium," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Calcium," Appendix B.
See "Halides, Cyanides, and Other Compounds," Appendix B.
Air Samples
Laboratory Method
See "Calcium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Calcium," Appendix B.
Water Samples
Laboratory Method
See "Calcium," Appendix B.
See "Chlorine," Appendix A.
A-70
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CHLORINE (CAS Number 7782-50-5)
RQ: 4.54 kg
SAFETY INFORMATION: Toxic (inhalation). Dangerous if in contact with
reducing agents.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
METHOD SUMMARY:
Analysis for chlorine in air may be performed by use of a detector tube.
A 2-liter sample is collected and analyzed with a hand-operated bellows pump
and a chlorine gas detector tube (Draeger® 67 28411 or equivalent). A positive
result is indicated by a color change in the tube from white to either pale
yellow or pale yellowish-orange. The test is based on the reaction of chlorine
with £-toluidine.
INTERFERENCES:
Chlorine dioxide will also give a positive result.
QUALITY CONTROL:
No quality control procedures are given.
SENSITIVITY:
The lower detection limit of the tube varies from approximately 0.5 to
1 milligram per cubic meter.
REFERENCES:
National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations
and Technical Gas Analysis with Draeger® Tubes", 4th ed.; Draeger: Pittsburgh,
August 1979.
National Draeger, Inc., Bulletin No. ND-105, Draeger: Pittsburgh, January 1,
1982.
National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit
Value Range, Draeger® Gas Analysis Product Information; Leaflet 4340.3e,
Draeger: Pittsburgh, December 1981.
COST INFORMATION;
The cost per sample by this method is approximately $13-18 (list).
A-71
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Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Halides, Cyanides, and Other Compounds," Appendix B.
Air Samples
Laboratory Method 1
METHOD SUMMARY;
Free chlorine in air may be determined colorimetrically. A known volume
of air is passed through a chromic acid scrubber and two impingers. The sample
is treated with an alkaline solution of 4-nitroaniline to produce an orange-
brown color that is measured at 485 nm with a spectrophotometer. Six standard
solutions, with concentrations from 10 micrograms to 2 milligrams of free
chlorine per liter, are used for calibration.
INTERFERENCES:
Sulfur dioxide interference is removed by the chromic acid scrubber.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS;
This method is not EPA-approved, but is used by the Alberta Environmental
Centre, Alberta, Canada. Precision and accuracy information is not furnished.
The method is sensitive to concentration levels of chlorine in the range of 0.2
to 50 micrograms per milliliter in the absorbing solution.
REFERENCES:
Alberta Environment, Methods Manual Chemical Analysis of Atmospheric Pollutants,
2nd ed., Method 11515, Alberta Environmental Centre: Vegreville, Alberta,
Canada, 1981.
Geabbay, J.; Davidson, M.; Donagi, A. "Spectrophotometric Determination of
Free Chlorine in Air," Analyst, 101, February 1976, p. 128-135.
COST INFORMATION;
The cost per sample for analysis by this method is approximately $20-25
(list), plus sampling costs.
A-72
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Air Samples
Laboratory Method 2
METHOD SUMMARY:
Free chlorine in air samples may be measured colorimetrically. A known
volume of air is passed through a fritted bubbler containing dilute methyl
orange. The methyl orange dye is bleached quantitatively by free chlorine, and
the extent of bleaching is determined with a spectrophotometer at 505 nm.
INTERFERENCES:
Free bromine, nitrogen dioxide, manganese, and possibly ozone interfere
positively. Sulfur dioxide in solution interferes negatively. Nitrites impart
an off-color orange to the methyl orange reagent.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is classifed as tentative by the National Institute of
Occupational Safety and Health (NIOSH) for use over the range of 145 to 2900
micrograms per cubic meter in a 30-liter sample. Limited precision informa-
tion is furnished.
REFERENCE:
U.S. Department of Health, Education and Welfare, NIOSH Manual of Analtyical
Methods, 2nd ed., Vol. 1, Method P&CAM 209; Publication No. 77-157-A, U.S.
DHEW: Cincinnati, 1977.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $20-25
(list), plus sampling costs.
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
METHOD SUMMARY:
Water samples may be analyzed for chlorine by spectrophotometry. A 10-
milliliter sample is treated with potassium iodide at a pH below 4; the liber-
ated iodine reacts with N,N-diethyl-p_-phenylenediamine (DPD) to produce a red-
colored solution, which is measured spectrophotometrically.
A-73
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INTERFERENCES:
Turbidity or color in the sample can preclude use of the method.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is approved for use in the National Pollutant Discharge
Elimination System (NPDES) of the Clean Water Act. Precision and accuracy
information is furnished.
REFERENCE:
U.S. Environmental Protection Agency, Methods for the Chemical Analysis of
Water and Wastes, Method 330.5, EPA-600/4-79-020; U.S. EPA: Cincinnati, 1979.
COST INFORMATION:
The cost per sample for analysis by this method is approximately $20-25
(list).
Water Samples
Laboratory Method 2
METHOD SUMMARY:
Water samples may be analyzed for chlorine by one of three iodometric
titrimetric methods. In each of the methods, iodine is stoichiometrically
liberated from potassium iodide by the chlorine in a 100- or 200-milliliter
sample. In the first method, the iodine is titrated with phenylarsine oxide,
and an amperemeter or a starch indicator can be used to detect the endpoint.
Stirring may lower the chlorine value, and copper, silver or substantial
amounts of organic matter must not be present. In the second method, an excess
of phenylarsine oxide is added and the excess is determined by back-titration
with a standard iodine titrant. Either a starch indicator or an amperemeter
can be used to determine the endpoint. In the third method, the liberated
iodine is titrated with N,N-diethyl-p-phenylenediamine (DPD), using ferrous
ammonium sulfate (FAS) as an indicator. All three methods will measure
chlorine concentrations above 1 milligram per liter.
INTERFERENCES:
Color and turbidity in the sample can make the endpoint difficult to
detect when a starch indicator is used, while copper and silver ions can
interfere with amperometric endpoint detection. Buffering the sample at pH 4
minimizes interferences for the starch-indicator methods from iron(III),
manganese(VI), and nitrite ions. Copper and dissolved oxygen are prevented
from interfering with the FAS/DPD procedure by addition of disodium ethylene-
diaminetetraacetate.
A-74
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QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
These methods are approved for use in the National Pollutant Discharge
Elimination System (NPDES) of the Clean Water Act. Precision and accuracy
information is furnished.
REFERENCE:
U.S. Environmental Protection Agency Methods for the Chemical Analysis of Water
and Wastes, Methods 330.1, 330.2, 330.3, 330.4; EPA-600/4-79-020, U.S. EPA:
Cincinnati, 1979.
COST INFORMATION:
The cost per sample for analysis by this method is approximately $13-18
(list).
A-75
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CHLOROSULFONIC ACID (CAS Number 7790-94-5)
RQ: 454 kg
SAFETY INFORMATION; Dangerously reactive with water or moisture; reacts to
form hydrochloric acid and sulfuric acid. Strong oxidiz-
ing agent. Highly toxic (inhalation). Strong irritant
(eye, skin). Flammable in contact with combustable
material; evolves hydrogen gas on contact with most
metals.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Laboratory Method
Field Method
Water Samples
Field Method
Reacts with water.
See "Cholinesterase-Inhibiting Compounds," Appendix B.
See "Fluorides and Other Compounds," Appendix B.
See "Halides, Cyanides, and Other Compounds, Appendix B,
Air Samples
Laboratory Method
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
Reacts with water.
A-76
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CHROMIC ACETATE (CAS Number 1066-30-4)
RQ: 454 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Chromium," Appendix B.
Soil/Sediment Samples
Field Method
See "Chromium," Appendix B.
Water Samples
Field Method
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
Air Samples
Laboratory Method
See "Chromic Acid and Chromates," Appendix B.
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Chromium," Appendix B.
See "Chromium, Trivalent," Appendix B.
A-77
-------
CHROMIC ACID (CAS Number 11115-74-5)
RQ: 454 kg
SAFETY INFORMATION; Strong oxidizer; can readily cause fires. Potentially
carcinogenic. Potentially chronically toxic. Strong
irritant to skin (corrosive).
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Chromium," Appendix B.
See "Chromic Acid and Strontium Chromate," Appendix B.
Soil/Sediment Samples
Field Method
See "Chromium," Appendix B.
Water Samples
Field Method
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
Air Samples
Laboratory Method
METHOD SUMMARY;
Chromic acid mist in air samples may be measured colorimetrically. The
chromic acid is collected on a polyvinyl chloride (PVC) filter, the filter is
washed in 0.5N sulfuric acid, diphenylcarbazide is added, and additional acid
is added to bring the solution to volume. The absorbance of the solution is
read at 540 nm on a spectrophotometer-
INTERFERENCES;
Many of the heavy metals may interfere at high concentrations.
QUALITY CONTROL:
Spiked filters should not be used for standards or other purposes since
such samples are not very stable. A blank should be processed and its value,
if any, should be used in calculation of results.
A-78
-------
EPA/TECHNICAL STATUS:
This method is classified as operational by the National Institute for
Occupational Safety and Health (NIOSH) for use over the range of 0.004 to 0.2
milligrams chromic acid per cubic meter, using a 100-liter air sample.
Precision and accuracy information is furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 169; Publication No. 77-157-A, U.S.
DHEW: Cincinnati, 1977.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, Method P&CAM 169; Publication No. 75-121, U.S. DHEW: Cincinnati, 1974.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $25-30
(list), plus sampling costs.
See also: "Chromic Acid and Chromates," Appendix B.
See also: "Chromium," Appendix B.
See also: "Hexavalent Chromium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
Water Samples
Laboratory Method
See "Chromium," Appendix B.
See "Chromium, Hexavalent," Appendix B.
A-79
-------
CHROMIC SULFATE (CAS Number 10101-53-8)
RQ: 454 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Chromium," Appendix B.
Soil/Sediment Samples
Field Method
See "Chromium," Appendix B,
Water Samples
Field Method
See "Chromium, Hexavalent," Appendix B.
See "Chromium," Appendix B.
Air Samples
Laboratory Method
See "Nitrates and Sulfates," Appendix B.
See "Sulfur Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Chromium," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Chromium," Appendix B.
See "Chromium, Trivalent," Appendix B.
A-80
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CHROMIUM (CAS Number 7440-47-3)
RQ: 0.454 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Chromium," Appendix B.
Soil/Sediment Samples
Field Method
See "Chromium," Appendix B.
Water Samples
Field Method
See "Chromium," Appendix B.
Air Samples
Laboratory Method
See "Chromium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Chromium," Appendix B.
See "Chromium, Hexavalent," Appendix B.
Water Samples
Laboratory Method
See "Chromium," Appendix B.
See "Chromium, Hexavalent," Appendix B.
A-81
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CHROMOUS CHLORIDE (CAS Number 10049-05-5)
RQ: 454 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Chromium," Appendix B.
Soil/Sediment Samples
Field Method
See "Chromium," Appendix B.
Water Samples
Field Method
See "Chromium," Appendix B.
Air Samples
Laboratory Method
See "Chromium," Appendix B.
See "Chlorides," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Chromium," Appendix B.
Water Samples
Laboratory Method
See "Chlorides," Appendix B.
See "Chromium," Appendix B.
A-82
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COBALTOUS BROMIDE (CAS Number 7789-43-7)
RQ: 454 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Cobalt," Appendix B.
Water Samples
Field Method
See "Cobalt," Appendix B.
See "Halides, Cyanides, and Other Compounds," Appendix B.
Air Samples
Laboratory Method
See "Cobalt," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Cobalt," Appendix B.
Water Samples
Laboratory Method
See "Cobalt," Appendix B.
A-83
-------
COBALTOUS FORMATE (CAS Number 544-18-3)
RQ: 454 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Cobalt," Appendix B.
See "Cobalt," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Cobalt," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Cobalt," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Cobalt," Appendix B.
A-84
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COBALTOUS SULFAMATE (CAS Number 14017-41-5)
RQ: 454 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Cobalt," Appendix B.
See "Cobalt," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Cobalt," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Cobalt," Appendix B.
Water Samples
Laboratory Method
See "Cobalt," Appendix B.
A-85
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COPPER (CAS Number 7440-50-8)
RQ: 2270 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Copper," Appendix B.
Soil/Sediment Samples
Field Method
See "Copper," Appendix B.
See "Copper," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Copper," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Copper," Appendix B.
Water Samples
Laboratory Method
See "Copper," Appendix B.
A-86
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COPPER CYANIDE (CAS Number 544-92-3)
RQ: 4.54 kg
SAFETY INFORMATION:
Toxic.
CAUTION:
The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Copper," Appendix B.
Soil/Sediment Samples
Field Method
See "Copper," Appendix B.
See "Cyanides," Appendix B,
Water Samples
Field Method
See "Copper," Appendix B.
See "Cyanides," Appendix B.
Air Samples
Laboratory Method
See "Copper," Appendix B.
See "Cyanides," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Copper," Appendix B.
See "Cyanides," Appendix B.
Water Samples
Laboratory Method
See "Copper," Appendix B.
See "Cyanides," Appendix B.
A-87
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CUPRIC ACETATE (CAS Number 142-71-2)
RQ: 45.4 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Copper," Appendix B.
Soil/Sediment Samples
Field Method
See "Copper," Appendix B.
See "Copper," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Copper," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Copper," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Copper," Appendix B.
A-88
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CUPRIC ACETOARSENITE (CAS Number 12002-03-8)
RQ: 45.4 kg
SAFETY INFORMATION: Highly toxic (ingestion).
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Copper," Appendix B.
Soil/Sediment Samples
Field Method
See "Arsenic," Appendix B.
See "Copper," Appendix B.
Water Samples
Field Method
See "Copper," Appendix B.
Air Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Copper," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Copper," Appendix B.
Water Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Copper," Appendix B.
A-89
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CUPRIC CHLORIDE (CAS Number 7447-39-4)
RQ: 4.54 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Copper," Appendix B,
Soil/Sediment Samples
Field Method
See "Copper," Appendix B.
Water Samples
Field Method
See "Copper," Appendix B.
See "Halides, Cyanides, and Other Compounds," Appendix B.
Air Samples
Laboratory Method
See "Chlorides," Appendix B.
See "Copper," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Copper," Appendix B.
Water Samples
Laboratory Method
See "Chlorides," Appendix B.
See "Copper," Appendix B.
A-90
-------
CUPRIC NITRATE (CAS Number 3251-23-8)
RQ: 45.4 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Copper," Appendix B.
Soil/Sediment Samples
Field Method
See "Copper," Appendix B.
Water Samples
Field Method
See "Copper," Appendix B.
See "Nitrate Ions," Appendix B.
Air Samples
Laboratory Method
See "Copper," Appendix B.
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Copper," Appendix B.
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
See "Copper," Appendix B.
See "Nitrates," Appendix B.
A-91
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CUPRIC OXALATE (CAS Number 5893-66-3)
RQ: 45.4 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Copper," Appendix B.
Soil/Sediment Samples
Field Method
See "Copper," Appendix B.
See "Copper," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Copper," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Copper," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Copper," Appendix B.
A-92
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RQ: 4.54 kg
SAFETY INFORMATION:
CUPRIC SULFATE (CAS Number 7758-98-7)
Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Copper," Appendix B.
Soil/Sediment Samples
Field Method
See "Copper," Appendix B.
See "Copper," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Copper," Appendix B.
See "Nitrates and Sulfates," Appendix B.
See "Sulfates (Particulate)," Appendix B.
See "Sulfur Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Copper," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
See "Copper," Appendix B.
See "Sulfates," Appendix B.
A-93
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CUPRIC SULFATE, AMMONIATED (CAS Number 10380-29-7)
RQ: 45.4 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Copper," Appendix B.
Soil/Sediment Samples
Field Method
See "Copper," Appendix B.
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Copper," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Copper," Appendix B.
See "Nitrates and Sulfates," Appendix B.
See "Sulfates," Appendix B.
See "Sulfur Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Copper," Appendix B.
See "Nitrates and Sulfates,
Appendix B.
Water Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Copper," Appendix B.
See "Sulfates," Appendix B.
A-94
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CUPRIC TARTRATE (CAS Number 815-82-7)
RQ: 45.4 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Copper," Appendix B.
Soil/Sediment Samples
Field Method
See "Copper," Appendix B.
See "Copper," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Copper," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Copper," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B,
See "Copper," Appendix B.
A-95
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CYANIDES (CAS Number 57-12-5)
RQ: 4.54 kg
SAFETY INFORMATION: Can form very toxic hydrogen cyanide upon contact with
water or acids.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Cyanides," Appendix B.
See "Hydrogen Cyanide," Appendix A.
Soil/Sediment Samples
Field Method
See "Cyanides," Appendix B.
Water Samples
Field Method
See "Cyanides," Appendix B.
Air Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Hydrogen Cyanide," Appendix A.
Soil/Sediment Samples
Laboratory Method
See "Cyanides," Appendix B.
Water Samples
Laboratory Method
See "Cyanides," Appendix B.
A-96
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CYANOGEN (CAS Number 460-19-5)
RQ: 45.4 kg
SAFETY INFORMATION; Highly toxic. Highly flammable gas.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Cyanides," Appendix B.
Water Samples
Field Method
See "Cyanides," Appendix B.
Air Samples
Laboratory Method
See "Cyanides," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Cyanides," Appendix B.
Water Samples
Laboratory Method
See "Cyanides," Appendix B.
A-97
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CYANOGEN BROMIDE (CAS Number 506-68-3)
RQ: 454 kg
SAFETY INFORMATION; Highly toxic. Strong irritant to eyes and skin.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
METHOD SUMMARY:
A cyanogen chloride gas detector tube (Draeger® CH 19801, or equivalent)
can be used for measurement of cyanogen bromide in air. The cyanogen bromide
reacts with pyridine, barbituric acid, and glutaconaldehyde cyanamide in the
indicating layer. A positive result is indicated by a color change from white
to brownish pink in the indicating layer of the tube.
INTERFERENCES:
Chlorine dioxide and cyanogen chloride can give a positive interference.
QUALITY CONTROL:
No quality control procedures are given.
SENSITIVITY:
This method is sensitive to concentration levels of cyanogen bromide over
5 milligrams per cubic meter.
REFERENCE:
National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations
and Technical Gas Analysis with Draeger® Tubes", 4th ed.; Draeger: Pittsburgh,
August 1979.
COST INFORMATION:
The cost per sample for analysts by this method is approximately $13-
(list).
Soil/Sediment Samples
Field Method
See "Cyanides," Appendix B.
A-98
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Water Samples
Field Method
See "Cyanides," Appendix B.
Air Samples
Laboratory Method
See "Cyanides," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Cyanides," Appendix B.
Water Samples
Laboratory Method
See "Substituted Nitriles and Tetranitromethane," Appendix B.
A-99
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CYANOGEN CHLORIDE (CAS Number 506-77-4)
RQ: 4.54 kg
SAFETY INFORMATION; Highly toxic (inhalation and injestion).
Air Samples
Field Method
METHOD SUMMARY:
Analysis for cyanogen chloride in air may be performed by use of a detec-
tor tube. A 0.1- to 2-liter sample is collected and analyzed with a hand-
operated bellows pump and a cyanogen chloride gas detector tube (Draeger® CH
19801 or equivalent). A positive result is indicated by a color change in the
tube from white to pink.
INTERFERENCES:
High concentrations of cyanogen bromide will cause a brownish to pink
color change.
QUALITY CONTROL;
No quality control procedures are given.
SENSITIVITY:
This method is sensitive to concentration levels of approximately 0.5 to
15 milligrams per cubic meter.
REFERENCES:
Snyder, R. E.; Jonkin, M. E.; McKissick, A. M. Development of Hazardous Toxic
Wastes Analytical Screening Procedures; Atlantic Research Corporation for U.S.
Army Medical Research and Development Command: Fort Detrick, Maryland, July 16,
1982, p. 4.
National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations
and Technical Gas Analysis with Draeger® Tubes", 4th ed.; Draeger: Pittsburgh,
August 1979.
National Draeger®, Inc., Bulletin No. ND-105; Draeger: Pittsburgh, January 1,
1982.
National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit
Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e;
Draeger: Pittsburgh, December 1981.
A-100
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COST INFORMATION:
The cost per sample for analysis by this method is approximately $13-20
(list).
Soil/Sediment Samples
Field Method
See "Cyanides," Appendix B.
Water Samples
Field Method
METHOD SUMMARY:
Cyanogen chloride in water samples can be measured spectrophotometrically.
Phosphate buffer and pyridine-barbituric acid reagent are added to the water
sample, and the color is read at 578 nm. The analysis should be conducted
immediately after sampling, since cyanogen chloride is volatile and labile.
This method may involve hazardous materials and operations.
INTERFERENCES:
Substances that create color or turbidity may interfere.
QUALITY CONTROL:
No quality control procedures are given.
SENSITIVITY:
The limit of detection is 0.005 milligrams of cyanide ion per liter.
REFERENCE:
American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.02, D4165-82; ASTM: Philadelphia, 1983, pp. 132-135.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $20 (list).
See also: "Cyanides," Appendix B.
Air Samples
Laboratory Method
See "Chlorides," Appendix B.
See "Cyanides," Appendix B.
A-101
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Soil/Sediment Samples
Laboratory Method
See "Cyanides," Appendix B.
Water Samples
Laboratory Method
See "Chlorides," Appendix B.
See "Cyanides," Appendix B.
A-102
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DICHLOROPHENYLARSINE (CAS Number 696-28-6)
RQ: 0.454 kg
SAFETY INFORMATION: Exhibits toxicity (skin). Potentially carcinogenic.
Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Arsines," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Arsenic," Appendix B.
Water Samples
Laboratory Method
See "Arsenic," Appendix B,
A-103
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DIETHYLARSINE (CAS Number 692-42-2)
RQ: 0.454 kg
SAFETY INFORMATION: Pyrophorlc. Potentially carcinogenic. Potentially
chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Arsines," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Arsenic," Appendix B.
Water Samples
Laboratory Method
See "Arsenic," Appendix B,
A-104
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FERRIC AMMONIUM CITRATE (CAS Number 1185-57-5)
RQ: 454 kg
SAFETY INFORMATION:
Air Samples
Field Method
See "Iron Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Iron," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Iron," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Iron," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Ammonia," Appendix B.
See "Iron," Appendix B.
A-105
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FERRIC AMMONIUM OXALATE (CAS Numbers 55488-87-4, 2944-67-4)
RQ: 454 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Iron Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Iron," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Iron," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Iron," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Ammonia," Appendix B.
See "Iron," Appendix B.
A-106
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FERRIC CHLORIDE (CAS Number 7705-08-0)
RQ: 454 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Iron Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Halides, Cyanides, and Other Compounds," Appendix B.
See "Iron," Appendix B.
Air Samples
Laboratory Method
See "Chlorides," Appendix B.
See "Iron," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Iron," Appendix B.
Water Samples
Laboratory Method
See "Chlorides," Appendix B.
See "Iron," Appendix B.
A-107
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FERRIC DEXTRAN (CAS Number 9004-66-4)
RQ; 0.454 kg
SAFETY INFORMATION; Potentially toxic,
Air Samples
Field Method
See "Iron Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
See "Iron," Appendix B.
See "Iron," Appendix B.
See "Iron," Appendix B.
See "Iron," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
A-108
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FERRIC FLUORIDE (CAS Number 7783-50-8)
RQ: 45.4 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Fluorides," Appendix B.
See "Iron Compounds (Particulate)." Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Fluorides," Appendix B.
See "Fluorides and Other Compounds," Appendix B.
See "Iron," Appendix B.
Air Samples
Laboratory Method
See "Fluorides," Appendix B.
See "Fluorides and Hydrogen Fluoride," Appendix B.
See "Iron," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Iron," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Fluorides," Appendix B.
See "Iron," Appendix B.
A-109
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FERRIC NITRATE (CAS Number 10421-48-4)
RQ: 454 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Iron Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Iron," Appendix B.
See "Nitrate Ions," Appendix B.
Air Samples
Laboratory Method
See "Iron," Appendix B.
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Iron," Appendix B.
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
See "Iron," Appendix B.
See "Nitrates," Appendix B.
A-110
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FERRIC SULFATE (CAS Number 10028-22-5)
RQ: 454 kg
SAFETY INFORMATION:
Air Samples
Field Method
See "Iron Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
See "Iron," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Iron," Appendix B.
See "Nitrates and Sulfates," Appendix B.
See "Sulfates (Particulate)," Appendix B.
See "Sulfur Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Iron," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
See "Iron," Appendix B.
See "Sulfates," Appendix B.
A-lll
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FERROUS AMMONIUM SULFATE (CAS Number 10045-89-3)
RQ: 454 kg
SAFETY INFORMATION:
Air Samples
Field Method
See "Iron Compounds (Particulate)." Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Iron," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Iron," Appendix B.
See "Nitrates and Sulfates," Appendix B.
See "Sulfur Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Iron," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Iron," Appendix B.
See "Sulfates," Appendix B.
A-112
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FERROUS CHLORIDE (CAS Number 7758-94-3)
RQ: 45.4 kg
SAFETY INFORMATION:
Air Samples
Field Method
See "Iron Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Halides, Cyanides, and Other Compounds," Appendix B,
See "Iron," Appendix B.
Air Samples
Laboratory Method
See "Chlorides," Appendix B.
See "Iron," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Iron," Appendix B.
Water Samples
Laboratory Method
See "Chlorides," Appendix B.
See "Iron," Appendix B.
A-113
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FERROUS SULFATE (CAS Numbers 7720-78-7, 7782-63-0)
RQ: 454 kg
SAFETY INFORMATION:
Air Samples
Field Method
See "Iron Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
See "Iron," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Iron," Appendix B.
See "Nitrates and Sulfates," Appendix B.
See "Sulfates (Particulate)," Appendix B.
See "Sulfur Compounds (Particulate)," Appendix B,
Soil/Sediment Samples
Laboratory Method
See "Iron," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
See "Iron," Appendix B.
See "Sulfates," Appendix B.
A-114
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FLUORINE (CAS Number 7782-41-4)
RQ: 4.54 kg
SAFETY INFORMATION: Strong oxidizer capable of Igniting substances and sustaining
combustion.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Reacts with water-
Water Samples
Field Method
Reacts with water.
Air Samples
Laboratory Method
METHOD SUMMARY:
Molecular fluorine in air samples can be determined electrochemically. The
air sample is passed through a bubbler containing lithium chloride solution.
The bubbler is part of a unit that acts as a reaction cell. The current gener-
ated by the cell when fluorine passes through is measured amperometrically, and
is proportional to the concentration of the fluorine.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
Calibration is limited to measurements of the sampling pump flow rate.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. No specific precision and accuracy data
are supplied, although a general statement is furnished.
A-115
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REFERENCE;
Kaye, S.; Griggs, M. "Electroanalytical Determination of Molecular Fluorine in
the Atmosphere," Anal. Chem., 40(14), 1968, pp. 2217-2218.
COST INFORMATION;
Cost information has not been obtained.
Soil/Sediment Samples
Laboratory Method
Reacts with water.
Water Samples
Laboratory Method
Reacts with water.
A-116
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HYDRAZINE (CAS Number 302-01-2)
RQ: 0.454 kg
SAFETY INFORMATION: Explosion hazard. Potentially carcinogenic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Hydrazines and Other Compounds," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Hydrazines and Other Compounds," Appendix B.
Air Samples
Laboratory Method
METHOD SUMMARY:
Colorimetry may be used for the analysis of hydrazine in air samples. A
known volume of air is drawn through a bubbler containing 0.1 M hydrochloric
acid. The resulting solution is made alkaline with 1.2 M sodium hydroxide and
reacted with £-dimethylaminobenzaldehyde. Glacial acetic acid is added,
followed by colorimetric analysis at 480 nm.
INTERFERENCES:
Hydrazine derivatives can interfere with the analysis.
QUALITY CONTROL:
A method blank should be processed with each 10 samples.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH), and validated over the range of 0.6 to 3.4 milligrams per
cubic meter. Precision and accuracy information is furnished.
A-117
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REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set Q, Method S237; PB-258 435 (NTIS), U.S. DHEW: Cincinnati, September 1976.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 3, Method S237; Publication No. 77-157-C, U.S. DHEW:
Cincinnati, 1977.
COST INFORMATION:
The cost per sample for analysis by this method is approximately $20-25
(list), plus sampling costs.
See also: "Hydrazines," Appendix B.
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
METHOD SUMMARY:
Hydrazine in water samples can be determined by gas chromatography with
nitrogen/phosphorus detection (GC/NPD). The sample is treated with an excess
of acetone to form acetone azine and is extracted three times with methylene
chloride. The extract is dried with sodium sulfate, concentrated, and an
aliquot is injected into the GC.
INTERFERENCES:
Aldehydes and unsymmetrical ketones can react with hydrazine to form syn-
and anti-isomers that can cause interferences with each other.
QUALITY CONTROL;
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Accuracy information is furnished. This
method is sensitive to concentration levels of hydrazine as low as 0.1 micro-
grams per liter of sample.
REFERENCE;
Selim, S.; Warner, C. R. "Residue Determination of Hydrazine in Water by
Derivatization and Gas Chromatography," J. Chromatogr., 166, 1978, pp. 507-511.
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COST INFORMATION:
Cost per sample for analysis by this method is approximately $175-215
(list).
A-119
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HYDROCHLORIC ACID (CAS Number 7647-01-0)
RQ: 2270 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
METHOD SUMMARY:
Analysis for hydrochloric acid in air may be performed by use of a
detector tube. A 1-liter air sample is collected with a hand-operated bellows
pump and analyzed with a hydrochloric acid gas detector tube (Draeger® CH
29501 or equivalent). A positive result is indicated by a color change
in the tube from blue to yellow.
INTERFERENCES:
A very high relative humidity may cause the hydrochloric acid determina-
tion to be low. Chlorine will produce a pale blue discoloration, but it will
still be possible to measure the hydrochloric acid concentration.
QUALITY CONTROL:
No quality control procedures are given.
SENSITIVITY:
This method is sensitive to concentration levels of approximately 1.5 to
15 milligrams per cubic meter.
REFERENCES:
National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations
and Technical Gas Analysis with Draeger® Tubes", 4th ed.; Draeger: Pittsburgh,
August 1979.
National Draeger, Inc., Bulletin No. ND-105; Draeger: Pittsburgh, January 1,
1982.
National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit
Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e;
Draeger: Pittsburgh, December 1981.
COST INFORMATION:
The cost per sample for analysis by this method is approximately $13-20
(list).
A-120
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See also: "Inorganic Acids," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Fluorides and Other Compounds," Appendix B.
Air Samples
Laboratory Method
METHOD SUMMARY;
Analysis for hydrochloric acid in air can be performed by collection of
the analyte from a known volume of air, using a midget bubbler charged with a
sodium acetate solution, followed by analysis of the resulting solution with a
chloride ion-specific electrode. This method is not specific to hydrogen
chloride, but measures all chlorides.
INTERFERENCES:
Bromide, iodide, and cyanide ions can interfere. High concentrations of
silver-complexing ligands (e.g. thiosulfate, ammonia) can interfere. The
presence of sulfide can poison the electrode, and sulfide ions must therefore
be removed by addition of cadmium carbonate.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH), has been evaluated and reviewed by that agency, and validated
over the range of 3.5 to 14 milligrams per cubic meter in a 15-liter sample.
Precision and accuracy information is furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set R, Method S246, PB-262 403 (NTIS). U.S. DHEW: Cincinnati, December 1976.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 3, Method S246; Publication No. 77-157-C, U.S. DHEW:
Cincinnati, 1977.
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COST INFORMATION;
The cost per sample for analysis by this method is approximately $15, plus
sampling costs.
Note: NIOSH Method P&CAM 310 (silica tube collection, eluent desorption,
analyses by ion chromatography) is applicable. (Reference furnished by
reviewer.)
See also: "Inorganic Acids," Appendix B.
See also: "Chlorides," Appendix B.
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
See "Chlorides," Appendix B.
A-122
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HYDROGEN CYANIDE (CAS Number 74-90-8)
RQ: 4.54 kg
SAFETY INFORMATION: Exhibits high toxicity (oral inhalation). Releases toxic
cyanide ion in water. Flash point -17.7°C (0°F).
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
METHOD SUMMARY:
Analysis for hydrogen cyanide in air may be performed by use of a detector
tube. A 0.5-liter air sample is collected and analyzed with a hand-operated
bellows pump and a hydrocyanic acid gas detector tube (Draeger® CH 25701 or
equivalent). A positive result is indicated by a color change in the tube from
yellow to red. The method is based on liberation of hydrochloric acid from
mercuric chloride, and subsequent reaction of the hydrochloric acid with methyl
red.
INTERFERENCES:
Both acidic and basic interfering gases (hydrogen sulfide, hydrogen
chloride, sulfur dioxide, nitrogen dioxide, and ammonia) are retained in the
precleanse layer of the tube and will not affect the hydrogen cyanide
determination.
QUALITY CONTROL:
No quality control procedures are given.
SENSITIVITY:
This method is senesitve to concentration level of approximately 2 to 35
milligrams per cubic meter.
REFERENCES:
Snyder, R. E.; Jankin, M. E.; McKissick, A. M. Development of Hazardous Toxic
Wastes Analytical Screening Procedures, Atlantic Research Corporation for U.S.
Army Medical Research and Development Command, Fort Detrick, Maryland, July 16,
1982, p. 4.
National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations
and Technical Gas Analysis with Draeger® Tubes", 4th ed.; Draeger: Pittsburgh,
August 1979.
National Draeger, Inc., Bulletin No. ND-105; Draeger: Pittsburgh, January 1,
1982.
A-123
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National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit
Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; Draeger:
Pittsburgh, December 1981.
COST INFORMATION:
The cost per sample for analysis by this method is approximately $13-20
(list).
See also: "Fumigants," Appendix B.
Soil/Sediment Samples
Field Method
See "Cyanides," Appendix B.
Water Samples
Field Method
See "Cyanides," Appendix B.
See "Halides," Appendix B.
See "Halides, Cyanides, and Other Compounds," Appendix B.
Air Samples
Laboratory Method 1
METHOD SUMMARY:
Infrared absorption spectrometry can be used to determine the concentration
of hydrogen cyanide in air samples. The absorbance at 3000 nm (3333 cm"*) is
measured, using a 10-meter pathlength cell. Air can be sampled in a Saran® or
Mylar® plastic bag and approximately 5 liters of the sample drawn into an
evacuated cell. Continuous monitoring of air flowing through the cell is
possible if the spectrometer is set to one particular wavelength. Some vapors
can be adsorbed on silica gel and quantitatively desorbed into the absorption
cell later. Tentative qualitative identification of compounds can be made
based on a full infrared absorption spectrum.
INTERFERENCES:
Compounds present in the sample that absorb infrared radiation at the
wavelength of interest will interfere.
QUALITY CONTROL:
No quality control procedures are given.
A-124
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EPA/TECHNICAL STATUS:
This method is not EPA-approved. The sensitivity of the method, using a
10-meter pathlength cell, is 50 milligrams per cubic meter or 50 parts per
million. No precision or accuracy information is furnished.
REFERENCE:
American Public Health Association, "Infrared Absorption Spectroscopy," In
Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; American Public
Health Association: Washington, 1977, pp. 79-84.
COST INFORMATION:
The cost per sample for analysis by this method is approximately $75-
85 (list), plus sampling costs.
Air Samples
Laboratory Method 2
METHOD SUMMARY;
Hydrogen cyanide in air samples can be measured using an ion selective
electrode. A known volume of air is drawn through a sodium hydroxide-charged
tube, then the analyte is desorbed. Alternatively, the sample may be passed
through a filter and midget bubbler containing 0.1 N potassium hydroxide, which
is later diluted. The resulting solution is analyzed with a cyanide ion selec-
tive electrode.
INTERFERENCES:
Sulfide ions irreversibly poison the electrode and must be removed if
present in the sample. Some halogen and metal ions may interfere.
QUALITY CONTROL:
A blank should be processed with every 10 samples. Recovery and blank
corrections should be included in the calculations.
EPA/TECHNICAL STATUS:
The filter/bubbler method is approved by the National Institute for
Occupational Safety and Health (NIOSH), and validated over the range of 5.2 to
21.0 milligrams per cubic meter, using a 12-liter sample. The sodium hydroxide-
charged tube method is sensitive to levels above approximately 500 micrograms
per cubic meter. Precision and accuracy information is furnished.
A-125
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REFERENCES;
Cadoff, B. C.; Taylor, J. K. Development of a Solid Sorption Tube and
Analytical Procedures for Hydrogen Cyanide in the Workplace Atmosphere, PB-253
228, (NTIS), U.S. Department of Health, Education, and Welfare: Cincinnati,
1976.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 4, Method S288; Publication No. 78-175, U.S. DHEW:
Cincinnati, August 1978.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $25 (list),
plus sampling costs.
Soil/Sediment Samples
Laboratory Method
See "Cyanides," Appendix B.
Water Samples
Laboratory Method
See "Cyanides," Appendix B.
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HYDROGEN FLUORIDE (CAS Number 7664-39-3)
RQ: 45.4 kg
SAFETY INFORMATION: Exhibits acute and chronic toxicity.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
METHOD SUMMARY;
Analysis for hydrogen fluoride in air may be performed by use of a detec-
tor tube. A 2-liter air sample is collected with a hand-operated bellows pump
and analyzed with a hydrogen fluoride gas detector tube (Draeger® CH 30301 or
equivalent). A positive result is indicated by a color change in the tube from
pale blue to pale pink. This method is based on the formation of quinalizarin
from a zirconium hydroxide and 1,2,5,8-tetrahydroxyanthraquinone lake and
hydrogen fluoride.
INTERFERENCES:
A high relative atmospheric humidity may cause the hydrogen fluoride
determination to be low.
QUALITY CONTROL;
No quality control procedures are given.
SENSITIVITY:
This method is sensitive to concentration levels of approximately 1 to 15
milligrams per cubic meter.
REFERENCES:
National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations
and Technical Gas Analysis with Draeger® Tubes", 4th ed.: Draeger: Pittsburgh,
August 1979.
National Draeger, Inc., Bulletin No. ND-105; Draeger: Pittsburgh, January 1,
1982.
National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit
Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; Draeger:
Pittsburgh, December 1981.
A-127
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COST INFORMATION;
The cost per sample for analysis by this method is approximately $13-20
(list).
See also; "Fluorides," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Fluorides and Other Compounds," Appendix B.
Air Samples
Laboratory Method
METHOD SUMMARY:
Analysis for hydrogen fluoride in air is performed by passage of 45 liters
of air through a midget bubbler containing 0.1 N sodium hydroxide, followed by
sample dilution with Total Ionic Strength Activity Buffer (TISAB) and analysis
of the resulting solution for fluoride ions with a fluoride ion specific elec-
trode. This method is not specific for hydrogen fluoride, but measures the
total fluoride content of the sample.
INTERFERENCES:
Very high amounts of fluoride-complexing metals can interfere with the
analysis.
QUALITY CONTROL;
A method blank must be processed and results adjusted accordingly.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH), and validated over the range of 1.3 to 4.5 milligrams per
cubic meter in a 45-liter sample. Precision and accuracy information is
furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set L, Method S176; PB-250 159 (NTIS), U.S. DHEW: Cincinnati, January 1976.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, Method P&CAM 117; Publication No. 75-121, U.S. DHEW: Cincinnati, 1974.
A-128
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U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 117; Publication No. 77-157-A, U.S.
DREW: Cincinnati, 1977.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 3, Method S176; Publication No. 77-157-C, U.S. DHEW:
Cincinnati, 1977.
COST INFORMATION:
Cost per sample for analysis by this method is $10-20 (list), plus sampling
costs.
See also: "Fluorides," Appendix B.
See also: "Fluorides and Hydrogen Fluoride," Appendix B.
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
See "Fluorides," Appendix B.
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HYDROGEN SULFIDE (CAS Number 7783-06-4)
RQ: 45.4 kg
SAFETY INFORMATION; Flammable gas. Toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method 1
METHOD SUMMARY:
Analysis for hydrogen sulfide in air may be performed by use of a detector
tube. A 0.1- to 1-liter air sample is collected and analyzed with a hand-
operated bellows pump and a hydrogen sulfide gas detector tube (Draeger® 67
19001 or equivalent). A positive result is indicated by a color change in the
tube from white to pale brown. The method is based on the formation of lead
sulfide.
INTERFERENCES:
High concentrations of sulfur dioxide may cause the hydrogen sulfide deter-
mination to be too high, although sulfur dioxide alone will not discolor the
tube.
QUALITY CONTROL:
No quality control procedures are given.
SENSITIVITY:
This method is sensitive to concentration levels of approximately 1 to 300
milligrams per cubic meter for the prescribed sample size.
REFERENCES:
National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations
and Technical Gas Analysis with Draeger® Tubes", 4th ed.; Draeger: Pittsburgh,
August 1979.
National Draeger, Inc., Bulletin No. ND-105; Draeger: Pittsburgh, January 1,
1982.
National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit
Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; Draeger:
Pittsburgh, December 1981.
COST INFORMATION;
The cost per sample for analysis by this method is approximately $13-20
(list).
A-130
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Air Samples
Field Method 2
METHOD SUMMARY:
Analysis for hydrogen sulfide in air can be performed by photorateometric
analysis, which utilizes the color developed from the reaction of hydrogen
sulfide with lead acetate-impregnated paper to indicate the concentration of
hydrogen sulfide in air.
INTERFERENCES;
There are no reported interferences.
QUALITY CONTROL:
No quality control procedures are given.
SENSITIVITY:
The method is sensitive to one part per billion hydrogen sulfide and
requires use of an electrical monitoring device [Model 825 R-d Rateometric
Analyzer, Houston Atlas, Inc., Houston, Texas].
REFERENCE:
Kimbell, C. L. "Atmospheric Monitoring for Hydrogen Sulfide by Photorateometric
Analysis" In Toxic Materials in the Atmosphere, STP-786, American Society for
Testing and Materials: Philadelphia, 1981, pp. 60-69.
COST INFORMATION:
The cost per sample for analysis by this method is approximately $8 (list),
plus sampling costs.
See also; "Organic Vapors," Appendix B.
Soil/Sediment Samples
Field Method
See "Sulfides," Appendix B.
Water Samples
Field Method
See "Sulfides," Appendix B.
A-131
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Air Samples
Laboratory Method 1
METHOD SUMMARY:
Analysis for hydrogen sulfide in air can be performed spectrophotometri-
cally. Two liters of air are aspirated through an aqueous cadmium hydroxide
suspension, to which Stractan 10® is added to minimize photo-decomposition.
The collected sulfide is determined by spectrophotometric measurement of the
methylene blue produced by the reaction of the sulfide with N,N-dimethyl-p-
phenylenediamine and ferric chloride.
INTERFERENCES:
Strong reducing agents (e.g. sulfur dioxide) inhibit color development.
High concentrations of nitrogen dioxide interfere, and ozone can cause a nega-
tive interference.
QUALITY CONTROL:
A method blank should be analyzed with each set of samples.
EPA/TECHNICAL STATUS;
This method is approved by the National Institute of Occupational Safety
and Health (NIOSH), and validated over the range of 8.5 to 63 milligrams per
cubic meter in 2 liters of air. Precision and accuracy information is fur-
nished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set A. Method S4; PB-245 850 (NTIS), U.S. DHEW: Cincinnati, October 1975.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 2, Method S4; Publication No. 77-157-B, U.S. DHEW:
Cincinnati, 1977.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 126; Publication No. 77-157-A, U.S. DHEW:
Cincinnati, 1977.
COST INFORMATION:
Cost information has not been obtained.
See also: "Sulfur-Containing Gases," Appendix B.
A-132
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Air Samples
Laboratory Method 2
METHOD SUMMARY:
Hydrogen sulfide in air samples can be measured by gas chromatography- A
known volume of air is drawn through a desiccant tube, then through a tube
containing molecular sieve that traps the hydrogen sulfide. The hydrogen
sulfide is released by thermal desorption, and the sample is analyzed by gas
chromatography with flame photometric detection (GC/FPD).
INTERFERENCES:
Humidity interferes, but its effect is eliminated by use of the desiccant
tube. Any sulfur-containing compound with the same retention time as hydrogen
sulfide can interfere.
QUALITY CONTROL:
Since no internal standard is used in this method, standard gases must be
analyzed at the same time the sample analysis is done.
EPA/TECHNICAL STATUS:
This method is proposed by the National Institute for Occupational Safety
and Health (NIOSH) for use over the range of 15 to 60 milligrams per cubic
meter for a 5-liter air sample. Precision and accuracy information is
furnished.
REFERENCE:
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods, Vol. 6, Method P&CAM 296; Publication No. 80-125, U.S. DHHS:
Cincinnati, August 1980.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $100-120
(list), plus sampling costs.
See also: "Sulfur-Containing Gases," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Sulfides," Appendix B.
Water Samples
Laboratory Method
See "Sulfides," Appendix B.
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RQ: 0.454 kg
SAFETY INFORMATION:
LEAD (CAS Number 7439-92-1)
Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Lead and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
See "Lead," Appendix B.
See "Lead," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Lead," Appendix B.
See "Lead and Cadmium," Appendix B.
See "Lead," Appendix B.
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
See "Lead," Appendix B.
A-134
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LEAD ACETATE (CAS Number 301-04-2)
RQ: 2270 kg
SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Lead and Compounds (Particulate)," Appendix B.
See "Lead," Appendix B.
See "Lead," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Lead," Appendix B.
See "Lead and Cadmium," Appendix B.
See "Lead," Appendix B.
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
See "Acid Anions," Appendix B,
See "Lead," Appendix B.
A-135
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LEAD ARSENATE (CAS Numbers 7784-40-9, 7645-25-2, 10102-48-4)
RQ: 2270 kg
SAFETY INFORMATION; Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Lead and Compounds (Particulate)." Appendix B.
Soil/Sediment Samples
Field Method
See "Arsenic," Appendix B,
See "Lead," Appendix B.
Water Samples
Field Method
See "Lead," Appendix B.
Air Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Lead," Appendix B.
See "Lead and Cadmium," Appendix B
Soil/Sediment Samples
Laboratory Method
See "Arsenic," Appendix B,
See "Lead," Appendix B.
Water Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Lead," Appendix B.
A-136
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LEAD CHLORIDE (CAS Number 7758-95-4)
RQ: 2270 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Lead and Compounds (Particulate)," Appendix B.
See "Lead," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Halides, Cyanides, and Other Compounds," Appendix B.
See "Lead," Appendix B.
Air Samples
Laboratory Method
See "Chlorides," Appendix B.
See "Lead," Appendix B.
See "Lead and Cadmium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Lead," Appendix B.
Water Samples
Laboratory Method
See "Chlorides," Appendix B.
See "Lead," Appendix B.
A-137
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LEAD FLUOBORATE (CAS Number 13814-96-5)
RQ: 2270 kg
SAFETY INFORMATION; Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Lead and Compounds (Particulate)," Appendix B.
See "Lead," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
METHOD SUMMARY:
Field analysis for lead fluoborate in water samples can be performed by
colorimetric analysis for boron. A 2-milliliter sample is treated with concen-
trated sulfuric acid and a carmine color reagent, and the intensity of the
resulting bluish-red or blue color is measured with a portable spectrophotom-
eter at 585 nm.
INTERFERENCES:
No specific interferences are given. With this method no specific boron-
containing compound can be identified, only the total boron content of the
sample is determined.
QUALITY ASSURANCE:
No quality assurance procedures are given.
SENSITIVITY:
The method is applicable to concentrations above approximately 5 milligrams
per liter.
REFERENCE:
Hach Chemical Co., Procedures, Chemical Lists and Glassware for Water and
Wastewater Analysis, 2nd ed.; Hach: Ames, Iowa, 1978, pp. 2-19. 2-20.
A-138
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COST INFORMATION:
The cost per sample for analysis by this method is approximately $25-40
(list).
See also; "Lead," Appendix B,
Air Samples
Laboratory Method
See "Lead," Appendix B.
See "Lead and Cadmium," Appendix B,
Soil/Sediment Samples
Laboratory Method
METHOD SUMMARY;
Soil/sediment samples may be analyzed for lead fluoborate by inductively
coupled plasma atomic spectrometry (ICP) or colorimetric analysis for boron. A
2-gram sample is digested with nitric acid and hydrogen peroxide and analyzed.
For colorimetric analysis, 1 milliliter of the digested sample is acidified and
evaporated in the presence of curcumin, and the resultant color is measured
photometrically. These methods are not specific for lead fluoborate, but
the total boron concentration of the sample is measured.
INTERFERENCES:
High concentrations of calcium and magnesium compounds in the sample may
make it necessary to pass the sample through a cation exchange resin.
QUALITY CONTROL;
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods when
using ICP- Using either method, a reference standard should be analyzed weekly
and at least 10 percent of the analyses should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for the
National Pollutant Discharge Elimination System (NPDES). Precision and
accuracy information is furnished.
REFERENCES:
U.S. Environmental Protection Agency Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media. Exhibit D, Invitation for Bid
(Solicitation Number WA 82-A072), U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency Methods for Chemical Analysis of Water and
Wastes Method 212.3; EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979.
A-139
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U.S. Environmental Protection Agency Technical Additions to Methods for
Chemical Analyses of Water and Wastes, Method 200.7; EPA-600/4-82-055, U.S.
EPA: Washington, 1982.
Federal Register, 44- (233), December 3, 1979, pp. 69559-69564.
COST INFORMATION:
Cost per sample for analysis by ICP is approximately $20 (list): by the
colorimetric method, it is approximately $35-45 (list).
See also; "Lead," Appendix B.
Water Samples
Laboratory Method
METHOD SUMMARY:
Colorimetric analysis or inductively coupled plasma atomic spectrometric
(ICP) analysis for boron may be used to analyze water samples for lead
fluoborate. A 100-milliliter sample is digested with nitric acid and hydrogen
peroxide and analyzed. For colorimetric analysis, 1 milliliter of the digested
sample is acidified and evaporated in the presence of curcumin and the resul-
tant color is measured photometrically. These methods are not specific for
lead fluoroborate, but the total boron content of the sample is weighed.
INTERFERENCES:
Total calcium and magnesium hardness exceeding 100 milligrams per liter
as calcium carbonated may make it necessary to pass the sample through a cation
exchange resin.
QUALITY CONTROL:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods.
Using either method, a reference standard should be analyzed weekly and at
least 10 percent of the analyses should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program and are approved for the
National Pollutant Discharge Elimination System (NPDES). Precison and accuracy
information is furnished.
REFERENCES;
U.S. Environmental Protection Agency, Chemical Analytical Services for Low and
Medium Concentration Inorganics in All Media, Exhibit D; Invitation for Bid
(Solicitation Number, WA 82-A072), U.S. EPA: Washington, April 23, 1982.
A-140
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U.S. Environmenal Protection Agency, Methods for Chemical Analysis of Water and
Wastes, Method 212.3: EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
U.S. Environmental Protection Agency Technical Additions to Methods for
Chemical Analyses of Water and Wastes, Method 200.7; EPA-600/4-82-055, U.S.
EPA: Washington, 1982.
Federal Register, 44_ (233), December 3, 1979, pp. 69559-69564.
COST INFORMATION:
Cost per sample for analysis by ICP is approximately $10 (list); by the
colorimetric method, it is approximately $35-40 (list).
See also; "Lead," Appendix B.
A-141
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LEAD FLUORIDE (CAS Number 7783-46-2)
RQ: 454 kg
SAFETY INFORMATION; Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Fluorides," Appendix B.
See "Lead and Compounds (Particulate)," Appendix B.
See "Lead," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Fluorides and Other Compounds," Appendix B.
See "Lead," Appendix B.
Air Samples
Laboratory Method
See "Fluorides," Appendix B.
See "Fluorides and Hydrogen Fluoride," Appendix B.
See "Lead," Appendix B.
See "Lead and Cadmium," Appendix B.
See "Lead," Appendix B.
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
See "Fluorides," Appendix B.
See "Lead," Appendix B.
A-142
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LEAD IODIDE (CAS Number 10101-63-0)
RQ: 2270 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Lead and Compounds (Particulate)," Appendix B.
See "Lead," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Halides, Cyanides, and Other Compounds," Appendix B.
See "Lead," Appendix B.
Air Samples
Laboratory Method
See "Lead," Appendix B.
See "Lead and Cadmium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Lead," Appendix B.
Water Samples
Laboratory Method
See "Lead," Appendix B.
See "Iodides and Bromides," Appendix B.
A-143
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LEAD NITRATE (CAS Number 10099-74-8)
RQ: 2270 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Lead and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
See "Lead," Appendix B.
Water Samples
Field Method
See "Lead," Appendix B.
See "Nitrate Ions," Appendix B.
Air Samples
Laboratory Method
See "Lead," Appendix B.
See "Lead and Cadmium," Appendix B.
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Lead," Appendix B.
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
See "Lead," Appendix B.
See "Nitrates," Appendix B.
A-144
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LEAD PHOSPHATE (CAS Number 7446-27-7)
RQ: 0.454 kg
SAFETY INFORMATION; Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Lead and Compounds (Particulate)," Appendix B.
See "Lead," Appendix B.
See "Lead," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Lead," Appendix B.
See "Lead and Cadmium," Appendix B.
See "Phosphorus," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Lead," Appendix B.
See "Phosphorus," Appendix B,
Water Samples
Laboratory Method
See "Lead," Appendix B.
See "Phosphorus," Appendix B.
A-145
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LEAD STEARATE (CAS Numbers 7428-48-0, 1072-35-1, 56189-09-4)
RQ: 2270 kg
SAFETY INFORMATION; Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Lead and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
See "Lead," Appendix B.
See "Lead," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Lead," Appendix B.
See "Lead and Cadmium," Appendix B.
See "Lead," Appendix B.
See "Lead," Appendix B.
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
A-146
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RQ: 0.454 kg
SAFETY INFORMATION:
LEAD SUBACETATE (CAS Number 1335-32-6)
Potentially carcinogenic. Potentially chronially toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Lead and Compounds (Particulate)." Appendix B.
See "Lead," Appendix B.
See "Lead," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Lead," Appendix B.
See "Lead and Cadmium," Appendix B.
See "Lead," Appendix B.
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
See "Lead," Appendix B.
A-147
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LEAD SULFATE (CAS Numbers 15739-80-7, 7446-14-2)
RQ: 2270 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Lead and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
See "Lead," Appendix B.
See "Lead," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Lead," Appendix B.
See "Lead and Cadmium," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Lead," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
See "Lead," Appendix B.
A-148
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LEAD SULFIDE (CAS Number 1314-87-0)
RQ: 2270 kg
SAFETY INFORMATION: Forms toxic I^S when in contact with acids. Potentially
chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Lead and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
See "Lead," Appendix B.
See "Sulfides," Appendix B.
Water Samples
Field Method
Insoluble in water-
Air Samples
Laboratory Method
METHOD SUMMARY:
Lead sulfide in air samples can be measured by X-ray diffraction. A known
volume of air is drawn through a membrane filter. The filter is dissolved in
tetrahydrofuran then redeposited on a silver membrane filter. The filter
samples are scanned qualitatively by X-ray powder diffraction to determine the
presence of lead sulfide. The mass of lead sulfide present is then determined
by measuring the diffraction peak intensity for the analyte and for the silver
filter.
INTERFERENCES:
Using copper Kct X-ray radiation, lead oxide, lead sulfate, and copper iron
sulfide will interfere with the primary lead sulfide peak. Lead oxide and lead
sulfate will also interfere with the secondary lead sulfide peak. The tertiary
lead sulfide peak interferes with the secondary silver peak.
QUALITY CONTROL:
Method blanks and standards are processed along with the samples.
A-149
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EPA/TECHNICAL STATUS;
This is an operational method, as classified by the National Institute for
Occupational Safety and Health (NIOSH), for use over the range of 0.06 to 40
milligrams per cubic meter in a 500-liter sample. Precision and accuracy
information is furnished.
REFERENCE;
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods, Vol. 7, Method P&CAM 350; Publication No. 82-100, U.S. DHHS:
Cincinnati, August 1981.
COST INFORMATION:
Cost information has not been obtained.
See also: "Lead," Appendix B.
See also: "Lead and Cadmium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Lead," Appendix B.
See "Sulfides," Appendix B.
Water Samples
Laboratory Method
Insoluble in water.
A-150
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LEAD THIOCYANATE (CAS Number 592-87-0)
RQ: 2270 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Lead and Compounds (Particulate)," Appendix B.
See "Lead," Appendix B.
See "Lead," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Lead," Appendix B.
See "Lead and Cadmium," Appendix B.
See "Lead," Appendix B,
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
See "Lead," Appendix B.
See "Thiocyanates," Appendix B.
A-151
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RQ: 454 kg
SAFETY INFORMATION:
LITHIUM CHROMATE (CAS Number 14307-35-8)
Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Chromium," Appendix B.
Soil/Sediment Samples
Field Method
See "Chromium," Appendix B.
Water Samples
Field Method
See "Chromates," Appendix B.
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
Air Samples
Laboratory Method
METHOD SUMMARY;
Atomic absorption (AA) spectrometric analysis for lithium may be used to
analyze air samples for lithium chromate. Samples are collected on cellulose
membrane filters. The filter medium is digested with nitric acid and the
digest is diluted and analyzed by AA. This method does not differentiate
between lithium-containing compounds, but measures the total lithium content of
the sample.
INTERFERENCES:
Cesium should be added to samples and standards to control ionization
interference. The method of standard additions and/or background monitoring
may be needed to correct for interferences.
QUALITY CONTROL:
A minimum of 1 filter blank for every 10 filter samples must be analyzed.
Standard solutions should match the sample matrix as closely as possible.
Standards should be analyzed in duplicate.
A-152
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EPA/TECHNICAL STATUS:
This method is classified as operational by the National Institute of
Occupational Safety and Health (NIOSH) for use over the range of 4.2 to 84
micrograms per cubic meter of air in a 240-liter sample. Precision information
is furnished.
REFERENCE:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed.. Vol. 1, Method P&CAM 173; Publication No. 77-157-A, U.S.
DHEW: Cincinnati, 1977.
COST INFORMATION:
The cost per sample for analysis by this method is approximately $10-20
(list), plus sampling costs.
See also: "Chromic Acid and Chromates," Appendix B.
See also: "Chromium," Appendix B.
See also: "Chromium, Hexavalent," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Chromium," Appendix B.
See "Chromium, Hexavalent," Appendix B.
Water Samples
Laboratory Method
See "Chromium," Appendix B.
See "Chromium, Hexavalent," Appendix B.
A-153
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RQ: 0.454 kg
SAFETY INFORMATION:
MERCURIC CYANIDE (CAS Number 592-04-1)
Releases toxic cyanide ions in water. Exhibits chronic
toxicity.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Cyanides," Appendix B.
Water Samples
Field Method
See "Cyanides," Appendix B.
See "Halides, Cyanides, and Other Compounds," Appendix B.
See "Mercury." Appendix B.
Air Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Mercury," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Mercury," Appendix B.
Water Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Mercury," Appendix B.
A-154
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MERCURIC NITRATE (CAS Number 10045-94-0)
RQ: 4.54 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Mercury," Appendix B.
See "Nitrate Ions," Appendix B.
Air Samples
Laboratory Method
See "Mercury," Appendix B.
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Mercury," Appendix B.
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
See "Mercury," Appendix B.
See "Nitrates," Appendix B.
A-155
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MERCURIC SULFATE (CAS Number 7783-35-9)
RQ: 4.54 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Mercury," Appendix B,
Air Samples
Laboratory Method
See "Mercury," Appendix B.
See "Nitrates and Sulfates," Appendix B.
See "Sulfates (Particulate)," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Mercury," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
See "Mercury," Appendix B.
See "Sulfates," Appendix B.
A-156
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MERCURIC THIOCYANATE (CAS Number 592-85-8)
RQ: 4.54 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Mercury," Appendix B.
Air Samples
Laboratory Method
See "Mercury," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Mercury," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Mercury," Appendix B.
See "Thiocyanates," Appendix B.
A-157
-------
MERCUROUS NITRATE (CAS Numbers 7782-86-7, 10415-75-5)
RQ: 4.54 kg
SAFETY INFORMATION; Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Mercury," Appendix B.
Air Samples
Laboratory Method
See "Mercury," Appendix B.
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Mercury," Appendix B.
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
See "Mercury," Appendix B.
See "Nitrates," Appendix B.
A-158
-------
MERCURY (CAS Number 7439-97-6)
RQ: 0.454 kg
SAFETY INFORMATION: Exhibits toxicity (inhalation). Exhibits chronic
toxicity.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
METHOD SUMMARY:
Analysis for mercury vapor in air may be performed by use of a detector
tube. A 0.1- to 2-liter air sample is collected and analyzed with a hand-operated
bellows pump and a mercury vapor detector tube (Draeger® CH 23101 or
equivalent). A positive result is indicated by a color change in the tube
from pale yellowish-grey to pale yellowish-orange. The method is based on
the reaction of mercury with copper(I)iodide to form a copper-mercury complex.
INTERFERENCES:
Chlorine will cause the mercury determination to be low.
QUALITY CONTROL:
No quality control procedures are given.
SENSITIVITY:
This method is sensitive to concentration levels of approximately 0.1 to 2
milligrams per cubic meter.
REFERENCES;
National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations
and Technical Gas Analysis with Draeger® Tubes", 4th ed.; Draeger: Pittsburgh,
August 1979.
National Draeger, Inc., Bulletin No. ND-105; Draeger: Pittsburgh, January 1,
1982.
National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit
Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; Draeger:
Pittsburgh, December 1981.
COST INFORMATION:
The cost per sample for analysis by this method is approximately $13-20
(list).
A-159
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Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Mercury," Appendix B.
Air Samples
Laboratory Method
METHOD SUMMARY:
Mercury in air samples can be measured by cold vapor atomic absorption
(AA) spectrometry. Elemental mercury vapor is collected on silver wool or
silvered Chromosorb P and released by heating. The released mercury is swept
through the absorption cell of an AA spectrometer, and the response at 253.7 nm
is measured. Calibration of the instrument with a series of five standards is
required.
INTERFERENCES:
High levels of chlorine and sulfur dioxide will poison the silver wool. A
tube packed with scarite® placed before the collector will remove the chlorine.
Hydrogen sulfide may interfere.
QUALITY CONTROL;
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH), and validated over the range of 0.046 to 0.18 milligrams
per cubic meter, using a 3-liter sample. The American Public Health Association
considers the procedure applicable to the determination of elemental mercury in
the range of 0.02 to 10.0 micrograms per cubic meter, at a collection flow rate
of 100 to 200 cubic centimeters per minute over a 24-hour period. The limit of
detection is approximately 0.001 microgram mercury. Precision and accuracy
information is furnished.
REFERENCES:
American Public Health Association, Methods of Air Sampling and Analysis, 2nd
ed., M. Katz, Ed.; APHA: Washington, 1977, pp. 488-492.
U.S. Deparment of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 4, Method S199; Publication No. 78-175, U.S. DHEW:
Cincinnati, August 1978.
A-160
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COST INFORMATION;
The cost per sample for analysis by this method is approximately $18-50
(list), plus sampling costs.
See also: "Mercury," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Mercury." Appendix B.
Water Samples
Laboratory Method
See "Mercury," Appendix B.
A-161
-------
MERCURY FULMINATE (CAS Number 628-86-4)
RQ: 0.454 kg
SAFETY INFORMATION: Explosive. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Mercury," Appendix B.
Air Samples
Laboratory Method
See "Mercury," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Mercury," Appendix B.
Water Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Mercury," Appendix B.
A-162
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NICKEL (CAS Number 7440-02-0)
RQ: 0.454 kg
SAFETY INFORMATION: Exhibits toxicity (oral). Potentially carcinogenic.
Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Nickel and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Nickel Ions," Appendix B.
Air Samples
Laboratory Method
See "Nickel," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Nickel," Appendix B.
Water Samples
Laboratory Method
See "Nickel," Appendix B,
A-163
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NICKEL AMMONIUM SULFATE (CAS Number 15699-18-0)
RQ: 2270 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Nickel and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Nickel Ions," Appendix B.
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Nickel," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Nickel," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Nickel," Appendix B.
A-164
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NICKEL CHLORIDE (CAS Numbers 7718-54-9, 37211-05-5)
RQ: 2270 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Nickel and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Halides, Cyanides, and Other Compounds," Appendix B.
See "Nickel Ions," Appendix B.
Air Samples
Laboratory Method
See "Chlorides," Appendix B.
See "Nickel," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Nickel," Appendix B.
Water Samples
Laboratory Method
See "Chlorides," Appendix B.
See "Nickel," Appendix B.
A-165
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NICKEL CYANIDE (CAS Number 557-19-7)
RQ: 4.54 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Nickel and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
See "Cyanides," Appendix B,
Water Samples
Field Method
See "Cyanides," Appendix B.
See "Nickel Ions," Appendix B.
Air Samples
Laboratory Method
See "Cyanides," Appendix B,
See "Nickel," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Nickel," Appendix B.
Water Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Nickel," Appendix B.
A-166
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NICKEL HYDROXIDE (CAS Number 12054-48-7)
RQ: 454 kg
SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic
Air Samples
Field Method
See "Nickel and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Nickel Ions," Appendix B.
Air Samples
Laboratory Method
See "Nickel," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Nickel," Appendix B.
Water Samples
Laboratory Method
See "Nickel," Appendix B,
A-167
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NICKEL NITRATE (CAS Number 14216-75-2)
RQ: 454 kg
SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Nickel and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Nickel Ions," Appendix B.
See "Nitrate Ions," Appendix B.
Air Samples
Laboratory Method
See "Nickel," Appendix B.
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Nickel," Appendix B.
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
See "Nickel," Appendix B.
See "Nitrates," Appendix B.
A-168
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NICKEL SULFATE (CAS Number 7786-81-4)
RQ: 2270 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Nickel and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Nickel Ions," Appendix B.
Air Samples
Laboratory Method
See "Nickel," Appendix B.
See "Nitrates and Sulfates," Appendix B.
See "Sulfates (Particulate)," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Nickel," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
See "Nickel," Appendix B.
See "Sulfates," Appendix B.
A-169
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NICKEL TETRACARBONYL (CAS Number 13463-39-3)
RQ: 0.454 kg
SAFETY INFORMATION; Exhibits toxicity (inhalation). Flash point -4°F.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
METHOD SUMMARY:
Analysis for nickel tetracarbonyl in air may be performed by use of a
detector tube. A 2-liter air sample is collected and analyzed with a hand-
operated bellows pump and a nickel tetracarbonyl gas detector tube (Draeger® CH
19501 or equivalent). A positive result is indicated by a color change in the
tube from pale brown to pink, caused by the reaction of the nickel tetracarbonyl
with iodine and a dioxime compounds.
INTERFERENCES:
Hydrogen sulfide and sulfur dioxide may lower the nickel tetracarbonyl
indication and iron pentacarbonyl may cause a brown discoloration.
QUALITY CONTROL;
No quality control procedures are given.
SENSITIVITY:
This method is sensitive to concentration levels of approximately 1 to 10
milligrams per cubic meter.
REFERENCES:
Snyder, R. E.; Jankin, M. E.; McKissick, A. M. Development of Hazardous Toxic
Wastes Analytical Screening Procedures, Atlantic Research Corporation for U.S.
Army Medical Research and Development Command, Fort Detrick, Maryland, July 16,
1982, p. 4.
National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations
and Technical Gas Analysis with Draeger® Tubes", 4th ed.; Draeger: Pittsburgh,
August 1979.
National Draeger, Inc., Bulletin No. ND-105; Draeger: Pittsburgh, January 1,
1982.
National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit
Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; Draeger:
Pittsburgh, December 1981.
A-170
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COST INFORMATION:
The cost per sample for analysis by this method is approximately $13-20
(list).
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
METHOD SUMMARY:
Atomic absorption spectrometry may be used for the analysis of nickel
tetracarbonyl in air samples. The analysis is performed by passage of a known
volume of air through an acid-washed charcoal-tube sampling device, followed by
desorption of the analyte with dilute nitric acid and analysis of the resulting
solution by graphite furnace atomic absorption spectrometry (AAS).
INTERFERENCES:
Particulate nickel compounds will interfere unless a pre-fliter is used.
QUALITY CONTROL:
Method blanks and standards are processed with the samples.
EPA/TECHNICAL STATUS:
This method is proposed by the National Institute for Occupational Safety
and Health (NIOSH), for use over the range of 2 to 60 micrograms per cubic
meter in an 80-liter sample. Precision and accuracy information is furnished.
REFERENCE:
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods. Vol. 7, Method P&CAM 344; Publication No. 82-100, U.S. DHHS:
Cincinnati, August 1981.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $23-55
(list), plus sampling costs.
See also: "Nickel," Appendix B.
A-171
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Soil/Sediment Samples
Laboratory Method
See "Nickel," Appendix B.
Water Samples
Laboratory Method
See "Nickel," Appendix B.
A-172
-------
NITRIC ACID (CAS Number 7697-37-2)
RQ: 454 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
METHOD SUMMARY:
Analysis for nitric acid in air may be performed by use of a detector
tube. A 1- to 2-liter air sample is collected and analyzed with a hand-
operated bellows pump and a nitric acid gas detector tube (Draeger® 67 28311 or
equivalent). A positive result is indicated by a color change in the tube from
blue to yellow. The test is based on the reaction of nitric acid with bromo-
phenol blue.
INTERFERENCES:
Nitrogen dioxide will also give a positive result.
QUALITY CONTROL:
No quality control procedures are given.
SENSITIVITY:
The tube will measure concentrations of approximately 3 to 130 milligrams
per cubic meter.
REFERENCES:
National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations
and Technical Gas Analysis with Draeger® Tubes", 4th ed.; Draeger: Pittsburgh,
August 1979.
National Draeger, Inc., Bulletin No. ND-105; Draeger: Pittsburgh, January 1,
1982.
National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit
Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; Draeger:
Pittsburgh, December 1981.
COST INFORMATION:
The cost per sample for analysis by this method is approximately $13-20
(list).
A-173
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Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Nitrate Ions," Appendix B.
Air Samples
Laboratory Method 1
METHOD SUMMARY:
Analysis for nitric acid in air can be performed by sampling air through a
47-millimeter nylon filter at 12 liters per minute, followed by analysis of the
filter medium for nitrate ion by ion chromatography (1C). If sampling is
performed at 1 liter per minute and analysis performed by a chemiluminescence
analyzer, the method can be used for continuous monitoring.
INTERFERENCES:
This analysis responds to any nitrate-containing salt trapped on the
filter disc, and is not specific to nitric acid.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
These methods have been evaluated, but are not EPA-approved. Precision
and accuracy information is furnished.
REFERENCES:
Forrest, J; Tamer, R.L; Spandau, D.; D'Ottavio, T.; Newman, L. "Determination
of Total Inorganic Nitrate Utilizing Collection of Nitric Acid on NaCl-
Impregnated Filters," Atmos. Environ.. 14, 1980, pp. 137-144.
Current Methods to Measure Atmospheric Nitric Acid and Nitrate Artifacts,
R. K.Stevens, Ed.; EPA-600/2-79-051, U.S. Environmental Protection Agency:
Research Triangle Park, March 1979.
COST INFORMATION:
The cost per sample for analysis by 1C is approximately $70-80 (list),
plus sampling costs; information about the chemiluminescence method has not
been obtained.
A-174
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Air Samples
Laboratory Method 2
METHOD SUMMARY:
Nitric acid in air samples may be measured by drawing a known volume of
air through a midget impinger containing distilled water, then analyzing the
contents of the impinger by direct potentiometry using a nitrate ion selective
electrode. This method is not specific for nitric acid, but measures the total
concentration of nitrates in the sample.
INTERFERENCES:
Anions, including bromide, chloride, fluoride, iodide, phosphate, and
nitrite, will interfere, but use of a buffer solution removes the interferences.
However, high concentrations of these species should be avoided.
QUALITY CONTROL;
A calibration standard is analyzed before and after each sample to assure
reliable results. A blank should be processed with every 10 samples.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH), and validated over the range of 2.60 to 108 milligrams per
cubic meter, using a 180-liter air sample. Precision and accuracy information
is furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 4, Method S319; Publication No. 78-175, U.S. DHEW:
Cincinnati, August 1978.
Note: NIOSH Method P & CAM 339 (silica get tube collection, elution, analyses
by ion chromatography) is applicable. (Reference provided by reviewer=)
COST INFORMATION:
Cost per sample for analysis by this method is approximately $10-15
(list), plus sampling costs.
See also: "Inorganic Acids," Appendix B.
See also: "Nitrates," Appendix B.
Soil/Sediment Samples
Laboratory Method
A-175
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See "Nitrates," Appendix B.
Water Samples
Laboratory Method
A-176
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NITRIC OXIDE (CAS Number 10102-43-9)
RQ: 4.54 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method 1
METHOD SUMMARY:
Infrared absorption spectrometry can be used to determine the concentration
of nitric oxide in air samples. The absorbance at 5250 nm (1905 cm~l) is
measured, using a 10-meter pathlength cell. Air can be sampled in a Saran® or
Mylar® plastic bag; approximately 5 liters of the sample are drawn into an
evacuated cell. Continuous monitoring of air flowing through the cell is
possible if the spectrometer is set to one particular wavelength. Some vapors
can be adsorbed on silica gel and quantitatively desorbed into the absorption
cell later. Tentative qualitative identification of compounds can be made
based on a full infrared absorption spectrum.
INTERFERENCES:
Compounds present in the sample that absorb infrared radiation at the
wavelength of interest will interfere.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The sensitivity of the method, using a
10-meter pathlength cell, is 200 milligrams per cubic meter or 100 parts per
million. No precision or accuracy information is furnished.
A-177
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REFERENCE;
American Public Health Association, "Infrared Absorption Spectroscopy;" In
Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington,
1977, pp.79-84.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $75-85
(list), plus sampling costs.
Air Samples
Laboratory Method 2
METHOD SUMMARY:
Nitric oxide in air samples can be determined spectrometrically. A
known volume of air is drawn through a sampling tube containing (in series)
triethanolamine-impregnated molecular sieve, Draeger oxidizer, and additional
triethanolamine-impregnated molecular sieve. The first section removes ambient
nitrogen dioxide. The Draeger oxidizer transforms nitric oxide to nitrogen
dioxide, and the last section adsorbs the nitrogen dioxide. The nitrogen
dioxide in the last section is desorbed and hydrolyzed in aqueous triethanol-
amine solution to yield nitrite ion. An aliquot is treated with hydrogen perox-
ide, sulfanilamide, and N-(l-naphthyl)ethylenediamine dihydrochloride, and the
intensity of the color of the reacted nitrite ion is determined on a spectro-
photometer at 540 nm.
INTERFERENCES:
High levels of nitrogen dioxide can interfere.
QUALITY CONTROL:
One blank should be processed with every 5 samples.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH), and validated over the range of 13.6 to 58.9 milligrams per
cubic meter, using a 1.5-liter sample. Precision and accuracy information is
furnished.
REFERENCE;
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 4, Method S321; Publication No. 78-175, U.S. DHEW:
Cincinnati, August 1978.
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COST INFORMATION:
The cost per sample for analysis by this method is approximately $55
(list), plus sampling costs.
See also: "Hazardous Organic Emissions," Appendix B.
See also: "Nitrogen Dioxide and Nitric Oxide," Appendix B.
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
METHOD SUMMARY:
Nitric oxide in water samples can be measured by chemiluminescence. The
nitric oxide is stripped from the water and the chemiluminescence of the nitric
oxide in the gaseous phase is determined.
INTERFERENCES;
No specific interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This procedure is not EPA-approved. Some precision information is
furnished.
REFERENCE:
Zafiriou, 0. C.; McFarland, M. "Determination of Trace Levels of Nitric Oxide
in Aqueous Solution," Anal. Chem. , 5_2(11), 1980, pp. 1662-1667.
COST INFORMATION;
Cost information has not been obtained.
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NITROGEN DIOXIDE (CAS Number 10102-44-0)
RQ: 4.54 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
METHOD SUMMARY:
Analysis for nitrogen dioxide in air may be performed by use of a detector
tube. A 0.2- to 0.5-liter air sample is collected and analyzed with a hand-
operated bellows pump and a nitrogen dioxide gas detector tube (Draeger® CH
30001 or equivalent). A positive result is indicated by a color change in the
tube from pale gray to bluish-gray. The analysis is based on reaction with
N,N-diphenylbenzidine.
INTERFERENCES:
Ozone and chlorine will also cause color changes. Ozone causes a color
change to pale gray. Chlorine is indicated with approximately one-half to one-
third the sensitivity of N02•
QUALITY CONTROL:
No quality control procedures are given.
SENSITIVITY:
This method is sensitive to concentration levels of approximately 1 to 50
milligrams per cubic meter.
REFERENCES:
Snyder, R. E.; Jankin, M. E.; McKissick, A. M. Development of Hazardous Toxic
Wastes Analytical Screening Procedures, Atlantic Research Corporation for U.S.
Army Medical Research and Development Command, Fort Detrick, Maryland, July 16,
1982, p. 4.
National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations
and Technical Gas Analysis with Draeger® Tubes", 4th ed.; Draeger: Pittsburgh,
August 1979.
National Draeger, Inc., Bulletin No. ND-105; Draeger: Pittsburgh, January 1,
1982.
National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit
Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; Draeger:
Pittsburgh, December 1981.
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COST INFORMATION:
The cost per sample for analysis by this method is approximately $13-22
(list).
See also: "Organic Vapors," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Fluorides and Other Compounds," Appendix B.
Air Samples
Laboratory Method 1
METHOD SUMMARY:
Analysis of air for nitrogen dioxide can be performed by passage of a
known volume of air through an impinger filled with Griess-Saltzman reagent,
followed by colorimetric analysis of the resulting solution. Five standard
solutions, with concentrations of 0.1 to 1 micrograms nitrogen dioxide per
milliliter should be used for calibration.
INTERFERENCES:
Sulfur dioxide interference is eliminated by addition of 1 percent acetone
to the color reagent; nitric oxide and ozone do not interfere.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
Method 13535 is used by the Alberta Environmental Centre and is not EPA-
approved. The method is suitable over the concentration range of 2 to 600
micrograms of nitrogen dioxide per liter of air. The detection limit is 2
milligrams per liter of test solution. Method 108 has been tentatively
approved by the National Institute for Occupational Safety and Health (NIOSH)
for use over the range of 0.01 to 10 micrograms per cubic meter. Precision and
accuracy information is furnished.
REFERENCES;
Alberta Environment, Methods Manual for Chemical Analysis of Atmospheric
Pollutants. 2nd ed.; Method 13535, Alberta Environmental Centre, Vegreville,
Alberta, Canada, 1981.
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American Society for Testing and Materials, 1983 Annual Book of ASTM Standards,
Vol. 11.03, D1607-76; ASTM: Philadelphia, 1983.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, Method P&CAM 108; Publication No. 75-121, U.S. DREW: Cincinnati, 1974.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 108; Publication No. 77-157-A, U.S.
DHEW, 1977.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $20-25
(list), plus sampling costs.
Air Samples
Laboratory Method 2
METHOD SUMMARY:
Nitrogen dioxide in air samples can be measured spectrophotometrically. A
known volume of air is drawn through triethanolamine-impregnated molecular
sieve. The nitrogen dioxide is desorbed from the molecular sieve with aqueous
triethanolamine. An aliquot of the solution is treated with hydrogen peroxide,
sulfanilamide, and N-(l-naphthyl)ethylenediamine dihydrochloride, and the color
intensity is determined on a spectrophotometer at 540 nm.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
A blank should be processed with every 10 samples.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH), and validated over the range of 5.8 to 21.6 milligrams per
cubic meter, using a 3.9-liter sample. The detection limit is approximately
0.2 milligrams per cubic meter. Precision and accuracy information is
furnished.
REFERENCE:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 4, Method S320; Publication No. 78-175, U.S. DHEW:
Cincinnati, August 1978.
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COST INFORMATION:
Cost per sample for analysis by this method is approximately $25-30
(list), plus sampling costs.
Air Samples
Laboratory Method 3
METHOD SUMMARY:
Infrared absorption spectrometry can be used to determine the concentration
of nitrogen dioxide in air samples. The absorbance at 7900 nm (1266 cm"1) is
measured, using a 10-meter pathlength cell. Air can be sampled in a Saran® or
Mylar® plastic bag; approximately 5 liters of the sample are drawn into an
evacuated cell. Continuous monitoring of air flowing through the cell is
possible if the spectrometer is set to one particular wavelength. Some vapors
can be adsorbed on silica gel and quantitatively desorbed into the absorption
cell later. Tentative qualitative identification of compounds can be made
based on a full infrared absorption spectrum.
INTERFERENCES:
Compounds present in the sample that absorb infrared radiation at the
wavelength of interest will interfere.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The sensitivity of the method, using a
10-meter pathlength cell, is 10 milligrams per cubic meter or 5 parts per
million. No precision or accuracy information is furnished.
REFERENCE:
American Public Health Association, "Infrared Absorption Spectroscopy," In
Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington,
1977, pp. 79-84.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $75-85
(list), plus sampling costs.
See also: "Hazardous Organic Emissions," Appendix B.
See also: "Nitrogen Dioxide and Nitric Oxide," Appendix B.
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Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
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OSMIUM TETROXIDE (CAS Number 20816-12-0)
RQ: 454 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
Soil/Sediment Samples
Laboratory Method
METHOD SUMMARY:
Analysis of soil/sediment samples for osmium tetroxide can be performed by
atomic spectrometric analysis for osmium. The sample is digested with nitric
acid and hydrogen peroxide, and the osmium content of the resulting solution is
determined by flame-atomization atomic absorption spectrometry (flame AA),
furnace atomization AA, or inductively coupled atomic plasma emission spectro-
meters (ICP). This method does not identify any particular osmium compound, but
measures the total osmium content of the sample.
INTERFERENCES:
Substances that emit or absorb light at the frequency being monitored can
interfere in AA. The method of standard additions can eliminate many matrix
effects.
QUALITY CONTROL:
Ten percent of the samples should be processed in duplicate and one method
blank should be analyzed with each set of samples.
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EPA/TECHNICAL STATUS:
This method is EPA-approved for analyses under the Resource Conservation
and Recovery Act (RCRA). No precision and accuracy information is furnished.
REFERENCE:
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed. Methods 3050, 7550, 7551; SW-846,
U.S. EPA Washington, 1982.
COST INFORMATION;
Cost per sample for analysis by flame AA is approximately $20-30 (list);
by furnace AA, it is approximately $28-60 (list); by ICP, approximately $20
(list).
Water Samples
Laboratory Method
METHOD SUMMARY:
Analysis for osmium tetroxide in water samples may be performed by atomic
absorption spectrometry (AA). A 100-milliliter sample is mixed with acid,
heated, filtered, and the resulting solution analyzed for osmium by flame or
furnace AA. Concentrations of osmium below 0.5 milligrams per liter should be
analyzed by furnace AA.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require background correction or standard addition
methods. A check standard should be analyzed each time a set of samples is run.
EPA/TECHNICAL STATUS:
These methods are approved for analyses under the National Pollutant Dis-
charge Elimination System (NPDES) and Resource Conservation and Recovery Act
(RCRA). Precision and accuracy information is furnished (Methods 252.1, 252.2),
REFERENCES:
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Methods 252.1, 252.2: EPA-600/4-79-020, U.S. EPA: Cincinnati, 1979.
U.S. Environmental Protection Agency, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods, 2nd ed., Methods 3050, 7550, 7551; SW-846, U.S. EPA:
Washington, 1982.
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COST INFORMATION;
Cost per sample for analysis by flame AA is approximately $10-20 (list):
by furnace AA, it is approximately $18-50 (list).
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PHENYLMERCURIC ACETATE (CAS Number 62-38-4)
RQ: 0.454
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Mercury," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Mercury," Appendix B.
Water Samples
Laboratory Method
See "Mercury," Appendix B.
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PHOSPHINE (CAS Number 7803-51-2)
RQ: 45.4 kg
SAFETY INFORMATION: Exhibits toxicity (inhalation). Flammable gas.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Methods
METHOD SUMMARY:
Analysis for phosphine in air may be performed by use of a detector tube.
A 1-liter air sample is collected and analyzed with a hand-operated bellows pump
and a phosphine gas detector tube (Draeger® CH 31101, or equivalent). A
positive result is indicated by a color change in the tube from white to weak
grayish-violet. The method is based on the reaction of phosphine with a gold
compound to form colloidal gold.
INTERFERENCES:
Arsine and antimony hydride will also give positive results. Ammonia,
hydrogen chloride, hydrogen selenide, hydrogen sulfide, and mercaptans are
retained by the precleanse layer of the tube.
QUALITY CONTROL:
No quality control procedures are given.
SENSITIVITY:
This method is sensitive to concentration levels of approximately 0.1 to 5
milligrams per cubic meter for the sample size given above.
REFERENCES:
Snyder, R. E.; Jankin, M. E.; McKissick, A. M. Development of Hazardous Toxic
Wastes Analytical Screening Procedures, Atlantic Research Corporation for U.S.
Army Medical Research and Development Command, Fort Detrick, Maryland, July 16,
1982, p. 4.
National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations
and Technical Gas Analysis with Draeger® Tubes", 4th ed.; Draeger: Pittsburgh,
August 1979.
National Draeger, Inc., Bulletin No. ND-105; Draeger: Pittsburgh, January 1,
1982.
National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit
A-189
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Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; Draeger
Pittsburgh, December 1981.
COST INFORMATION:
The cost per sample for analysis by this method is approximately $13-22
(list).
See also: "Organic Vapors," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Fumigants," Appendix B.
Soil/Sediment Samples
Laboratory Method
METHOD SUMMARY:
Phosphine in waterlogged soils can be measured by gas chromatography (GC)
with helium-ionization detection. The soil is air-dried and crushed, then
incubated in sealed reaction vessels. The gases evolved are analyzed by GC
with helium ionization detection. Some phosphine may remain sorbed on the
soil after incubation, instead of escaping to the atmosphere being analyzed.
INTERFERENCES:
Sorption of the phosphine on the soil may affect results.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision and accuracy information is
not furnished.
REFERENCE:
Burford, J. R.; Bremner, J. M. "Is Phosphate Reduced to Phosphine in Water-
A-190
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logged Soils ?" Soil Biol. Biochem., 4(4), 1972, pp. 489-495.
COST INFORMATION;
Cost information has not been obtained.
Water Samples
Laboratory Method
METHOD SUMMARY:
Phosphine in water samples can be measured by gas chromatography with
flame photometric detection (GC/FPD) in the phosphorus mode. A thermionic
detector or a microcoulometric detector may be employed as an alternative, if
the phosphine is present in sufficient quantity.
INTERFERENCES:
Large concentrations of sulfur gases or vapors can interfere, unless
preventive measures are taken.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision information is furnished. The
limit of detection is 0.5, 500, or 2 micrograms of analyte per liter, respec-
tively, using FPD, microcoulometric, or thermionic detection.
REFERENCE:
Berck, B.; Westlake, W. E.; Gunther, F. A. "Microdetermination of Phosphine by
Gas-Liquid Chromatography with Microcoulometric, Thermionic, and Flame Photo-
metric Detection," J. Agric. Food Chem., 1^(1), 1970, pp. 143-147.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $120 (list).
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PHOSPHORIC ACID (CAS Number 7664-38-2)
RQ: 2270 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
METHOD SUMMARY:
Analysis for phosphoric acid in air can be performed colorimetrically. A
known volume of air is passed through a membrane filter and the analyte is
removed from the filter by hot-water leaching. The resulting solution is
reacted with sodium molybdate and hydrazine sulfate to form a blue (molybdenum
blue) complex. The absorbance is read at 830 nm on a spectrophotometer.
INTERFERENCES;
Airborne particulate salts of phosphoric acid will interfere with this
determination.
QUALITY CONTROL:
Percent recovery must be determined for the analytical procedure and
results should be corrected for recoveries of less than 95 percent. Duplicate
determinations should agree within 5 percent, and a method blank must be
analyzed with each sample or set of samples.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH), and validated over the range of 0.5 to 1.9 milligrams per
cubic meter for a 90-liter sample of air- A variation of this method is
A-192
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classified as operational by NIOSH over the range of 0.2 to 4 milligrams per
cubic meter for the same sample size. Precision and accuracy information is
furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods. 2nd ed., Vol. 1, Method P&CAM 216; Publication No. 77-157-A, U.S.
DREW: Cincinnati, 1977.
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set M, Method S333; PB-265 029 (NTIS), U.S. DHEW: Cincinnati, December 1976.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 3, Method S333; Publication No. 77-157-C, U.S DHEW:
Cincinnati, 1977.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $30-35 (list).
See also: "Inorganic Acids," Appendix B.
See also: "Phosphorus," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Phosphorus," Appendix B.
Water Samples
Laboratory Method
See "Phosphorus," Appendix B.
See "Weak Acids," Appendix B.
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PHOSPHORUS (CAS Number 7723-14-0)
RQ: 0.454 kg
SAFETY INFORMATION: Flammable solid; inflames on contact with air. Potentially
chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
METHOD SUMMARY:
White phosphorus (also called yellow phosphorus) in air samples may be
measured by gas chromatography. A known volume of air is passed through a tube
containing Tenax GC resin to collect the phosphorus vapor, and the phosphorus
is desorbed into xylene. Alternatively, the air sample may be passed through a
midget impinger containing xylene. In either case, the xylene solution is
analyzed by gas chromatography with flame photometric detection (GC/FPD).
INTERFERENCES:
Phosphorus compounds having retention times close to that of phosphorus
will interfere.
QUALITY CONTROL:
Desorption efficiency must be determined over the range of interest when
Tenax GC is used for sample collection, and a method blank should be processed
with every 10 samples. The desorption efficiency and the results of the method-
blank analysis should be used in calculation of results.
A-194
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EPA/TECHNICAL STATUS;
The Tenax GC collection method is approved by the National Institute for
Occupational Safety and Health (NIOSH), and has been validated over the range
of 0.056 to 0.244 milligrams per cubic meter, using a 12-liter sample. The
method is capable of measurement of much lower levels if the desorption
efficiency is adequate. A second method utilizing Tenax GC collection is
proposed by NIOSH for use over the range of 0.01 to 1.00 milligrams per cubic
meter in a 20-liter air sample. A method employing collection in an impinger
is proposed by NIOSH for use over the range of 0.005 to 5.0 milligrams per
cubic meter in a 50-liter air sample. Precision and accuracy information is
furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 4, Method S334; Publication No. 78-175, U.S. DHEW:
Cincinnati, August 1978.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 242; Publication No. 77-157-A, U.S.
DHEW: Cincinnati, 1977.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods. 2nd ed., Vol. 1, Method P&CAM 257; Publication No. 77-157-A, U.S.
DHEW: Cincinnati, 1977.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $110-130
(list), plus sampling costs.
See also: "Phosphorus," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Phosphorus," Appendix B.
Water Samples
Laboratory Method
See "Phosphorus," Appendix B.
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PHOSPHORUS OXYCHLORIDE (CAS Number 10025-87-3)
RQ: 454 kg
SAFETY INFORMATION: Reacts violently with water or moisture to yield
hydrogen chloride.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Reacts with water.
Water Samples
Field Method
Reacts with water-
See "Halides, Cyanides, and Other Compounds," Appendix B.
Air Samples
Laboratory Method
See "Phosphorus," Appendix B.
Soil/Sediment Samples
Laboratory Method
Reacts with water.
See "Phosphorus," Appendix B.
Water Samples
Laboratory Method
Reacts with water.
See "Phosphorus," Appendix B.
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PHOSPHORUS PENTASULFIDE (CAS Number 1314-80-3)
RQ: 45.4 kg
SAFETY INFORMATION: Forms hydrogen sulfide on contact with water-
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Reacts with water.
See "Sulfides," Appendix B.
Water Samples
Field Method
Reacts with water.
See "Aromatics and Other Compounds," Appendix B.
See "Fluorides and Other Compounds, Appendix B.
See "Halides, Cyanides, and Other Compounds," Appendix B,
See "Sulfides," Appendix B.
Air Samples
Laboratory Method
See "Phosphorus," Appendix B.
See "Sulfur Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Laboratory Method
Reacts with water-
See "Phosphorus," Appendix B.
See "Sulfides," Appendix B.
Water Samples
Laboratory Method
Reacts with water,
A-197
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See "Phosphorus," Appendix B.
See "Sulfides," Appendix B.
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PHOSPHORUS TRICHLORIDE (CAS Number 7719-12-2)
RQ: 454 kg
SAFETY INFORMATION;
Reacts violently with water to produce hydrochloric and
phosphorus acids.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Reacts with water.
Water Samples
Field Method
Reacts with water.
See "Halides, Cyanides, and Other Compounds," Appendix B.
Air Samples
Laboratory Method
See "Chlorides," Appendix B.
See "Phosphorus," Appendix B.
Soil/Sediment Samples
Laboratory Method
Reacts with water.
See "Phosphorus," Appendix B.
Water Samples
Laboratory Method
Reacts with water.
See "Chlorides," Appendix B.
See "Phosphorus," Appendix B.
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POTASSIUM ARSENATE (CAS Number 7784-41-0)
RQ: 454 kg
SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Arsenic," Appendix B.
Water Samples
Field Method
See "Potassium," Appendix B.
Air Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Potassium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Potassium," Appendix B.
Water Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Potassium," Appendix B.
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POTASSIUM ARSENITE (CAS Number 10124-50-2)
RQ: 454 kg
SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Arsenic," Appendix B.
Water Samples
Field Method
See "Potassium," Appendix B.
Air Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Potassium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Potassium," Appendix B.
Water Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Potassium," Appendix B.
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POTASSIUM CHROMATE (CAS Number 7789-00-6)
RQ: 454 kg
SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Chromium," Appendix B,
Soil/Sediment Samples
Field Method
See "Chromium," Appendix B.
Water Samples
Field Method
See "Chromates," Appendix B.
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
See "Potassium," Appendix B.
Air Samples
Laboratory Method
See "Chromic Acid and Chromates," Appendix B.
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
See "Potassium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
See "Potassium," Appendix B.
Water Samples
Laboratory Method
See "Chromium," Appendix B.
See "Chromium, Hexavalent," Appendix B.
See "Potassium," Appendix B.
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POTASSIUM CYANIDE (CAS Number 151-50-8)
RQ: 4.54 kg
SAFETY INFORMATION; Exhibits toxicity (oral). Produces toxic hydrogen cyanide
upon contact acids.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Cyanides," Appendix B.
Soil/Sediment Samples
Field Method
See "Cyanides," Appendix B.
Water Samples
Field Method
See "Cyanides," Appendix B.
See "Halides, Cyanides, and Other Compounds," Appendix B.
See "Potassium," Appendix B.
Air Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Potassium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Potassium," Appendix B.
Water Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Potassium," Appendix B.
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POTASSIUM DICHROMATE (CAS Number 7778-50-9)
RQ: 454 kg
SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Chromium, Appendix B.
Soil/Sediment Samples
Field Method
See "Chromium," Appendix B,
Water Samples
Field Method
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
See "Potassium," Appendix B.
Air Samples
Laboratory Method
See "Chromic Acid and Chromates," Appendix B.
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
See "Potassium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
See "Potassium," Appendix B.
Water Samples
Laboratory Method
See "Chromium," Appendix B.
See "Chromium, Hexavalent," Appendix B.
See "Potassium," Appendix B.
A-204
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POTASSIUM HYDROXIDE (CAS Number 1310-58-3)
RQ: 454 kg
SAFETY INFORMATION: Generates heat in contact with water. Generates flammable
hydrogen gas in contact with some metals.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Hydroxides," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Potassium," Appendix B.
Air Samples
Laboratory Method
See "Potassium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Potassium," Appendix B,
Water Samples
Laboratory Method
See "Potassium," Appendix B.
A-205
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POTASSIUM PERMANGANATE (CAS Number 7722-64-7)
RQ: 45.4 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
METHOD SUMMARY:
Analysis for potassium permanganate in air can be performed by filtration
of air, followed by X-ray fluorescence analysis of the filter for manganese,
using a portable X-ray fluorescence spectrometer and a radioisotope excitation
source. Sampling time may be up to 8 hours, but analysis may be performed in
approximately 1 minute. This method is non-destructive, so that further analy-
sis of the filtered material may be undertaken following this measurement. The
method is not specific for potassium permanganate, but measures the total
manganese content of the sample.
INTERFERENCES:
Polyvinyl chloride filters are unacceptable for sampling, and silica
quartz filter materials contain silicon, aluminum, and phosphorus, which
interfere in the analysis. Cellulose membrane or fiber filters and polycarbonate
or fluorocarbon membrane filters are acceptable, while glass fiber filters are
satisfactory for sampling only if of the highest purity.
QUALITY CONTROL:
No quality control procedures are given.
SENSITIVITY:
This method is not EPA-approved. Precision information is furnished. The
method is sensitive to amounts of manganese over 280 micrograms, or approxi-
mately 0.1 to 10.0 micrograms per cubic meter, depending on the volume of air
sampled.
REFERENCES:
Rhodes, J. R.; Stout, J. C.; Schindler, J. S.; Piorek, S. "Portable X-ray
Survey Meters for in Situ Trace Element Monitoring of Air Particulates," In
Toxic Materials in the Atmosphere, STP-786; American Society for Testing and
Materials: Philadelphia, 1981, pp. 70-82.
Rhodes, J. R.; Pradzynski, A. H.; Hunter, C. B.; Payne, J. S.; Lindgren, J. L.
"Energy Dispersive X-ray Fluorescence Analysis of Air Particulates in Texas,"
Environ. Sci. Technol., 6(10), 1972, pp. 922-927.
A-206
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COST INFORMATION:
The cost per sample for analysis by this method is approximately $30,
plus sampling costs.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Potassium," Appendix B.
Air Samples
Laboratory Method 1
METHOD SUMMARY:
Analysis for potassium permanganate in air can be performed by filtration
of air, followed by X-ray fluorescence analysis of the filter for manganese.
Sampling time may be up to 8 hours but analysis may be performed in approxi-
mately 1 minute. This method is non-destructive, so that further analysis of
the filtered material may be undertaken following this measurement. The method
is not specific for potassium permanganate, but measures the total manganese
content of the sample.
INTERFERENCES:
Polyvinyl chloride filters are unacceptable for sampling, and silica
quartz filter materials contain silicon, aluminum, and phosphorus which inter-
fere . Cellulose membrane or fiber filters and polycarbonate or fluorocarbon
membrane filters are acceptable, while glass fiber filters are satisfactory for
sampling only if of the highest purity.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Precision information is furnished. The
method is sensitive to amounts of manganese over 280 micrograms, or approx-
imately 0.1 to 10.0 microgram per cubic meter, depending on the volume of air
sampled.
A-207
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REFERENCES:
Rhodes, J. R.; Stout, J. C.; Schindler, J. S.; Piorek, S. "Portable X-ray
Survey Meters for in Situ Trace Element Monitoring of Air Particulates," In
Toxic Materials in the Atmosphere, STP-786; American Society for Testing and
Materials: Philadelphia, 1981, pp. 70-82.
Rhodes, J. R.; Pradzynski, A. H.; Hunter, C. B.; Payne, J. S.; Lindgren, J. L.
"Energy Dispersive X-ray Fluorescence Analysis of Air Particulates in Texas,"
Environ. Sci. Technol., 6(10), 1972, pp. 922-927.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $30 (list),
$20 (bid), plus sampling costs.
See also: "Potassium," Appendix B.
Air Samples
Laboratory Method 2
METHOD SUMMARY:
Analysis for potassium permanganate in air samples may be performed by
flame atomic absorption (AA) spectrometric determination of manganese. A known
volume of air is drawn through a membrane or glass fiber filter. The filter
with the collected particulates is digested with nitric or nitric and hydro-
fluoric acids, and an aliquot of the resulting solution is aspirated into the
AA instrument. This method does not specifically identify potassium permanga-
nate, but measures the total manganese content of the sample.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
A blank should be processed with every 10 samples. Standard solutions
should be analyzed in duplicate.
EPA/TECHNICAL STATUS:
This method is classified as operational by the National Institute of
Occupational Safety and Health (NIOSH) for use over the range of 21 to 125
micrograms manganese per cubic meter in a 240-liter air sample. Precision
information is furnished. Alberta Environment has determined the limit of
detection to be 0.01 micrograms manganese per cubic meter of air.
A-2 08
-------
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 173; Publication No. 77-157-A, U.S.
DREW: Cincinnati, 1977.
Alberta Environment, Methods Manual for Chemical Analysis of Atmospheric
Pollutants, Methods 23535, 23542, Alberta Environmental Centre, Vegreville,
Alberta, Canada, 1981.
COST INFORMATION;
Cost per sample for analysis by this method is approximately $10-20
(list), plus sampling costs.
Soil/Sediment Samples
Laboratory Method
METHOD SUMMARY:
Analysis for potassium permanganate in soil/sediment samples can be per-
formed by atomic spectrometric analysis for manganese. A 2-gram sample is
digested with nitric acid and hydrogen peroxide and analyzed by inductively
coupled plasma (ICP) or flame atomic absorption spectrometry (AA). Flame AA is
not recommended for low levels of manganese. Analysis for manganese in oil may
be performed by ICP after sample dilution with methyl isobutyl ketone (MIBK) or
xylene, using standards miscible with these solvents. This method is not
specific for potassium permanganate, but measures the total manganese content
of the sample.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods.
Standards should be analyzed at least daily and a reference standard should be
run weekly. At least 10 percent of the analyses should be duplicates and/or
standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program, and are required for use
in Resource Conservation and Recovery Act (RCRA) and Clean Water Act analyses.
Precision and accuracy information is furnished.
A-209
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REFERENCES:
Exhibit D, Chemical Analytical Services for Low and Medium Concentration
Inorganics in All Media, Invitation for Bid (Solicitation Number WA 82-A072),
U.S. EPA: Washington, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 243.1, EPA-600/4-79-020, U.S. EPA: Cincinnati, March 1979.
Federal Register, 44(233), December 3, 1979. pp. 69559 - 69564.
Fassel, V- A.; Peterson, C. A.; Abercrombie, F. N.; Kniseley, R. N. "Simultan-
eous Determination of Wear Metals in Lubricating Oils by Inductively-Coupled
Plasma Atomic Emission Spectrometry" Anal. Chem., 48_(3), 1976, p. 516.
COST INFORMATION:
Cost per sample for analysis by flame AA is approximately $20-30 (list);
by ICP, it is approximately $20 (list).
See also: "Potassium," Appendix B.
Water Samples
Laboratory Method
METHOD SUMMARY:
Analysis for potassium permanganate in water samples may be performed by
atomic spectrometric analysis for manganese. A 100-milliliter sample is di-
gested with nitric acid and hydrogen peroxide and analyzed by inductively
coupled plasma (ICP) or flame atomic absorption spectrometry (AA). Flame AA is
not recommended for low levels of manganese. This method is not specific for
potassium permanganate, but measures the total manganese content of the sample.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
For each matrix analyzed, it is necessary to determine if matrix effects
and/or interferences require standard addition or serial dilution methods. A
reference standard should be analyzed weekly and at least 10 percent of the
analyses should be duplicates and/or standards.
EPA/TECHNICAL STATUS:
These methods are in use in the CERCLA program, and are required for
Resource Conservation and Recovery Act (RCRA) and National Pollutant Discharge
Elimination System (NPDES) analyses. Precision and accuracy information is
furnished.
A-210
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REFERENCES:
Exhibit D, Chemical Analytical Services for Low and Medium Concentration
Inorganics in All Media, Invitation for Bid (Solicitation Number WA 82-A072),
U.S. EPA: Cincinnati, April 23, 1982.
U.S. Environmental Protection Agency, Methods for Chemical Analysis of Water
and Wastes, Method 243.1, EPA-606/479-020, U.S. EPA: Cincinnati, March 1979.
Federal Register, 4_4(233), December 3, 1979. pp. 69559-69564.
COST INFORMATION:
Cost per sample for analysis by flame AA is approximately $10-20 (list);
by ICP, it is approximately $10 (list).
See also: "Potassium," Appendix B.
A-211
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POTASSIUM SILVER CYANIDE (CAS Number 506-61-6)
RQ: 4.54 kg
SAFETY INFORMATION: Strong oxidizer; can readily cause fires.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Field Method
Soil/Sediment Samples
Field Method
See "Cyanides," Appendix B.
Water Samples
Field Method
See "Cyanides," Appendix B.
See "Potassium," Appendix B.
See "Silver," Appendix B.
Air Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Potassium," Appendix B.
See "Silver," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Potassium," Appendix B.
See "Silver," Appendix B.
Water Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Potassium," Appendix B.
See "Silver," Appendix B.
A-212
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SELENIOUS ACID (CAS Number 7783-00-8)
RQ: 0.454 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Selenium," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Selenium," Appendix B.
Air Samples
Laboratory Method
See "Selenium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Selenium," Appendix B,
Water Samples
Laboratory Method
See "Selenium," Appendix B.
A-213
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SELENIUM (CAS Number 7782-49-2)
RQ: 0.454 kg
SAFETY INFORMATION: Exhibits toxicity (inhalation). Potentially chronically
toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Selenium," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Selenium," Appendix B.
Air Samples
Laboratory Method
See "Selenium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Selenium," Appendix B.
Water Samples
Laboratory Method
See "Selenium," Appendix B.
A-214
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SELENIUM DIOXIDE (CAS Number 7446-08-4)
RQ: 454 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Selenium," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Selenium," Appendix B.
Air Samples
Laboratory Method
See "Selenium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Selenium," Appendix B.
Water Samples
Laboratory Method
See "Selenium," Appendix B.
A-215
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SELENIUM DISULFIDE (CAS Number 7488-56-4)
RQ: 0.454 kg
SAFETY INFORMATION: Forms toxic hydrogen sulfide in contact with acid. Poten-
tially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Selenium," Appendix B.
Soil/Sediment Samples
Field Method
See "Sulfides," Appendix B.
Water Samples
Field Method
Insoluble in water.
Air Samples
Laboratory Method
See "Selenium," Appendix B.
See "Sulfur Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Selenium," Appendix B.
See "Sulfides," Appendix B.
Water Samples
Laboratory Method
Insoluble in water.
A-216
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SELENOUREA (CAS Number 630-10-4)
RQ: 0.454 kg
SAFETY INFORMATION; Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Selenium," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Selenium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Selenium," Appendix B.
Water Samples
Laboratory Method
See "Selenium," Appendix B.
A-217
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SILVER (CAS Number 7440-22-4)
RQ: 454 kg
SAFETY INFORMATION: Potentially chronically toxic.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Silver," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Silver," Appendix B.
See "Silver," Appendix B.
Water Samples
Laboratory Method
A-218
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SILVER CYANIDE (CAS Number 506-64-9)
RQ: 0.454 kg
SAFETY INFORMATION: Exhibits chronic toxicity.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Cyanides," Appendix B.
Water Samples
Field Method
See "Cyanides," Appendix B.
See "Silver," Appendix B.
Air Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Silver," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Silver," Appendix B.
Water Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Silver," Appendix B.
A-219
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SILVER NITRATE (CAS Number 7761-88-8)
RQ: 0.454 kg
SAFETY INFORMATION; Exhibits chronic toxicity.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Nitrate Ions," Appendix B.
See "Silver," Appendix B.
Air Samples
Laboratory Method
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
See "Silver," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
See "Silver," Appendix B.
Water Samples
Laboratory Method
See "Nitrates," Appendix B.
See "Silver," Appendix B.
A-220
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RQ: 4.54 kg
SAFETY INFORMATION:
SODIUM (CAS Number 7740-23-5)
Inflames upon contact with water.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Reacts with water.
Water Samples
Field Method
Reacts with water.
Air Samples
Laboratory Method
See "Sodium," Appendix B.
Soil/Sediment Samples
Laboratory Method
Reacts with water.
See "Sodium," Appendix B,
Water Samples
Laboratory Method
Reacts with water.
See "Sodium," Appendix B.
A-221
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SODIUM ARSENATE (CAS Number 7631-89-2)
RQ: 454 kg
SAFETY INFORMATION; Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Arsenic," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Sodium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Sodium," Appendix B.
Water Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Sodium," Appendix B.
A-222
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SODIUM ARSENITE (CAS Number 7784-46-5)
RQ: 454 kg
SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Arsenic," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Sodium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Arsenic," Appendix B.
See "Sodium," Appendix B.
Water Samples
Laboratory Method
See "Arsenic," Appendix B,
See "Sodium," Appendix B.
A-223
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SODIUM AZIDE (CAS Number 26628-22-8)
RQ: 454 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
METHOD SUMMARY:
Analysis for sodium azide in air can be performed by high-volume filtra-
tion of air, followed by dissolution of particulates in deionized water and
analysis of the resulting solution for azide ion by ion chromatography.
INTERFERENCES;
Use of an alkaline sodium carbonate eluant may eliminate interferences
due to the presence of phosphate ions. The presence of bromide ions in the
sample interferes with accurate determination of azide concentration.
QUALITY CONTROL:
The air filter should collect greater than 99.96 percent of particulates
larger than 3 micrometers in diameter.
EPA/TECHNICAL STATUS:
This method has not been extensively evaluated and precision and accuracy
information is not furnished.
A-224
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REFERENCE:
Westwood, L. C.; Stokes, E. L. In Ion Chromatographic Analysis of Environ-
mental Pollutants, Vol. 2; J. D. Mulik and E. G. Sawicki, Eds.; Ann Arbor
Science: Ann Arbor, 1979, pp. 141-156.
See also: "Sodium," Appendix B.
COST INFORMATION:
The cost per sample for method is approximately $75-80 (list), plus
sampling costs.
Soil/Sediment Samples
Laboratory Method
See "Sodium, " Appendix B.
Water Samples
Laboratory Method
See "Sodium," Appendix B.
A-225
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SODIUM BIFLUORIDE (CAS Number 1333-83-1)
RQ: 45.4 kg
SAFETY INFORMATION; Reacts with water to form hydrofluoric acid.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Fluorides," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Fluorides and Other Compounds," Appendix B.
Air Samples
Laboratory Method
See "Fluorides," Appendix B.
See "Sodium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Fluorides," Appendix B.
See "Sodium," Appendix B.
Water Samples
Laboratory Method
See "Fluorides," Appendix B.
See "Sodium," Appendix B.
A-226
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SODIUM BISULFITE (CAS Number 7631-90-5)
RQ: 2270 kg
SAFETY INFORMATION:
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Sodium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Sodium," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B,
See "Sodium," Appendix B.
See "Sulfites," Appendix B.
A-227
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SODIUM CHROMATE (CAS Number 7775-11-3)
RQ: 454 kg
SAFETY INFORMATION; Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Chromium," Appendix B.
Soil/Sediment Samples
Field Method
See "Chromium," Appendix B,
Water Samples
Field Method
See "Chromates," Appendix B.
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
Air Samples
Laboratory Method
See "Chromic Acid and Chromates," Appendix B.
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
See "Sodium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
See "Sodium," Appendix B.
Water Samples
Laboratory Method
See "Chromium," Appendix B.
See "Chromium, Hexavalent," Appendix B.
See "Sodium," Appendix B.
A-228
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RQ: 4.54 kg
SAFETY INFORMATION:
SODIUM CYANIDE (CAS Number 143-33-9)
Exhibits toxicity (oral). Reacts with acid to form very
toxic hydrogen cyanide.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Cyanides," Appendix B.
Soil/Sediment Samples
Field Method
See "Cyanides," Appendix B.
Water Samples
Field Method
See "Cyanides," Appendix B.
See "Halides, Cyanides, and Other Compounds," Appendix B.
Air Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Sodium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Sodium," Appendix B.
Water Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Sodium," Appendix B.
A-229
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SODIUM BICHROMATE (CAS Number 10588-01-9)
RQ: 454 kg
SAFETY INFORMATION: Potentially carcinogenic. Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Chromium," Appendix B.
Soil/Sediment Samples
Field Method
See "Chromium," Appendix B.
Water Samples
Field Method
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
Air Samples
Laboratory Method
See "Chromic Acid and Chromates," Appendix B.
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
See "Sodium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
See "Sodium," Appendix B.
Water Samples
Laboratory Method
See "Chromium," Appendix B.
See "Chromium, Hexavalent," Appendix B.
See "Sodium," Appendix B.
A-230
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SODIUM DODECYLBENZENE SULFONATE (CAS Number 25155-30-0)
RQ: 454 kg
SAFETY INFORMATION:
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Anionic Detergents," Appendix B.
See "Sodium," Appendix B.
Air Samples
Laboratory Method
See "Sodium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Sodium," Appendix B.
Water Samples
Laboratory Method
See "Alkyl Benzene Sulfonates," Appendix B
See "Sodium," Appendix B.
A-231
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SODIUM FLUORIDE (CAS Number 7681-49-4)
RQ: 454 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Fluorides," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Fluorides and Other Compounds," Appendix B.
Air Samples
Laboratory Method
See "Fluorides," Appendix B.
See "Fluorides and Hydrogen Fluoride," Appendix B.
See "Sodium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Sodium," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Fluorides," Appendix B.
See "Sodium," Appendix B.
A-232
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SODIUM HYDROSULFIDE (CAS Number 16721-80-5)
RQ: 2270 kg
SAFETY INFORMATION: Evolves toxic hydrogen sulfide on contact with acids.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Sulfides," Appendix B.
Water Samples
Field Method
See "Halides, Cyanides, and Other Compounds," Appendix B.
See "Sulfides," Appendix B.
Air Samples
Laboratory Method
See "Sodium," Appendix B.
See "Sulfides," Appendix B, Part II, Section A.
See "Sulfur Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Sodium," Appendix B.
See "Sulfides," Appendix B.
Water Samples
Laboratory Method
See "Sodium," Appendix B.
See "Sulfides," Appendix B.
A-233
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SODIUM HYDROXIDE (CAS Number 1310-73-2)
RQ: 454 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Hydroxides," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
METHOD SUMMARY:
Sodium hydroxide in air samples can be measured by titration. A known
volume of air is drawn through a polytetrafluoroethylene filter. The sodium
hydroxide is extracted with a known amount of excess hydrochloric acid, and the
solution is purged with nitrogen. The excess hydrochloric acid is titrated
under nitrogen with a standard solution of sodium hydroxide and the amount of
sodium hydroxide collected is calculated from the difference between the amount
of acid added and the amount remaining after extraction of the filter. An
alternative sampling procedure is collection of the sodium hydroxide in a
fritted glass bubbler containing excess hydrochloric acid. These methods
are not specific for sodium hydroxide, but measure the total alkalinity in
particulate form when a filter is used for sampling, or total alkalinity in all
phases when a bubbler is used.
INTERFERENCES:
No specific interferences are reported.
QUALITY CONTROL:
A method blank should be processed with each set of samples. Results of
the method-blank analysis should be used in calculations. A recovery factor
should be determined when a filter is used for sampling.
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EPA/TECHNICAL STATUS:
The filter sampling method is approved by the National Institute for
Occupational Safety and Health (NIOSH), and validated over the range of 0.76 to
3.9 milligrams per cubic meter, using a 360-liter sample. The detection limit
is estimated to be 77 micrograms per cubic meter. The bubbler-sampling method
is proposed by NIOSH for the range of 1 to 4 milligrams per cubic meter in a
420-liter sample. Precision and accuracy information is furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 4, Method S381; Publication No. 78-175, U.S. DHEW:
Cincinnati, August 1978.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 241; Publication No. 77-157-A, U.S.
DHEW: 1977.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $30 (list),
plus sampling costs.
See also: "Sodium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Sodium," Appendix B.
See "Sodium," Appendix B.
Water Samples
Laboratory Method
A-235
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SODIUM HYPOCHLORITE (CAS Numbers 7681-52-9, 10022-70-5)
RQ: 45.4 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Halides, Cyanides, and Other Compounds," Appendix B.
Air Samples
Laboratory Method
See "Sodium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Sodium," Appendix B,
Water Samples
Laboratory Method
See "Sodium," Appendix B.
A-236
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SODIUM METHYLATE (CAS Number 124-41-4)
RQ: 454 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Reacts with water.
Water Samples
Field Method
Reacts with water.
Air Samples
Laboratory Method
See "Sodium," Appendix B.
Soil/Sediment Samples
Laboratory Method
Reacts with water -
See "Sodium," Appendix B.
Water Samples
Laboratory Method
Reacts with water-
See "Sodium," Appendix B.
A-237
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SODIUM NITRITE (CAS Number 7632-00-0)
RQ: 45.4 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Sodium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Sodium," Appendix B.
See "Sodium," Appendix B.
Water Samples
Laboratory Method
A-238
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SODIUM PHOSPHATE, DIBASIC (CAS Numbers 7558-79-4, 10039-32-4, 10028-24-7,
10140-65-5)
RQ: 2270 kg
SAFETY INFORMATION:
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Phosphorus," Appendix B.
See "Sodium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Phosphorus," Appendix B.
See "Sodium," Appendix B.
Water Samples
Laboratory Method
See "Phosphorus," Appendix B.
See "Sodium," Appendix B.
A-239
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SODIUM PHOSPHATE, TRIBASIC (CAS Numbers 7601-54-9, 7785-84-4, 10101-89-0,
10361-89-4, 7758-29-4, 10124-56-8)
RQ: 2270 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Phosphorus," Appendix B.
See "Sodium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Phosphorus," Appendix B.
See "Sodium," Appendix B.
Water Samples
Laboratory Method
See "Phosphorus," Appendix B.
See "Sodium," Appendix B.
A-240
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SODIUM SELENITE (CAS Numbers 10102-18-8, 7782-82-3)
RQ: 454 kg
SAFETY INFORMATION: Exhibits toxicity (oral). Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Selenium," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Selenium," Appendix B.
Air Samples
Laboratory Method
See "Selenium," Appendix B.
See "Sodium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Selenium," Appendix B.
See "Sodium," Appendix B.
Water Samples
Laboratory Method
See "Selenium," Appendix B.
See "Sodium," Appendix B.
A-241
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STRONTIUM CHROMATE (CAS Number 7789-06-2)
RQ: 454 kg
SAFETY INFORMATION: Potentially carcinogenic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Chromic Acid and Strontium Chromate," Appendix B.
See "Chromium," Appendix B.
Soil/Sediment Samples
Field Method
See "Chromium," Appendix B.
Water Samples
Field Method
See "Chromates," Appendix B.
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
Air Samples
Laboratory Method
See "Chromic Acid and Chromates," Appendix B.
See "Chromium," Appendix B.
See "Heavy Metals and Compounds (Particulate)," Appendix B,
See "Strontium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Chromium," Appendix B.
See "Hexavalent Chromium," Appendix B.
See "Strontium," Appendix B.
Water Samples
Laboratory Method
See "Chromium," Appendix B.
See "Chromium, Hexavalent," Appendix B.
See "Strontium," Appendix B.
A-242
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STRONTIUM SULFIDE (CAS Number 1314-96-1)
RQ: 45.4 kg
SAFETY INFORMATION: Reacts to form toxic H2S upon contact with acids.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
See "Sulfides," Appendix B.
Water Samples
Field Method
See "Sulfides," Appendix B.
Air Samples
Laboratory Method
See "Strontium," Appendix B.
See "Sulfur Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Strontium," Appendix B.
See "Sulfides," Appendix B.
Water Samples
Laboratory Method
See "Strontium," Appendix B.
See "Sulfides," Appendix B.
A-243
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SULFURIC ACID (CAS Number 7664-93-9)
RQ: 454 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
METHOD SUMMARY:
Sulfuric acid in air samples can be measured by titration. The sample is
passed through filter paper (Whatman No. 4 or equivalent). The filter paper is
macerated in distilled water and the resulting solution is titrated with 0.002
N sodium hydroxide, using a pH meter to determine the endpoint.
INTERFERENCES:
Since matter normally present as dust is neutral, and gases such as sulfur
dioxide, hydrogen chloride, oxides of nitrogen, and ammonia pass through the
filter without affecting its pH, the residual acidity measured equals the
acidity of the sulfuric acid aerosol collected. This method will measure any
acidic particulate or aerosol compounds in the sample and does not identify
sulfuric acid.
QUALITY CONTROL:
The pH of the filter paper batch must have a consistency of 0.03 pH unit,
and a deviation of no more than 0.10 pH unit from that of the distilled water
used in the measurement.
SENSITIVITY:
This method is sensitive to concentration levels of sulfuric acid greater
than 10 nanograms per cubic meter.
REFERENCE:
Mader, P- P.; Hamming, W. J.; Bellin, A. "Determination of Small Amounts of
Sulfuric Acid in the Atmosphere" Anal. Chem., 22/9), 1950, pp. 1181-1183.
COST INFORMATION:
Cost information has not been obtained.
Note: NIOSH Method 267 is applicable, (reference furnished by reviewer).
A-244
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Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
METHOD SUMMARY:
Analysis for sulfuric acid in air can be performed by volatilization,
prefiltration, and derivatization of the sulfuric acid in air samples, followed
by ion chromatographic analysis of the decomposition products of the derivative
for sulfate ions. The method is sensitive to concentration levels of sulfuric
acid above approximately 0.5 micrograms per cubic meter. Samples are stable on
the collection medium for some time. This method is specific for sulfuric acid
and does not give positive results for ammonium sulfate, sulfur dioxide, or
other sulfur compounds.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved and has not been extensively evaluated.
Precision and accuracy information is not furnished.
REFERENCE:
Mason, D. W.; Miller, H. C. In Ion Chromatographic Analysis of Environmental
Pollutants, Vol. 2; J. D. Mulik and E. Sawicki, Eds.; Ann Arbor Science: Ann
Arbor, 1979, p. 193.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $108-120
(list), plus sampling costs.
Air Samples
Laboratory Method 2
A-245
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METHOD SUMMARY:
Sulfuric acid in air samples can be measured by titration. A known volume
of air is drawn through a cellulose membrane filter. The analyte is extracted
with distilled water and isopropyl alcohol followed by pH adjustment with dilute
perchloric acid. The resulting solution is titrated with 0.005 M barium
perchlorate using Thorin as the indicator. The endpoint is reached when the
solution color abruptly changes from yellow to apricot.
INTERFERENCES:
Metal ion interferences can be eliminated by passing the solution through
cation exchange resin. When concentrations of phosphate ions are high the
phosphate ions can be removed by precipitation with magnesium carbonate.
QUALITY CONTROL:
A method blank is analyzed for every 10 samples obtained.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH), and validated over the range of 0.6 to 2.6 milligrams
per cubic meter in a 180-liter sample. Precision and accuracy information is
furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set L, Method S174; PB-250 159 (NTIS), U.S. DHEW: Cincinnati, January 1976.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 3, Method S174; Publication No. 77-157-C, U.S. DHEW:
Cincinnati, 1977.
COST INFORMATION:
Cost per sample by this method is approximately $20-45 (list), plus sam-
pling costs.
Air Samples
Laboratory Method 3
METHOD SUMMARY:
Sulfuric acid mist in air samples may be measured by turbidimetry. The
sulfuric acid is collected in a midget impinger containing distilled water.
The sulfate in the solution is precipitated as barium sulfate and the turbidity
of the suspension is measured at 420 nm on a spectrophotometer-
A-246
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INTERFERENCES:
Large concentrations of colored or suspended matter or organic materials
may interfere. Silica may interfere, and if sulfate salts are present as
particulates in the sample air, they will be reported as sulfuric acid.
QUALITY CONTROL:
One out of every 10 samples should be processed without addition of the
barium reagent for use as a blank.
EPA/TECHNICAL STATUS:
This method is proposed by the National Institute of Occupational Safety
and Health (NIOSH) for use over the range of 0.1 to 4.0 milligrams per cubic
meter of air in a 10-liter sample. Limited precision and accuracy information
is furnished.
REFERENCE:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 1, Method P&CAM 187; Publication No. 77-157-A, U.S. DHEW,
1977.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $30-35
(list), plus sampling costs.
Note: NIOSH Method 267 is applicable (reference furnished by reviewer).
See also: "Inorganic Acids," Appendix B.
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
A-247
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SULFUR MONOCHLORIDE (CAS Number 12771-08-3)
RQ: 454 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
METHOD SUMMARY:
Sulfur monochloride can be measured by titration. The sample is collected
in silver nitrate contained in a fritted bubbler, and acidified with nitric
acid. Sodium chloride is added and the sample is titrated with 0.1 N silver
nitrate. (This method is described by Jacobs, M. B. The Analytical Toxicology
of Industrial Inorganic Poisons; Interscience: New York, 1967, p. 568, and
summarized in the reference given below.)
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
No quality control procedures are given.
SENSITIVITY:
This method is sensitive to concentration levels of approximately 5 milli-
grams of sulfur monochloride per cubic meter- It should be considered a source
method.
REFERENCE:
Quantitative Analysis of Gaseous Pollutants, W. E. Ruch, Ed.; Ann Arbor-Humphrey
Science: Ann Arbor, 1970, p. 218.
COST INFORMATION:
Cost information has not been obtained.
Soil/Sediment Samples
Field Method
Reacts with water.
Water Samples
"Field Method
Reacts with water.
A-248
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See "Aroraatics and Other Compounds," Appendix B.
Air Samples
Laboratory Method
Soil/Sediment Samples
Laboratory Method
Reacts with water.
Water Samples
Laboratory Method
Reacts with water.
A-249
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TETRAETHYL LEAD (CAS Number 78-00-2)
RQ: 45.4
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Organic Vapors," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
METHOD SUMMARY:
Analysis for tetraethyl lead in air can be performed by passage of 120
liters of air through XAD-2 resin, desorbing the tetraethyl lead with pentane,
and analyzing the resulting solution by gas chromatography with photoionization
detection (GC/PID).
INTERFERENCES:
Compounds that coelute with tetraethyl lead can interfere. In such cases,
separation conditions should be changed.
QUALITY CONTROL:
The desorption efficiency must be determined over the concentration
range of interest. Sampling apparatus must be calibrated before use. With each
batch of ten samples a method blank should be processed. Results should be
corrected to reflect the desorption efficiency.
EPA/TECHNICAL STATUS:
This method has been reviewed and evaluated by the National Institute for
Occupational Safety and Health (NIOSH) and has been validated over the range of
45 to 200 micrograms tetraethyl lead per cubic meter in a 120-liter sample of
air. The sensitivity of the method is estimated to be at least 0.1 tnicrograra
per milliliter. Precision and accuracy information is furnished.
A-250
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REFERENCE:
U.S. Department of Health, Education, and Welfare, Ten NIOSH Analytical Methods,
Set 3, Method S383, PB275-834 (NTIS), U.S. DREW: Cincinnati, 1977.
COST INFORMATION:
The cost per sample for analysis by this method is approximately $100-135
(list), plus sampling costs.
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
METHOD SUMMARY;
Tetraethyl lead in water samples can be determined by gas chromatography,
using an atomic absorption spectrometer as the detector (GC/AA). A 200-
milliliter water sample is extracted with hexane, and an aliquot of the solvent
containing the analyte is injected directly into the injection port of the
chromatograph.
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL:
The method of standard addition is used.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. Accuracy information is furnished.
REFERENCE:
Chau, Y. K.; Wong, P- T. S.; Bengert, G. A.; Kramar, 0. "Determination of
Tetraalkyllead Compounds in Water, Sediment, and Fish Samples, Anal. Chem.,
51.(2), 1979, pp. 186-188.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $220-300
(list).
A-251
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THALLIC OXIDE (CAS Number 1314-32-5)
RQ: 0.454 kg
SAFETY INFORMATION; Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Thallium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Thallium," Appendix B.
Water Samples
Laboratory Method
See "Thallium," Appendix B.
A-252
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THALLIUM (CAS Number 7440-28-0)
RQ: 0.454 kg
SAFETY INFORMATION; Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Reacts with water.
Water Samples
Field Method
Reacts with water.
Air Samples
Laboratory Method
See "Thallium," Appendix B.
Soil/Sediment Samples
Laboratory Method
Reacts with water.
See "Thallium," Appendix B,
Water Samples
Laboratory Method
Reacts with water,
See "Thallium," Appendix B.
A-253
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THALLIUM(I)ACETATE (CAS Number 563-68-8)
RQ: 0.454 kg
SAFETY INFORMATION: Potentially chronically toxic.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Thallium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Thallium," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Thallium," Appendix B.
A-254
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THALLIUM(I)CARBONATE (CAS Number 6533-73-9)
RQ: 0.454 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Nitrates," Appendix B.
See "Thallium Compounds," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Thallium," Appendix B.
Water Samples
Laboratory Method
See "Thallium," Appendix B.
A-255
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THALLIUM(I)CHLORIDE (CAS Number 7791-12-0)
RQ: 0.454 kg
SAFETY INFORMATION; Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Chlorides," Appendix B.
See "Thallium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Thallium," Appendix B.
Water Samples
Laboratory Method
See "Chloride," Appendix B.
See "Thallium," Appendix B.
A-256
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THALLIUM(I)NITRATE (CAS Number 10102-45-1)
RQ: 0.454 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Nitrate Ions," Appendix B.
Air Samples
Laboratory Method
See "Nitrates," Appendix B.
See "Nitrates and Sulfates,'1 Appendix B.
See "Thallium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
See "Thallium," Appendix B.
Water Samples
Laboratory Method
See "Nitrates," Appendix B.
See "Thallium," Appendix B.
A-257
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THALLIUM(I)SELENIDE (CAS Number 12039-52-0)
RQ: 0.454 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Selenium," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Insoluble in water -
Air Samples
Laboratory Method
See "Selenium," Appendix B.
See "Thallium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Selenium," Appendix B.
See "Thallium," Appendix B.
Water Samples
Laboratory Method
See "Selenium," Appendix B.
See "Thallium," Appendix B.
A-258
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THALLIUM(I)SULFATE (CAS Number 7446-18-6)
RQ: 454 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Nitrates and Sulfates," Appendix B.
See "Sulfates (Particulate)," Appendix B.
See "Sulfur Compounds (Particulate)," Appendix B
See "Thallium," Appendix B.
Soil/Sediment Samples
Laboratory Method"
See "Nitrates and Sulfates," Appendix B.
See "Thallium," Appendix B.
Water Samples
Laboratory Method
See "Thallium," Appendix B.
See "Sulfates," Appendix B.
A-259
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URANYL ACETATE (CAS Number 541-09-3)
RQ: 2270 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
See "Uranium," Appendix B.
A-260
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URANYL NITRATE (CAS Numbers 10102-06-4, 36478-76-9)
RQ: 2270 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Nitrate Ions," Appendix B.
Air Samples
Laboratory Method
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
See "Nitrates," Appendix B.
See "Uranium," Appendix B.
A-261
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VANADIUM PENTOXIDE (CAS Number 1314-62-1)
RQ: 454 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
METHOD SUMMARY:
Analysis for particulate vanadium pentoxide in air can be performed by
membrane-filtration of 25 liters of air, followed by alkaline digestion of the
sampling medium and analysis of the resulting solution for vanadium by atomic
absorption spectrometry (AA) using graphite-furnace atomization. The method
is specific for vanadium oxides, not vanadium metal.
INTERFERENCES:
There are no reported interferences.
QUALITY CONTROL:
A method blank should be processed with each set of 10 or fewer samples.
The percent recovery of spiked samples should be determined and, if it is less
than 95 percent, results should be corrected accordingly. Duplicate analyses
should agree within 5 percent.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH), and validated over the ranges of 0.2 to 0.9 milligrams per
cubic meter in a 25-liter air sample and 0.06 to 0.29 milligrams per cubic meter
in a 22.5-liter air sample. Precision and accuracy information is furnished.
A-262
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REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods. 2nd ed., Vol. 3, Method S391; Publication No. 77-157-C, U.S. DREW:
Cincinnati, 1977.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 4, Method S388; Publication No. 78-175, U.S. DHEW:
Cincinnati, 1978.
U.S. Department of Health, Education, and Welfare, Ten NIOSH Analytical Methods,
Set 1. Method S391; PB-271 712 (NTIS), U.S. DHEW: Cincinnati, 1977.
U.S. Department of Health, Education, and Welfare, Ten NIOSH Analytical Methods,
Set 2, Method S388; PB-271 464 (NTIS), U.S. DHEW: Cincinnati, July 1977.
COST INFORMATION;
Cost per sample for analysis by furnace AA is approximately $18-50 (list),
plus sampling costs.
Note: NIOSH Mehod P&CAM 290 (analysis by graphite furnace AA) is applicable.
(Reference furnished by reviewer).
See also: "Vanadium," Appendix B.
Soil/Sediment Samples
| Laboratory Method
See "Vanadium," Appendix B.
Water Samples
Laboratory Method
See "Vanadium," Appendix B.
A-263
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VANADYL SULFATE (CAS Number 27774-13-6)
RQ: 454 kg
SAFETY INFORMATION; Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Nitrates and Sulfates," Appendix B.
See "Sulfates (Particulate)," Appendix B.
See "Sulfur Compounds (Particulate)," Appendix B,
See "Vanadium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Nitrates and Sulfates," Appendix B.
See "Vanadium," Appendix B.
Water Samples
Laboratory Method
See "Sulfates," Appendix B.
See "Vanadium," Appendix B.
A-264
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RQ: 0.454 kg
SAFETY INFORMATION:
ZINC (CAS Number 7440-66-6)
Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Zinc and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
See "Zinc," Appendix B.
See "Zinc," Appendix B.
See "Zinc," Appendix B.
See "Zinc," Appendix B.
See "Zinc," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
A-265
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ZINC ACETATE (CAS Number 557-34-6)
RQ: 454 kg
SAFETY INFORMATION; Potentially chronically toxic.
Air Samples
Field Method
See "Zinc and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
See "Zinc," Appendix B.
See "Zinc," Appendix B.
See "Zinc," Appendix B.
See "Zinc," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Zinc," Appendix B.
A-266
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ZINC AMMONIUM CHLORIDE (CAS Numbers 52628-25-8, 14639-97-5, 14639-98-6)
RQ: 2270 kg
SAFETY INFORMATION; Potentially chronically toxic.
Air Samples
Field Method
See "Zinc and Compounds (Particulate)," Appendix B.
See "Zinc," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Ammonia," Appendix B.
See "Halides, Cyanides, and Other Compounds," Appendix B.
See "Volatile Species," Appendix B.
See "Zinc," Appendix B.
Air Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Zinc," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Zinc," Appendix B.
Water Samples
Laboratory Method
See "Ammonia," Appendix B.
See "Zinc," Appendix B.
A-267
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ZINC BORATE (CAS Number 1332-07-6)
RQ: 454 kg
SAFETY INFORMATION: Potentially chronically toxic.
Air Samples
Field Method
See "Zinc and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
See "Zinc," Appendix B.
See "Zinc," Appendix B.
See "Zinc," Appendix B.
See "Zinc," Appendix B.
See "Zinc," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
A-268
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ZINC BROMIDE (CAS Number 7699-45-8)
RQ: 2270 kg
SAFETY INFORMATION; Potentially chronically toxic.
Air Samples
Field Method
See "Zinc and Compounds (Particulate)," Appendix B.
See "Zinc," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Halides, Cyanides, and Other Compounds," Appendix B,
See "Zinc," Appendix B.
See "Zinc," Appendix
See "Zinc," Appendix B,
Air Samples
Laboratory Method
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
See "Zinc," Appendix B.
See "Iodides and Bromides," Appendix B,
A-269
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ZINC CARBONATE (CAS Number 3486-35-9)
RQ: 454 kg
SAFETY INFORMATION: Potentially chronically toxic.
Air Samples
Field Method
See "Zinc and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
See "Zinc," Appendix B.
Water Samples
Field Method
See "Halides, Cyanides, and Other Compounds," Appendix B.
See "Zinc," Appendix B.
See "Zinc," Appendix B.
See "Zinc," Appendix B.
See "Zinc," Appendix B.
Air Samples
Laboratory Method
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
A-270
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ZINC CHLORIDE (CAS Number 7646-85-7)
RQ: 2270 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Zinc and Compounds (Particulate)," Appendix B.
See "Zinc," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Halides, Cyanides, and Other Compounds," Appendix B.
See "Zinc," Appendix B.
Air Samples
Laboratory Method
See "Chlorides," Appendix B.
See "Zinc," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Zinc," Appendix B,
Water Samples
Laboratory Method
See "Chlorides," Appendix B,
See "Zinc," Appendix B.
A-271
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ZINC CYANIDE (CAS Number 557-21-1)
RQ: 4.54 kg
SAFETY INFORMATION; Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Zinc and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
See "Cyanides," Appendix B.
See "Zinc," Appendix B.
Water Samples
"Field Method"
See "Cyanides," Appendix B.
See "Halides, Cyanides, and Other Compounds," Appendix B.
See "Zinc," Appendix B.
Air Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Zinc," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Zinc," Appendix B.
Water Samples
Laboratory Method
See "Cyanides," Appendix B.
See "Zinc," Appendix B.
A-272
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ZINC FLUORIDE (CAS Number 7783-49-5)
RQ: 454 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Fluorides," Appendix B.
See "Zinc and Compounds (Particulate)," Appendix B.
See "Zinc," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Fluorides and Other Compounds," Appendix B.
See "Zinc," Appendix B.
Air Samples
Laboratory Method
See "Fluorides," Appendix B.
See "Fluorides and Hydrogen Fluoride," Appendix B.
See "Zinc," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Zinc," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B,
See "Fluorides," Appendix B.
See "Zinc," Appendix B.
A-273
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ZINC FORMATE (CAS Number 557-41-5)
RQ: 454 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Zinc and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
See "Zinc," Appendix B.
Water Samples
Field Method
See "Zinc," Appendix B.
See "Zinc," Appendix B.
See "Zinc," Appendix B.
Air Samples
Laboratory Method
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Zinc," Appendix B.
A-274
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ZINC HYDROSULFITE (CAS Number 7779-86-4)
RQ: 454 kg
SAFETY INFORMATION; Potentially chronically toxic.
Air Samples
Field Method
See "Zinc and Compounds (Particulate)," Appendix B.
See "Zinc," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Sulfite Ions," Appendix B.
See "Zinc," Appendix B.
Air Samples
Laboratory Method
See "Sulfur Compounds (Particulate)," Appendix B,
See "Zinc," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Zinc," Appendix B,
Water Samples
Laboratory Method
See "Sulfites," Appendix B.
See "Zinc," Appendix B.
A-275
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ZINC NITRATE (CAS Number 7779-88-6)
RQ: 2270 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Zinc and Compounds (Particulate)," Appendix B.
See "Zinc," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Nitrate Ions," Appendix B.
See "Zinc," Appendix B.
Air Samples
Laboratory Method
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
See "Zinc," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
See "Zinc," Appendix B.
Water Samples
Laboratory Method
See "Nitrates," Appendix B.
See "Zinc," Appendix B.
A-276
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ZINC PHENOLSULFONATE (CAS Number 127-82-2)
RQ: 2270 kg
SAFETY INFORMATION: Potentially chronically toxic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Phenolic Compounds," Appendix B.
See "Zinc and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
See "Phenolic Compounds," Appendix B.
See "Zinc," Appendix B.
See "Zinc," Appendix B.
See "Zinc," Appendix B.
See "Zinc," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
See "Zinc," Appendix B.
A-277
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ZINC PHOSPHIDE (CAS Number 1314-84-7)
RQ: 454 kg
SAFETY INFORMATION: Potentially chronically toxic. Forms toxic phosphine upon
contact with water.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Zinc and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
Reacts with water.
See "Zinc," Appendix B.
Water Samples
Field Method
Reacts with water.
See "Zinc," Appendix
Air Samples
Laboratory Method
See "Phosphorus," Appendix B.
See "Zinc," Appendix B.
Soil/Sediment Samples
Laboratory Method
Reacts with water.
See "Phosphorus," Appendix B.
See "Zinc," Appendix B.
Water Samples
Laboratory Method
Reacts with water.
A-278
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See "Phosphorus," Appendix B.
See "Zinc," Appendix B.
A-279
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ZINC SILICOFLUORIDE (CAS Number 16871-71-9)
RQ: 2270 kg
SAFETY INFORMATION: Potentially chronically toxic.
Air Samples
Field Method
See "Zinc and Compounds (Particulate)," Appendix B.
Soil/Sediment Samples
Field Method
See "Zinc," Appendix B.
See "Zinc," Appendix B.
See "Zinc," Appendix B.
See "Zinc," Appendix B.
Water Samples
Field Method
Air Samples
Laboratory Method
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
See "Fluorides," Appendix B.
See "Zinc," Appendix B.
A-280
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ZINC SULFATE (CAS Number 7733-02-0)
RQ: 454 kg
SAFETY INFORMATION: Potentially chronically toxic.
Air Samples
Field Method
See "Zinc and Compounds (Particulate)," Appendix B.
See "Zinc," Appendix B.
See "Zinc," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Nitrates and Sulfates," Appendix B.
See "Sulfates (Particulate)," Appendix B.
See "Sulfur Compounds (Particulate)," Appendix B,
See "Zinc," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Nitrates and Sulfates," Appendix B.
See "Zinc," Appendix B.
Water Samples
Laboratory Method
See "Sulfates," Appendix B.
See "Zinc," Appendix B.
A-281
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ZIRCONIUM NITRATE (CAS Number 13746-89-9)
RQ: 2270 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Nitrate Ions," Appendix B.
See "Zirconium," Appendix B.
Air Samples
Laboratory Method
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
See "Zirconium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Nitrates," Appendix B.
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
See "Nitrates," Appendix B.
A-282
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ZIRCONIUM POTASSIUM FLUORIDE (CAS Number 16923-95-8)
RQ: 454 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Fluorides," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method"
See "Fluorides and Other Compounds," Appendix B.
See "Potassium," Appendix B.
See "Zirconium," Appendix B.
Air Samples
Laboratory Method
See "Potassium," Appendix B.
See "Zirconium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Potassium," Appendix B.
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Fluorides," Appendix B.
See "Potassium," Appendix B.
A-283
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ZIRCONIUM SULFATE (CAS Number 14644-61-2)
RQ: 2270 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
See "Zirconium," Appendix B.
Air Samples
Laboratory Method
See "Nitrates and Sulfates," Appendix B.
See "Sulfur Compounds (Particulate)," Appendix B.
See "Zirconium," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Nitrates and Sulfates," Appendix B.
Water Samples
Laboratory Method
A-284
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ZIRCONIUM TETRACHLORIDE (CAS Number 10026-11-6)
RQ: 2270 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Reacts with water.
Water Samples
Field Method
Reacts with water.
See "Zirconium," Appendix B.
Air Samples
Laboratory Method
Reacts with water.
See "Zirconium," Appendix B,
Soil/Sediment Samples
Laboratory Method
Reacts with water.
Water Samples
Laboratory Method
Reacts with water.
A-285
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Part II: Organic Compounds
A-286
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ACENAPHTHENE (CAS Number 83-32-9)
R£: 0.454 kg
SAFETY INFORMATION: Potentially carcinogenic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Polycyclic Aromatic Hydrocarbons," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Acid and Base/Neutral Extractable Organics," Appendix B.
See "Polycyclic Aromatic Hydrocarbons," Appendix B.
Water Samples
Laboratory Method
See "Base/Neutral Extractable Organic Compounds," Appendix B,
See "Organic Compounds," Appendix B.
See "Polycyclic Aromatic Hydrocarbons," Appendix B.
See "Trace Organic Contaminants," Appendix B.
A-287
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ACENAPHTHYLENE (CAS Number 208-96-8)
RQ: 0.454 kg
SAFETY INFORMATION: Potentially carcinogenic.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
Soil/Sediment Samples
Laboratory Method
See "Acid and Base/Neutral Extractable Organics," Appendix B.
See "Polycyclic Aromatic Hydrocarbons," Appendix B.
Water Samples
Laboratory Method
See "Base/Neutral Extractable Organic Compounds," Appendix B.
See "Polycyclic Aromatic Hydrocarbons," Appendix B.
A-288
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ACETALDEHYDE (CAS Number 75-07-0)
R£: 454 kg
SAFETY INFORMATION: Flash point -38°F (-39°C).
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
METHOD SUMMARY:
Analysis for acetaldehyde in air may be performed by use of a detector
tube. A 2-liter air sample is collected and analyzed with a hand-operated
bellows pump and an acetaldehyde gas detector tube (Draeger® 67 26665, or
equivalent). A positive result is indicated by a color change in the tube from
orange to brownish-green.
INTERFERENCES:
Other aldehydes and easily oxidized organic compounds may also give
positive results.
QUALITY CONTROL;
No quality control procedures are given.
SENSITIVITY:
This method is sensitive to concentration levels of approximately 180 to
1800 milligrams per cubic meter.
REFERENCES:
National Draeger, Inc., Draeger® Detector Tube Handbook, "Air Investigations
and Technical Gas Analysis with Draeger® Tubes", 4th ed.; Draeger: Pittsburgh,
August 1979.
National Draeger, Inc., Bulletin No. ND-105; Draeger: Pittsburgh, January 1,
1982.
National Draeger, Inc., Measurements with Draeger® Tubes in the Threshold Limit
Value Range, Draeger® Gas Analysis Product Information, Leaflet 4340.3e; Draeger:
Pittsburgh, December 1981.
COST INFORMATION:
The cost per sample for analysis by this method is approximately $13-20
(list), plus sampling costs.
A-289
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See also: "Aldehydes," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
METHOD SUMMARY:
Acetaldehyde in water samples can be measured colorimetrically. The
Acetaldehyde reacts with propionaldehyde (3-pheny-12-quinoxalinyl)-hydrazone
in 95 percent ethanol to form a red product. Reaction is complete in 20 minutes.
The absorbance of the solution is read at 465 nm on a portable spectrometer.
INTERFERENCES:
Aromatic aldehydes, glucose, and ketones do not react.
QUALITY CONTROL
No quality control procedures are given.
SENSITIVITY
This method is suitable for acetaldehyde concentrations between approximately
2 and 44 milligrams per liter.
REFERENCE:
Tagami, S.; Nakamura, T.; Nakano, T.; Shiho, D. "Characteristic Detection and
Determination of Aliphatic Aldehydes," Chem. Pharm. Bull., 23/4), 1975, pp. 891-
894.
COST INFORMATION:
The cost per sample for analysis by this method is approximately $35-50
(list).
See also: "Volatile Species," Appendix B.
Air Samples
Laboratory Method
METHOD SUMMARY:
Infrared absorption spectrometry can be used to determine the concentration
of acetaldehyde in air samples. The absorbance at 8900 nm (1123 cm~l) is
measured, using a 10-meter pathlength cell. Air can be sampled in a Saran® or
A-290
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Mylar® plastic bag: approximately 5 liters of the sample are drawn into an
evacuated cell. Continuous monitoring of air flowing through the cell is
possible if the spectrometer is set to one particular wavelength. Some vapors
can be adsorbed on silica gel and quantitatively desorbed into the absorption
cell later. Tentative qualitative identification of compounds can be made
based on a full infrared absorption spectrum.
INTERFERENCES:
Compounds present in the sample that absorb infrared radiation at the
wavelength of interest will interfere.
QUALITY CONTROL;
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The sensitivity of the method, using a
10-meter pathlength cell, is 55 milligrams per cubic meter. No precision or
accuracy information is furnished.
REFERENCE:
American Public Health Association, "Infrared Absorption Spectroscopy," In
Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington,
1977, pp. 79-84.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $75-85
(list), plus sampling costs.
Note: NIOSH Method S345 (bubbler collection, derivatization with Girad T
reagent, analysis by HPLC) is applicable. (Reference furnished by
reviewer).
See also: "Aliphatic Aldehydes," Appendix B.
See also: "Halogenated, Aromatic and Other Compounds," Appendix B.
See also: "Hazardous Organic Emissions," Appendix B.
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
See "Aliphatic Compounds," Appendix B.
See "Organic Compounds," Appendix B.
See "Volatile Alcohols and Other Organic Compounds," Appendix B,
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See "Volatile Carbonyl Compounds," Appendix B.
See "Volatile Organics," Appendix B.
A-292
-------
ACETIC ACID (CAS Number 64-19-7)
Rpj 2270 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See j'Acetic Acid and Acetic Anhydride," Appendix B.
See "Volatile Organic Compounds," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method 1
METHOD SUMMARY:
Gas chromatography may be used for the determination of acetic acid in air
samples. The analysis is performed by passage of a known volume of air through
a charcoal-tube sampling device, followed by desorption of the analyte with
formic acid, and analysis of the resulting solution by gas chromatography with
flame ionization detection (GC/FID).
INTERFERENCES:
Any compound with the same retention time as acetic acid is an interferent.
QUALITY CONTROL:
Desorption efficiency must be determined over the range of interest, and a
method blank should be processed with each 10 samples. The desorption efficiency
and the results of the method-blank analysis should be used in the calculation of
the results.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH) , and validated over the range of 12.5 to 50 milligrams per
cubic meter, using a 173-liter sample. The method is capable of measurement of
lower levels if the desorption efficiency is adequate. Precision and accuracy
information is furnished.
A-293
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REFERENCE:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 4, Method S169; Publication No. 78-175, U.S. DREW:
Cincinnati, August 1978.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $70-90
(list), plus sampling costs.
Air Samples
Laboratory Method 2
METHOD SUMMARY:
Infrared absorption spectrometry can be used to determine the concentra-
tion of acetic acid in air samples. The absorbance at 8500 nm (1176 cm~l) is
measured, using a 10-meter pathlength cell. Air can be sampled in a Saran® or
Mylar® plastic bag; approximately 5 liters of the sample are drawn into an
evacuated cell. Continuous monitoring of air flowing through the cell is
possible if the spectrometer is set to one particular wavelength. Some vapors
can be adsorbed on silica gel and quantitatively desorbed into the absorption
cell later. Tentative qualitative identification of compounds can be made
based on a full infrared absorption spectrum.
INTERFERENCES:
Compounds present in the sample that absorb infrared radiation at the
wavelength of interest will interfere.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The sensitivity of the method, using a
10-meter pathlength cell, is 12 milligrams per cubic meter. No precision or
accuracy information is furnished.
REFERENCE:
American Public Health Association, "Infrared Absorption Spectroscopy" In
Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington,
1977, pp. 79-84.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $75-85
(list), plus sampling costs.
A-294
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?ee a*SO: "Halogenated, Aromatic and Other Compounds," Appendix B.
§ee also: Volatile Organic Compounds," Appendix B.
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
See "Acid Anions," Appendix B.
See "Aliphatic Compounds," Appendix B.
See "Carboxylic Acids," Appendix B.
See "Organic Acids," Appendix B.
See "Volatile Organic Acids," Appendix B.
A-295
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ACETIC ANHYDRIDE (CAS Number 108-24-7)
ROj 2270 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Acetic Acid and Acetic Anhydride," Appendix B.
See "Volatile Organic Compounds," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
METHOD SUMMARY:
Analysis for acetic anhydride in air is performed by collection of the
acetic anhydride from 100 liters of air in a midget bubbler and colorimetric
analysis of the resulting solution. The bubbler is charged with an alkaline
hydroxylamine solution, and iron(III)chloride is used to develop color in the
solution. This method is a source method for high concentrations of acetic
anhydride.
INTERFERENCES:
Substances containing a carbonyl group (such as aldehydes, esters, acid
chlorides, and ketones) interfere. The most likely potential interference is
ketene because it is likely to coexist with acetic anhydride in air.
QUALITY CONTROL:
A method blank should be analyzed with each set of samples.
EPA/TECHNICAL STATUS:
The method is approved by the National Institute for Occupational Safety
and Health and has been validated over the range of 9 to 37 milligrams per
cubic meter. The method is capable of measurement of lower concentrations by
A-296
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1186 rfria?8r SamPl6S °r a 10nger absorption-cell pathlength. Precision and
accuracy information is furnished.
REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 3, Method S170; Publication No. 77-157-C, U.S. DHEW:
Cincinnati, 1977.
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Method for
Set L' Method S170' PB-250 159 (NTIS), U.S. DHEW: Washington, January 1976.
COST INFORMATION:
The cost per sample for analysis by this method is approximately
$20-25 (list), plus sampling costs.
See also: "Halogenated, Aromatic, and Other Compounds," Appendix B.
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
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ACETONE (CAS Number 67-64-1)
ROj 2270 kg
SAFETY INFORMATION: Flash point -4°F.
Air Samples
Field Method
See "Acetone and Methyl Ketones," Appendix B.
See "Volatile Organic Compounds," Appendix B.
See "Organic Vapors," Appendix B.
Soil/Sediment Samples
Field Method
See "Volatile Species," Appendix B.
Water Samples
Field Method
See "Volatile Species," Appendix B.
Air Samples
Laboratory Method 1
METHOD SUMMARY:
Analysis for acetone in air is performed by passage of a known volume of
air through a charcoal-tube sampling device, followed by desorption of the
analyte with carbon disulfide and analysis of the resulting solution by gas
chromatography with flame ionization detection (GC/FID).
INTERFERENCES:
High humidity severely decreases the capacity of the sampling apparatus.
QUALITY CONTROL:
Desorption efficiency must be determined over the range of interest, and a
method blank should be processed with every 10 samples. The desorption effi-
ciency and the results of the method-blank analysis should be used in the calcu-
lation of the results.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH), and has been validated over the range of 1200 to 4500
milligrams per cubic meter, using a 2-liter sample. Precision and accuracy
information is furnished. The method is capable of measurement of much lower
levels if the desorption efficiency is adequate.
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REFERENCES;
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 2, Method SI; Publication No. 77-157-B, U.S. DHEW:
Cincinnati, 1977.
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set A' Method S15 PB-245 850 (NTIS). U.S. DHEW: Washington, October 1975.
COST INFORMATION:
The cost per sample for analysis by this method is approximately
$70-90, plus sampling costs.
Air Samples
Laboratory Method 2
METHOD SUMMARY:
Infrared absorption spectrometry can be used to determine the concentra-
tion of acetone in air samples. The absorbance at 8200 nm (1219 cm"!) is
measured, using a 10-meter pathlength cell. Air can be sampled in a Saran© or
Mylar® plastic bag; approximately 5 liters of the sample are drawn into an
evacuated cell. Continuous monitoring of air flowing through the cell is
possible if the spectrometer is set to one particular wavelength. Some vapors
can be adsorbed on silica gel and quantitatively desorbed into the absorption
cell later. Tentative qualitative identification of compounds can be made
based on a full infrared absorption spectrum.
INTERFERENCES:
Compounds present in the sample that absorb infrared radiation at the
wavelength of interest will interfere.
QUALITY CONTROL:
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The sensitivity of the method, using a
10-meter pathlength cell, is 12 milligrams per cubic meter. No precision or
accuracy information is furnished.
REFERENCE:
American Public Health Association, "Infrared Absorption Spectroscopy." In
Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington,
1977, pp. 79-84.
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COST INFORMATION:
Cost per sample for analysis by this method is approximately $75-85 (list),
plus sampling costs.
See also: "Halogenated, Aromatic, and Other Compounds," Appendix B.
See also; "Hazardous Organic Emissions," Appendix B.
See also: "Volatile Carbonyl Compounds," Appendix B.
See also: "Volatile Organic Compounds," Appendix B.
See also: "Volatile Organic Solvents," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Volatile Organic Compounds," Appendix B.
Water Samples
Laboratory Method
See "Aliphatic Compounds," Appendix B.
See "Organic Compounds," Appendix B.
See "Volatile Alcohols and Other Organic Compounds," Appendix B.
See "Volatile Carbonyl Compounds," Appendix B.
See "Volatile Organic Compounds," Appendix B.
See "Volatile Organics," Appendix B.
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ACETONE CYANOHYDRIN (CAS Number 75-86-5)
RQ: 4.54 kg
SAFETY INFORMATION: CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Volatile Organic Compounds," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
METHOD SUMMARY:
Acetone cyanohydrin can be detected in water samples by visible spectro-
photometry. Copper sulfate solution and ammonia are added to a water sample,
and the blue tetraamine copper complex is destroyed by acetone cyanohydrin.
(This method is described by Legradi, L. Mikrochim.Acta 4, 1974, pp. 759-764,
and is summarized in the reference given below.)
INTERFERENCES:
No interferences are reported.
QUALITY CONTROL;
No quality control procedures are given.
SENSITIVITY:
This method is sensitive to concentration levels of acetone cyanohydrin
higher than 50 micrograms.
REFERENCE:
Simons, J. R. Bibliography on Hazardous Materials Analysis Methods; EPA 600/2-
81-094, U.S. Environmental Protection Agency: Cincinnati, 1981, p. 12.
COST INFORMATION:
The cost per sample for analysis by this method is approximately $15-23
(list).
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See also: "Halides, Cyanides, and Other Compounds," Appendix B.
Air Samples
Laboratory Method
METHOD SUMMARY:
Gas chromatography may be used for the analysis of acetone cyanohydrin in
air samples. A known volume of air is drawn through a tube containing Porapak QS®,
followed by desorption with ethyl acetate. An aliquot of the resulting solution
is injected into a gas chromatograph equipped with a nitrogen-phosphorus detector
(GC/NPD).
INTERFERENCES:
Samples taken in humid atmospheres should be refrigerated immediately to
protect the analyte from decomposition in the presence of water vapor.
QUALITY CONTROL:
Method blanks and standards are processed with the samples.
EPA/TECHNICAL STATUS:
This method has been proposed by the National Institute for Occupational
Safety and Health (NIOSH) for use over the range of 0.33 to 16.7 milligrams
per cubic meter for a 3-liter sample. Precision and accuracy information is
furnished. This method should be applicable over a broader range of concentra-
tions, provided that good desorption efficiency can be achieved.
REFERENCE:
U.S. Department of Health and Human Services, NIOSH Manual of Analytical
Methods, Vol. 7, Method P&CAM 340; Publication No. 82-100, U.S. DHHS:
Cincinnati, August 1981.
COST INFORMATION:
Cost per sample for analysis by this method is approximately $130 (list),
plus sampling costs.
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
See "Substituted Nitriles and Tetranitromethane," Appendix B,
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ACETONITRILE (CAS Number 75-05-8)
R£: 454 kg
SAFETY INFORMATION: Exhibits chronic toxicity. Flash point 42°F.
CAUTION: The user should obtain additional toxicity/hazard
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Organic Vapors," Appendix B.
See "Volatile Organic Compounds," Appendix B.
Soil/Sediment Samples
Water Samples
Field Method
Air Samples
Laboratory MeFhod 1
METHOD SUMMARY:
Analysis for acetonitrile in air is performed by passage of a known volume
of air through a charcoal-tube air sampler, followed by desorption of the
analyte with benzene and gas chromatographic analysis with flame ionization
detection (GC/FID) of the resulting solution.
INTERFERENCES:
High humidity severely decreases the efficiency of the sampling apparatus.
QUALITY CONTROL:
Desorption efficiency must be determined and results corrected accord-
ingly. A method blank should be analyzed with each set of samples and the
results used to correct the data for each sample.
EPA/TECHNICAL STATUS:
This method is approved by the National Institute for Occupational Safety
and Health (NIOSH) , and validated over the range of 30 to 140 milligrams per
cubic meter in a 10-liter sample. The method should be applicable over a
broader range of concentrations, provided that good desorption efficiency can
be achieved. Precision and accuracy information is furnished.
A-30 3
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REFERENCES:
U.S. Department of Health, Education, and Welfare, NIOSH Analytical Methods for
Set L, Method S165; PB-250 159 (NTIS), U.S. DHEW: Washington, January 1976.
U.S. Department of Health, Education, and Welfare, NIOSH Manual of Analytical
Methods, 2nd ed., Vol. 3, Method S165; Publication No. 77-157-C, U.S. DHEW:
Cincinnati, 1977.
COST INFORMATION:
The cost per sample for analysis by this method is approximately $70-90
(list), plus sampling costs.
Air Samples
Laboratory Method 2
METHOD SUMMARY:
Infrared absorption spectrometry can be used to determine the concentra-
tion of acetonitrile in air samples. The absorbance at 9580 nm (1044 cm~l) is
measured, using a 10-meter pathlength cell. Air can be sampled in a Saran® or
Mylar® plastic bag; approximately 5 liters of the sample as drawn into an
evacuated cell. Continuous monitoring of air flowing through the cell is
possible if the spectrometer is set to one particular wavelength. Some vapors
can be adsorbed on silica gel and quantitatively desorbed into the absorption
cell later. Tentative qualitative identification of compounds can be made
based on a full infrared absorption spectrum.
INTERFERENCES:
Compounds present in the sample that absorb infrared radiation at the
wavelength of interest will interfere.
QUALITY CONTROL;
No quality control procedures are given.
EPA/TECHNICAL STATUS:
This method is not EPA-approved. The sensitivity of the method, using a
10-meter pathlength cell, is 160 milligrams per cubic meter. No precision or
accuracy information is furnished.
REFERENCE:
American Public Health Association, "Infrared Absorption Spectroscopy." In
Methods of Air Sampling and Analysis, 2nd ed., M. Katz, Ed.; APHA: Washington,
1977, pp. 79-84.
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COST INFORMATION:
Cost per sample for analysis by this method is approximately $75-85
(list), plus sampling costs.
See also: "Gaseous Contaminants," Appendix B.
See also: "Halogenated, Aromatic, and Other Compounds," Appendix B.
Soil/Sediment Samples
Laboratory Method
See "Non-Halogenated Volatile Organic Compounds," Appendix B.
Water Samples
Laboratory Method
See "Nitriles," Appendix B.
See "Non-Halogenated Volatile Organic Compounds," Appendix B.
See "Organic Compounds," Appendix B.
See "Volatile Alcohols and Other Organic Compounds," Appendix B.
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ACETOPHENONE (CAS Number 98-86-2)
RQ: 2270 kg
SAFETY INFORMATION; CAUTION: The user should obtain additional toxicity/hazar(
information before handling this substance or
using this analytical procedure.
Air Samples
Field Method
See "Volatile Organic Compounds," Appendix B.
Soil/Sediment Samples
Field Method
Water Samples
Field Method
Air Samples
Laboratory Method
See "Halogenated, Aromatic, and Other Compounds," Appendix B.
See "Hazardous Organic Emissions," Appendix B.
Soil/Sediment Samples
Laboratory Method
Water Samples
Laboratory Method
See "Trace Organic Contaminants," Appendix B.
See "Volatile Alcohols and Other Organic Compounds," Appendix B,
A-306
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