United States
Environmental Protection
Agency
Office of Emergency and
Remedial Response
Washington DC 20460
EPA/540/2-88/005
September 1 9 i
Superfund
Field Screening
Methods Catalog
User's Guide
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EPA/540/2-88/005
September 1988
Field Screening Methods Catalog
User's Guide
Office of Emergency and Remedial Response
Hazardous Site Evaluation Division
U.S. Environmental Protection Agency
Washington, DC 20460
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NOTICE
The information in this document has been funded, wholly or in part, by the United
Slates Environmental Protection Agency under Contract No. 66-01-6939 to COM
Federal Programs Corporation and Roy F. Weston inc. It has been subject to the
Agency's peer and administrative review and has been approved for publication as
an EPA document. Mention of trade names or commercial products does not neces-
sarily constitute endorsement or recommendation for use.
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EXECUTIVE SUMMARY
The Field Screening Methods Catalog (FSMC) is a technical document produced by
the United States Environmental Protection Agency's Office of Emergency and
Remedial Response - Analytical Operations Branch. This document is a compila-
tion of methods that were identified as being used in EPA Regions. Several methods
contain no method performance information, because this information was not avail-
able. The methods are provided as submitted by the technical contact listed in the
method description. The Analytical Operations Branch has not evaluated the meth-
ods contained in this document, but has simply compiled existing methods.
The methods presented in this Catalog should not be viewed as Standard Operating
Procedures (SOP) but rather as a compilation of available technologies which have
been successfully utilized on a site-specific basis. Prior to the application of any of
these methods, the user is urged to consult with the technical contact listed for each
method, and an analytical chemist familiar with both the instrumentation/method and
the specific conditions inherent to the site under consideration. It is also critical that
an assessment be made of these site specific conditions, and how they may effect
the utility of the method and the resulting data quality.
The FSMC is available to users, particularly those individuals responsible for devel-
oping and overseeing sampling activities at Superfund hazardous waste sites, e.g.,
Regional Project Managers (RPMs) and contractor Site Managers (SMs). The
Catalog currently consists of a User's Manual Including a listing of all methods, a
"pocket guide," a field screening methods data base and a computerized informa-
tion retrieval system contained on two floppy discs. The discs are not included with
this User's Guide but will be distributed separately to EPA Regional Offices for
further distribution as the Region sees fit. Information on how to acquire copies of
the discs is available from the EPA Headquarters FSMC Systems Coordinator -
Analytical Operations Branch (WH548A).
The Catalog was developed to assist the user in identifying field screening methods
applicable to specific site characteristics. The computer system was developed.
using dBase III Plus and operates on an IBM compatible microcomputer. The user
may search for field methods by entering selection criteria, including chemical class,
name, or CAS number, method name or number, matrix type (air, soil, and/or water)
and a minimum detection limit.
It is important to note that the methods presented in this Catalog are an option
available to RPMs and SMs; the methods are not designed to "take the place" of
other analytical options. They are intended to supplement existing methods and
provide options based on the specific needs of the sampling/analytical activity.
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Based on the anticipated momentum that the FSMC will generate within the Agency
and in the private sector, this Catalog is provisional and is expected to be revised
and updated as more information becomes available on existing screening/analytical
techniques, and as new techniques are developed, tested and applied to field
analysis at hazardous waste sites.
In order to develop a historic data base on the range of data quality achieved by
each method it is critical that users conduct sufficient QC analysis to allow a deter-
mination of data quality as defined by precision and accuracy. Additional information
which will assist in defining the overall utility of the method includes method detec-
tion limits (sensitivity determination), matrix effects, interferences, as well as any
sample preparation/processing specifications and overall operator assessment of the
method. It Is requested that as this type of information is developed, It be forwarded
to the FSMC System Coordinator. A User Comment form has been included in
Appendix C.
IV
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FIELD SCREENING METHODS Catalog (FSMC)
TABLE OF CONTENTS
1.0 Introduction and Background 1
1.1 Field Screening Methods Catalog 3
1.2 Intended Users 5
1.3 System Updates 5
1.4 Technical Considerations 5
1.5 Overview of Levels I and II Analysis 10
2.0 Installing the System 14
2.1 Installation on a Two Disk Drive Computer System 14
2.2 Installation on a Hard Drive Computer System 15
2.3 Installing FSMC More Than Once 16
3.0 Getting Started 17
3.1 Searching the Data Base 16
3.1.1 Searching by Chemical Name 19
3.1.2 Searching by Chemical Abstract Services Number
20
3.1.3 Searching by Chemical Class 21
3.1.4 Searching by Method Name or Number 22
3.1.5 Searching by the Sample Matrix 23
3.1.6 Searching by the Detection Limit Values and
Units 23
4.0 Displaying and Printing Reports 24
5.0 FSMC System Requirements 25
5.1 Software Characteristics 25
5.2 Hardware Requirements 25
Appendix A
Field Method Listing
Appendix B
Historic Precision and Accuracy Data
Appendix C
User Comment Form
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LIST OF FIGURES
3-1 Main Menu is
3-2 Searching by Chemical Name 19
3-3 Searching by CAS Number 20
3-4 Searching by Chemical Class 21
3-5 Searching by Method Name 22
VI
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LISTING OF METHODS
PRIMARY METHODS
FM-I Field Atomic Absorption Analysis 1
FM-2 X-Ray Fluorescence in Laboratory for Heavy Metals 3
FM-3 X-Ray Fluorescence for Heavy Metals (On-site). 5
FM-4 Air Monitoring for Volatile Organic Compounds Using
Programmed Thermal Desorption and GC 7
FM-5 Volatile Organic Compound Analysis Using GC with
Automated Headspace Sampler 9
FM-6 Headspace Technique Using an Ion Detector for VOC Analysis. 11
FM-7 Headspace Technique Using an OVA for VOCs. 13
FM-8 Headspace Analysis Using HNU for Total Volatile Organics... 15
FM-9 Headspace Technique Using a Mobile GC for VOCs 17
FM-10 Passive Soil Gas Sampling Using Industrial Hygiene Samplers 19
FM-11 Soil Gas Sampling Using Mini-Barrel Sampler 21
FM-12 Soil Gas Sampling Using a One-Liter Syringe. 23
FM-13 Soil Gas Sampling Using Direct Injection - Stopper. 25
FM-14 Soil Gas Sampling Using a Perforated Tube 27
FM-1 5 Soil Gas Sampling Using Tenax Tubes 29
FM-16 Soil Gas Sampling for Downhole Profiling. 31
FM-17 Soil Gas Sampling Direct Injection - Auger 33
FM-18 PCB Analysis Using a Gas Chromatograph in an On-Site
Laboratory - Hexane/Methano/WaterExtractlon. 35
FM-19 PC6 Analysis Using a Gas Chromatograph In an On-Site
Laboratory - Hexane Extraction. 37
FM-20 PCS Analysis Using a Gas Chmatograph in an On-Site
Laboratory - Hexanel/Methanol 39
FM-21 PCB Analysis Using a Gas Chromatograph in an On-Site
Laboratory - Hexane/Acetone Extraction 41
FM-22 Pesticide Analysis Using a GC with ECD - Hexane/Methanol
Extraction 43
FM-23 Pesticide Analysis Using Isothermal GC with ECD - Hexane
Extraction 45
FM-24 Phenol Determination by Liquid-Liquid Extraction and GC Analysis 47
FM-25 PAH Analysis Using GC with Heated Column 49
FM-26 Total PNA Analysis Using an Ultraviolet Fluorescence
Spectrophotometer 51
vil
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METHODS UNDER DEVELOPMENT
FM-D1 Trace Atmospheric Gas Analyzer (TAGA) 53
FM-D2 Use of Bonded Sorbents for Pesticide Analysis 57
FM-D3 Use of Bonded Sorbents for Semi-Volatile Analysis 59
FM-D4 Immunoassays for Trace Organic Analysis 61
FM-D5 Use of Fiber Optic Sensors in Environmental Monitoring 63
Viii
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ACKNOWLEDGMENTS
This document was developed for the Office of Emergency and Remedial Response
(OSWER), Hazardous Site Evaluation Division with assistance from the following
individuals:
Carla Dempsey (U.S. EPA Hazardous Site Evaluation Division)
David Bennett (U.S. EPA Toxic Integration Branch)
Andrew P. Szilagyi (COM Federal Programs Corporation)
Claire M. Gesalman (Roy F. Weston Inc.)
Brian Dougherty (Roy F. Weston Inc.)
The following individuals were largely responsible for the technical development of
the field screening/analytical methods:
Thomas Spittler (U.S. EPA Region I Laboratory)
Tom Pritchett (U.S. EPA Emergency Response Team)
S.H. Mo (New York State Department of Environmental Conservation)
William Loy (U.S. EPA Region IV Environmental Services Division)
James Jerpe (U.S. EPA Region III Central Regional Laboratory)
Lisa Gatton-Vidulich (U.S. EPA Region II Monitoring Management Branch)
John Kinrade (Scintrex Limited)
Richard Chappell (Camp Dresser & McKee Inc.)
Henry Kerfoot (Lockheed Engineering and Management Services Co. Inc.)
Steve Simon (Lockheed Engineering and Management Services Co. Inc.)
Andrew Hafferty (Ecology and Environment Inc.)
Hunt Chapman (Ecology and Environment Inc.)
John Ryding (C.C. Johnson & Malhotra)
Stacie Popp (Roy F. Weston Inc.)
Patricia Gardner (Analytichem International)
Joseph Paladino (Westinghouse Bio-Analytic Systems Company)
Helpful suggestions and comments on the draft document were provided by the
following, as well as other EPA and contractor staff:
Jeffery Sullivan (Camp Dresser & McKee inc.)
Joan Fisk (U.S. EPA Hazardous Site Evaluation Division)
Dennis Wesolowskl (U.S. EPA Region V)
Lisa Woodson Feldt (U.S. EPA Hazardous Site Control Division)
William Venit (U.S. EPA Region VI)
Herbert Moseley (U.S. EPA Systems Coordination Section)
P.K. Chattapadhyay (Ecology and Environment Inc.)
ix
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1.0 INTRODUCTION AND BACKGROUND
The United States Environmental Protection Agency (EPA) awarded the first two
major hazardous waste contracts in 1979. Since that time, the scope and nature of
hazardous waste Investigations have grown and matured. The culmination of this
maturation process is the present day Super-fund Program, as amended by the
Superfund Amendments and Reauthorization Act of 1988 (SARA).
Throughout this period of maturation, the basic initial (yet complex) premise of field
investigations has remained the same - to determine the chemical constitue its
(identity and quantitation) in environmental media (air, soil, water) as well as
"source" media such as sludges, and materials from containers including drums and
tanks. An additional complexity, which became evident as field investigations were
initiated, was the frequent need for "rapid turnaround" of sample analysis results.
This was critical, for example, to evaluate if emergency response was necessary.
The Contract Laboratory Program (CLP) was established by EPA to provide analyti-
cal support for the massive amount of data that was being generated by the nu-
merous hazardous waste sites throughout the country. This program provides a
range of analytical chemistry services of known quality on a high-volume, cost-
effective basis. The central and overriding assumption governing the structure and
function of the CLP is the basic requirement to provide legally-defensible analytical
results for use in supporting Agency actions. As of early 1987, the CLP was "able to
provide over 6,000 sample analyses per month through its Routine and Specialized
Analytical Services (RAS and SAS) Programs". Based on the "central and overriding
assumption. ... to provide legally-defensible analytical results. ., "CLP data deliverable
packages are accompanied by very specific documentation containing information
which includes initial and continuing calibration, GC/MS tuning, surrogate percent
recovery, matrix spike duplicate results, GC chromatograms, Furnace AA analysis,
digestion/distillation logs, ICP interference and serial dilution analysis, and spectra
for every sample and every blank, standard, or spike run with a particular set of
samples. Data delivery for this complete data package takes approximately 3540
days after submission. An additional 30 days for Regional review of each data pack-
age is also required. Faster turn-around times can be achieved through the SAS and
through expedited review by the Regions.
It is now recognized in the scientific/regulatory community that, frequently, the ap-
proximately 65-70 day turn-around in sample analyses is unacceptable, and that the
"quality" of data provided by the CLP is not required for ail samples. Two distinct
developments within EPA address this concern: first, the increasing use of field
screening/analytical methods, and second, the issuance of the Data Quality
Objectives for Remedial Response Activities (EPA, 1987 - OSWER Directive 9355.0-
7A). The development of field analytical methods was initiated early in the hazardous
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waste program history. The FITS developed and used field analytical techniques, first
for health and safety related (air) monitoring and subsequently for sample screening
and analyses of increasing complexity. This use of field methods was frequently
performed in conjunction with EPA laboratories and the Environmental- Response
Teams (ERTs). As such, initial use of Instruments such as the Foxboro Organic
Vapor Analyzer (OVA) and the HNu Systems HNu 101 were limited to air monitoring
to determine levels of safety protection. This initial use of field instrumentation made
the FITs and ERTs familiar with the capability of these and other instruments and
paved the way for their use as analytical tools in the Superfund Program.
The second development, while discussed for many years, was initiated and codified
in 1986 with the issuance of a number of EPA sponsored documents, the foremost of
which were the Data Quality Objectives for Remedial Response Activities (EPA, 1987 -
OSWER Directive 9355-0-7A) and A Compendium of Superfund Field Operations
Methods (EPA 1987a - OSWER Directive 9355.0-14). Data Quality Objectives (DQOs)
recognize and promote the concept that In the course of a typical Superfund reme-
dial investigation, samples are taken with various objectives and that these various
objectives require different "data quality". In other words, not all objectives require,
for example, CLP quality data. While DQOs present a framework for identifying and
achieving site specific data quality objectives through the appropriate sampling and
analytical techniques, the Compendium "focuses primarily on (sampling) techniques
and methods used during the fieldwork phase of a remedial investigation."
DQOs define five levels of analytical support which are available for sample analysis.
These levels are based on numerous factors, Including and foremost, data quality
requirements. These five levels of analytical support are defined as Levels I through
V and range from hand-held equipment and screening techniques to sophisticated
GUMS instrumentation and analysis. Specific discussions of these analytical levels,
their applicability, and limitations, as well as specific directions for use are contained
in both the Compendium of Superfund Field Operations Methods and in the Data
Quality Objectives for Remedial Response Activities (EPA, 1987a - OSWER Directive
9355.0-14, 1987 - OSWER Directive 9355.0-7A). In addition, a brief overview of these
five analytical levels is Included in Sections 1.4 and 1.5. It should be noted that no
clear delineation exist, especially between Levels I and II analysis. As a general
rule-of-thumb, Level I analysis typically result in qualitative measurements for the
presence or absence of classes of contaminants (typically volatile organics, although
specific compounds can also be measured in certain instances), while Level II
analyses can provide qualitative and frequently quantitative values for both groups
and specific analytes. At times, the same instrument can be used for both Levels I
and li analyses. For example, an OVA (a flame ionization organic vapor detector) can
be used in the "survey mode" for Level I analyses to measure total organic vapor. In
the GO mode, this same instrument can be used to obtain Level II data of specific
analytes.
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1.1 FIELD SCREENING METHODS CATALOG
One of the primary reasons for Superfund (as well as RCRA and other EPA pro-
grams) contamination monitoring at potential and known hazardous waste sites is the
determination of the identity, concentrations and vertical and horizontal extent of
chemical contamination. An essential element of any monitoring effort is analytical
support that provides rapid sample throughput while matching the data quality objec-
tives of the sampling effort.
Experience gained during the first five years of the Superfund program has shown
that various types of field screening/analytical methods are suitable and are being
used during field investigations to characterize "hot spots," evaluate the necessity of
emergency response, define general site conditions, assist in well placement and
screen setting, aid in the selection of sampling locations, compare off- and on-site
conditions, estimate potential population exposures, determine the completeness of
cleanup actions' (such as excavations), and establish long-term monitoring.
Presently, field screening/analytical techniques are routinely being used throughout
the Superfund program. However, because of the decentralized nature of the pro-
gram, knowledge and skills gained in one region or state, or even at one site, are not
necessarily transferred to others. Many personnel responsible for developing/
overseeing site sampling efforts need to have timely and accurate information re-
garding the availability of appropriate analytical methods. To meet this need and to
facilitate transfer of information about methods for measuring and screening chemi-
cals in the field, the United States Environmental Protection Agency has developed
the Field Screening Methods Catalog (FSMC).
To date, thirty-one methods have been compiled and documented in the Catalog. Of
the thirty-one methods contained in this Catalog, four are in the developmental stage
(Use of Bonded Sorbents for Pesticide Analysis, Use of Bonded Sorbents for Semi-
Volatile Analysis, immunoassays for Trace Organic Analysis, and Use of Fiber Optic
Sensors in Environmental Monitoring) and one (Trace Atmospheric Gas Analyzer -
TAGA) cannot truly be considered a viable "field method" due to its size, limited
availability, and cost. However, since these methods represent an available tech-
nology they have been retained in this Catalog in a separate section. These five
methods have not been segregated in the computerized data base and as such will
be selected when the appropriate parameters are input, in considering the applica-
bility of these five methods, the user should be aware of the above mentioned
limitations, and take sufficient CWQC steps to allow an assessment of data quality to
be performed.
For the purposes of this Catalog, the term "field methods" is used as a catch-ail
phrase and includes methods which utilize hand held instrument and/or instruments
which can be carried with relative ease, portable instruments which can be set up
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and used in the back of a van or field trailer, and fieldable instruments which usually
require a more stationary and stable environment such as a field (mobile) laboratory.
These terms are defined in more detail in Section 1.5.
The methods presented in this Catalog include analyses for metals, volatile and
semi-volatile organics, phenols, pesticides, PCBs, dioxins and polycyclic aromatic
hydrocarbons. In addition, several soil gas sampling techniques have been included
because of the expanding use of such techniques.
The FSMC consists of a reduced "pocket guide," a computerized retrieval system
stored on two floppy disks and a user's guide. The pocket guide was designed for
field personnel and provides a concise description of each method which provides
field staff with the information needed to consider the range of analytical methods
that might be appropriate for the site. The computer program is written on dBase III,
is IBM compatible, and provides search capabilities according to chemical of interest
(class, name or CAS number) or method name or number. The search options also
prompt the user to select a matrix of Interest (air, soil and/or water) and a detection
limit to match and provide an available method that will meet the need of the user as
closely as possible. Once a method or methods that can potentially meet the user's
need is found, a number of options are available to view and/or print the method(s).
These options are discussed in more detail in Section 4.0. In addition, this volume
provides an Introduction, a computer user's guide, including an appendix containing
copies of the thirty-one methods.
For ease of use and consistency, a standard set of "Fields" (or major headings)
have been developed to organize method specific information. These information
provided for each method include the following:
Method name and number (number is specific to this Catalog);
Summary and method description;
* Application, limitations, and instrumentation used;
« Performance specifications such as detection limits, selectivity, ac-
curacy, precision and repeatability;
•* Use of the method (location, CERCLIS site number [where appropriate],
and matrix);
* Preparation, maintenance, and cleanup;
* Calibration;
* Analysis time;
* Capital costs; and
^ Source of technical information.
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It is important to note that these fields specify the parameters that have been utilized
in the development and subsequent use of the methods and not necessarily the only
possible choices. For example, the Instrument Used field for PCB Analysis Using a
Gas Chromatograph in an On-Site Laboratory - Hexane Extraction, shows that a
Hewlett-Packard 5880 Gas Chromatograph with an electron capture detector was
used. However any GC with analogous capabilities could be used to perform this
analysis, Caution should however be used to assure that modifications to the method
will not effect the quality of the resulting data. As such it is important to consult with
an analytical chemist prior to modifying any of the methods contained in this
Catalog.
1.2 INTENDED USERS
The FSMC system has been developed for individuals who are responsible for devel-
oping or overseeing sampling activities at Superfund hazardous waste sites. As
already mentioned, these individuals require information regarding analytical/
screening techniques which have demonstrated field utility and which complement
those methods used by the CLP.
The FSMC addresses the need of site personnel to determine what field methods, if
any, are most appropriate in a given situation. Based on preliminary site information
such as types of contaminants, the user can identify field analytical/screening meth-
ods that have been developed and applied at other similar sites and therefore may
be of use for site characterization and other screening/analytical requirements.
1.3 SYSTEM UPDATES
Documentation and system revisions will be made to the pocket-guide, user docu-
mentation, and computer retrieval system. The documentation updates will focus on
the user documentation and the method descriptions to ensure accuracy and com-
pleteness of available methods, and additions of new methods on a periodic basis.
1.4 TECHNICAL CONSIDERATIONS
The appropriate type of sampling and analysis at a given site depends on numerous
factors, the foremost of which are the intended end use of the data and associated
data quality requirements, Data quality, as stated in the Data Quality Objectives for
Remedial Response Activities (EPA, 1987 - OSWER Directive 9355.0-7A), is defined
by the level of analytical support appropriate to various data uses. As such, five
levels of analytical support (Levels I-V) are defined below and are appropriate to a
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number of overlapping data uses as shown on Tables 2-1 and 2-2.
LEVEL I - Field Screening or analyses using portable instruments.
Results are often not compound specific and not quantitative but results
are available in real-time. It is typically the least costly of the analytical
options.
LEVEL II - Field analyses using more sophisticated field portable analyti-
cal instruments. In some cases, the instruments can be set up in a
mobile laboratory on site. There is a wide range in the quality of data
that can be generated from qualitative to quantitative.
LEVEL III- Laboratory analysis using methods other than the CLP-RAS.
This level is used primarily in support of engineering studies using stan-
dard EPA approved procedures. Some procedures may be equivalent to
CLP-RAS, but without the CLP requirements for documentation.
LEVEL IV - CLP Routine Analytical Services (RAS). This level is
characterized by rigorous QA/QC protocols and documentation and pro-
vides qualitative and quantitative analytical data. (Some Regions have
obtained similar support via their own regional laboratories, university
laboratories, or other commercial laboratories).
LEVEL V - Non-standard methods. Analyses which may require method
modification and/or development. CLP Special Analytical Services (SAS)
are considered Level V.
Whereas the "quality" of data generally increases from Level I through Level V as
shown above, this can only be stated in a general way and in certain instances and
with the appropriate QA/QC procedures, the "quality" of Level II and III data can
parallel that achieved by Level IV and V data. Consider for example a Level II
analysis for volatile organics using a GC in a field laboratory; in this situation, the
"quality" of the data may be higher than that achieved in an offsite laboratory (Level
III, IV, orV) due to sample handling considerations. Similarly, Level II and III analyses
can at times provide lower detection limits than those required by Level IV require-
ments, and as such, the "quality" of data is higher based on the data quality
objectives.
It is important to note that in most situations the exact "quality" of an analysis
cannot be specified or determined prior to the analysis and as such sufficient QA/QC
steps have to be taken (e.g., documentation of blank injections, calibration standard
runs, runs of qualitative standards between samples, and analysis of duplicates and
spikes) to be able to assess the quality achieved. As such, one of the major benefits
of Level IV analysis is that it provides sufficient documentation to allow (qualified)
personnel to review and evaluate data quality. In other words, while the "quality" of
Level IV data may not be higher (as defined by the precision and accuracy) than
those achieved by other levels of analysis, it does provide data of "known quality"
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TABLE 2-1
SUMMARY OF ANALYTICAL LEVELS APPROPRIATE TO
DATA USES
DATA USES
ANALYTICAL LEVEL
TYPE OF ANALYSIS
LIMITATIONS
DATA QUALITY
SITE CHARACTERIZATION
MONffGHNG DURING
IMPLEMENTATION
SITE CHARATERIZATION
EVALUATION OF ALTERNATIVES
ENGINEERING DESIGN
MONITORING DURING
IMPLEMENTATION
RISK ASSESSMENT
PRP DETERMINATION
SITE CHARACTERIZATION
EVALUATION OF ALTERNATIVES
ENGINEERING DESIGN
MONITORING DURING
IMPLEMENTATION
RISK ASSESSMENT
PRPDETERMINATION
EVALUATION OF ALTERNATIVES
ENGINEERING DESIGN
RISK ASSESSMENT
PAP DETERMINATION
TOTAL ORGANIC/INORGANIC
VAPOR DETECTION USING
PORTABLE INSTRUMENTS
- VARIETY OF ORGAN ICS BY
GC; INORGANICS BY AA;
XRF
LEVEUI - TENTATIVE ID; ANALYTE-
SPECIFIC
-DETECTION LIMITS VARY
FROM LOW ppm TO LOW ppb
. ORGANICS/ORGANICS
USING EPA PROCEDURES
OTHER THAN CLP CAN BE
LEVEL III ANALYTE-SPECIFIC
- RCRA CHARACTERISTIC TESTS
HSL ORGANCICS/INORGANICS
BY GC/MS.;AA; ICP
LEVEL IV
. LOW ppb DETECTION LIMIT
.NONCONVENTIAL
PARAMETERS
LEVELV - METHOD-SPECIFC
DETECTION LIMITS
-MODIFICATION OF
EXISTING METHODS
-APPENDIX B PARAMETERS
- INSTRUMENTS RESPOND TO
NATURALLY-OCCURING
COMPOUNDS
. TENTATIVE ID
. TECHNIQUES/INSTRUMENTS
LIMITED MOSTLY TO
VOLATILES. METALS
- TENTATIVE ID IN SOME
CASES
- CAN PROVIDE DATA OF
SAME QUALITY AS
LEVELS IV. NS
- ENTATIVE IDENTIFCATION
OF NON-HSL PARAMETERS
- SOME TIME MAY BE REQUIRED
FOR VALDATION OF PACKAGES
MAY REQUIRE METHOD
DEVELOPMENT/MODIFCATION
MECHANISM TO OBTAIN
SERVICES REQUIRES
SPECIAL LEAD TIME
- IF INSTRUMENTS CALIBRATED
AND DATA INTERPRETED
CORRECTLY, CAN PROVE
INDICATION OF CONTAMINATION
- DEPENDENT ON QA/QC
STEPS EMPLOYED
DATA TYPICALLY REPORTED
IN CONCENTRATION RANGES
SIMILAR DETECTION
LIMITS TO CLP
LESS RIGOROUS QA/QC
GOAL IS DATA OF KNOWN
QUALITY
RIGEROUS QA/QC
METHOD-SPECIFIC
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TABLE 2.2
APPROPRIATE ANALYTICAL LEVELS - BY DATA USE
^"^V^ DATA USE
LEva ^v^
LEVEL 1
LEVEL II
LEVEL III
LEVEL IV
LEVEL V
OTHER
SITE
CHARACTERIZATION
(NCLUDNG
HEALTH*
SAFETY)
^/
^/
N/
RISK
ASSESSMENT
N/
N/
N/
EVALUATION OF
ALTERNATIVES
N/
N/
N/
BJGMEERNG
DESIGN OF
REMEDIAL ACTION
N/
N/
N/
MONITORNG
DURNG
IMPLEMENTATION
OF
REMEDIAL ACTION
N/
N/
N/
PRP
N/
N/
N/
OTHER
NOTE: CHECK APPROPRIATE BOX (ES)
COM SFDOO 1001
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The decision to use field analytical/screening techniques (i.e., Levels I and ii) must
be made on a site specific, and on a sampling-event-by-sampling event basis.
Factors to be considered include data quality requirements, parameters for which
the analytical method is valid, contaminants of concern, required detection limits,
and the range of precision, accuracy, representativeness, completeness, and com-
parability (PARCC) required and provided by each analytical option. Documentation
and chain-of-custody considerations are also relevant and should be considered.
While representativeness, completeness and comparability are, for ail practical pur-
poses, sampling considerations, precision and accuracy encompass both sampling
and analytical considerations and define the quality of the resulting data. Precision
measures the reproducibility of measurements under a given set of conditions.
Specifically, it is a quantitative measure of the variability of a group of measurements
compared to their average value. Precision is usually stated in terms of standard
deviation but other estimates such as coefficient of variation (relative standard de-
viation), range (maximum value minus minimum value), and relative range are also
common. Since precision defines the scatter of results about a mean value, a lower
standard deviation means less scatter.
The overall precision of measurement data is a mixture of sampling and analytical
factors. Analysis of field and laboratory replicates provides a measure of overall
precision.
Accuracy measures the bias in a measurement system. Sources of error are the
sampling process, field contamination, preservation, handling, sample matrix,
sample preparation and analysis techniques. Sampling accuracy can be assessed by
measuring the concentration of contaminants in field/trip blanks, while analytical
accuracy may be assessed through use of known and unknown QC samples and
matrix spikes.
Accuracy is most frequently reported as percent recovery, or percent bias. A 100%
recovery indicates a completely accurate measurement; the greater the deviation
(i.e., under or over) is from IOO%, the less accurate the measurement. Percent bias
reports the difference of the result from the true value. A completely accurate
measurement would have zero percent bias; the lower the percent bias, the more
accurate the measurement.
While historical accuracy and precision information which is classified by media are
available for CLP analytical methods (Level IV), significantly less information exists
for the other levels of analysis (including Level V). Historic accuracy and precision
information has been compiled and classified by media and by analytical level (EPA,
1987 - OSWER Directive 9355.0-7A). This information is excerpted and presented in
Appendix B.
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The available data base for documenting accuracy and precision (as well as mini
mum detection limits) for Levels I and II is sparse. To supplement the sparse and
scattered information which exist in published and unpublished reports etc., person-
nel who use the methods presented in the FSMC are encouraged to catalog the
precision and accuracy that is obtained during his/her specific use, and to provide
this Information to the FSMC Systems Coordinator.
Based on the required data quality objectives and data uses, the choice to use field
screening/analytical methods should be made in conjunction with a "confirmation"
program to include a rigorous QA/QC program (analysis of QC samples), instrument
calibration, and Level III or IV confirmation. The user is urged to consult both the
Data Quality Objectives for Remedial Response Activities and the Compendium of
Superfund Field Operations Methods Manuals (EPA, 1987 - OSWER Directive 9355.0-
7A and EPA, 1987a - OSWER Directive 9355.0-14) as part of the decision process
used to define the appropriate levels of analytical support. It is further recommended
that, based on the Intended data uses and associated data quality requirements, the
data obtained through field analysis/screening be confirmed by CLP analysis.
1.5 OVERVIEW OF LEVELS I AND II ANALYSES
Level I and II analyses are defined as field screening/analytical methods which utilize
equipment amenable to the rigors of field conditions, and are located at or near the
sampling site.
Level I analytical support Is typically defined as field screening, with the objective of
generating data which will generally be used (for example during Phase 1 Investiga-
tions), In refining sampling plans and determining the extent of contamination. A
second objective of Level I analyses is to conserve other analytical support
resources.
Level I analyses are generally effective for total vapor readings using portable pho-
toionization or flame lonization detectors (PID or FID) which respond to a variety of
organic and Inorganic volatile compounds. Detection is typically limited to volatile
compounds. These types of analyses provide data for on site, real time total vapor
measurements, evaluation of existing conditions, sample location optimization,
extent of contamination, and health and safety evaluations. Data generated from
Level I analyses are considered qualitative in nature although semi-quantitative and/
or quantitative data can be generated, for example, by using the GC option of a FID,
with sufficient calibration. Data generated from Level I analyses provide the
10
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following:
Identification of soil, water, air and waste locations which have a high
likelihood of showing contamination through subsequent analysis;
Real-time data to be used for health and safety considerations during
site investigations;
Qualitative data relative to a primary calibration standard if the contami-
nants being measured are unknown:
Quantitative data if a contaminant is known and the instrument is cali-
brated to that substance: and
Presence or absence of contamination.
Level II analytical support is designed to provide real-time data for ongoing field
activities or when initial data will provide the basis for seeking laboratory analytical
support. As such, Level II analytical methods can be effectively utilized when a
phased approach Is used for field sampling. There have also been a significant
number of instances where data derived from Level II support have been used to
make decisions about site disposition.
Field analysis using Level II analytical options can provide data from the analysis of
air, water, soil, and waste materials for many Target Compound List (TCL) organic
compounds including volatiles, base neutral acid (BNA), extractabie organlcs, and
pesticides/PCBs. Inorganic analysis can also be conducted using field atomic ad-
sorption (AA) and other instruments.
Level II analyses are used for on site, real-time baseline data development, extent of
contamination and remedial activities and generally provide rapidly available data for
a variety of activities including hydrological investigations (establish depth/
concentration profiles); extent of contaminant determination including special activi-
ties such as vadose zone sampling; cleanup operations (determine extent of con-
taminated soil excavation), and health and safety considerations.
Typically, a gas chromatograph and more sophisticated instruments operated in the
field provide the bulk of the analytical support at this level. The ability to assess the
data quality (accuracy and precision) is dependent upon the QA/QC steps taken in
the process, including documentation of blank injections, calibration standard runs
and runs of standards between samples.
The level of precision and accuracy that can be achieved by a specific Level I or II
analysis varies as a function of numerous factors including the matrix and contami-
nant being sampled, and perhaps most importantly, the skill of the analyst doing the
work. As summarized in the Data Quality Objectives for Remedial Response Activities
(EPA, 1987 - OSWER Directive 9355.0-7A) "because the procedures (for Level II) are
11
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not formalized, a great deal of improvisation usually takes place. The inherent
variability of the procedures themselves would make the development of a
centralized quality assurance data base tenuous. The same reasoning would apply
to making uncertainty predictions based on a centralized data base". On the other
hand, Level II analyses based in a mobile laboratory setting and using state of the art
sophisticated instrumentation, can allow mobile laboratory capabilities to approach
the analytical range and performance (accuracy, sensitivity and precision) achieved
in off-site analytical facilities.
Based on the undocumented data quality of most Level I and II analyses, data
generated in the field are typically confirmed by submitting duplicate samples to the
CLP. Although no statistical methods are available to determine the exact number of
samples to submit for confirmation, numerous factors have to be considered includ-
ing:
^Objective of sampling (i.e., data quality objectives);
^Data uses, and
^Method of analysis used and the level of accuracy and precision achieved.
In general, confirmation samples should include a subset (or all) of designated
critical samples, a subset of samples covering the entire range of identified con-
centrations, and a subset of samples near the action level and near the "0" con-
centration or not detectable range.
An additional factor to consider is the measured precision of the field instrument in
use. When high precision is measured, less samples need to be confirmed; if how-
ever, a low precision Is calculated, It is recommended that based on the data quality
objectives defined for the site, the analysts be suspended until a qualified chemist
determines the reason for the low precision.
The equipment utilized for Level I and II analyses can vary greatly in terms of
physical configuration, size, weight, power requirements, and the level of accuracy
and precision achievable. Based on the mobility of the equipment, three terms are
typically used to describe the mobility of the equipment:
Portable: Requires no external power requirements; hand held devices which
can be easily carried by one person. Typically includes photoionization detec-
tion (PID) and flame ionization detection (FID) to measure the total amount of
ionizable materials, mostly volatile organic compounds. Also includes suitcase-
sized gas chromatographs (GC) with assorted detectors and capabilities, and
X-Ray fluorescence devices.
12
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Fieldable: Particularly rugged; limited external power required. Easily
transported in a van, pick-up, or four wheel drive.
Mobile: Small enough to carry in a mobile lab; Includes most analytical instru-
ments. Power considerations may limit the use of many instruments in mobile
laboratories.
As outlined in this brief discussion of Level I and II analytical methods, numerous
factors must be considered when determining which method should be implemented
at a site. Data quality objective for the sampling event in question and the ultimate
end use of the data developed should also be considered.
13
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2.0 INSTALLING THE SYSTEM
The first time the FSMC system is run, an installation menu will appear and request
information about your computer. This system will run on a computer with two floppy
disk drives or one floppy disk drive and at least one hard drive. The floppy disk drive
on the hard disk system is used to copy all programs and data files to the hard drive
(usually C:), it is not used to run the system once all programs and data files have
been copied to the hard drive.
It is assumed that the computer used has already been turned on and loaded with
MS-DOS version 2.0 or higher. Consult your computer's operating manual for these
procedures.
Some users will have to change the CONFIG.SYS file to properly run the compiled
dBASE III code. The CONFIG.SYS file should have the following two lines:
BUFFERS = 25
FILES = 20
To list the file, enter
C> TYPE \CONFIG.SYS
If the two values are equal to or larger than listed above, then no changes are
needed. If the values are less than those listed above, or if the lines are missing, the
file will have to be edited. Please consult your MS-DOS manual for instructions on
editing this file.
2.1 INSTALLATION ON A TWO DISK DRIVE COMPUTER SYSTEM
Users with a dual-floppy disk drive system may use FSMC. The following procedures
should be followed the first time the system is used so that the FSMC will recognize
which disk drives will be used.
The user should make a copy of the two system diskettes and return the originals to
the manual for any future installations.
1. Insert FSMC disk A into drive A and
disk B into drive B.
2. If the A: drive is not the current drive, enter
B: >A: (RETURN/ENTER]
14
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3. To start the FSMC system, enter
A: > FSMC [RETURN/ENTER]
4. When asked "Do you have a hard drive [Y/N] ?," enter
N [RETURN/ENTER]
The installation procedure will take about one minute. After the installation is com-
pleted, the main menu will appear.
2.2 INSTALLATION ON A HARD DRIVE COMPUTER SYSTEM
Throughout this manual It Is assumed that the hard disk is named "C:" and the
directory on which FSMC resides is "C:\FSMC". Other combinations are valid and
should be designated during the Installation process.
1. Create a directory on your hard disk
C: >MKDIR \FSMC [RETURN/ENTER]
2. Switch to the FSMC directory
C: >CHDIR \FSMC [RETURN/ENTER]
3. Insert the FSMC program diskette into drive A
Switch to A: drive
C: >A: [RETURN/ENTER]
4. Start the system
A: > FSMC [RETURN/ENTER]
5. When asked "Do you have a hard drive [Y/N] ?", enter
Y [RETURN/ENTER]
6. Enter a valid hard disk name
c: [RETURN/ENTER]
The installation will then proceed. After the installation is completed, the main menu
will appear. The C: drive will now be your current drive. Return the program diskettes
to the manual for future installations.
15
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2.3 INSTALLING FSMC MORE THAN ONCE
The FSMC system has no limit to the number of times it may be installed, however
the installation procedures will appear automatically only the first time. To install the
system more than once, select option "5-Utillities" from the main menu and select
"install the FSMC system". You will then be able to Install the system as described
above.
Note: Installation from option "S-Utilities" will only work from the floppy disks. It
will not work from a hard disk because the FSMC copy of the program has
already been installed to the hard disk drive.
16
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3.0 GETTING STARTED
If the FSMC system has not yet been installed, proceed as described in the section
entitled "Installing the System. "
For a two floppy system, insert disk A into drive A and disk B into drive B and enter
A: > FSMC
For a hard drive system, change the current directory so that the FSMC is ac-
cessible, then enter
FSMC
From this point on, all instructions are the same for both computer configurations.
17
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3.1 SEARCHING THE DATA BASE
The data base may be searched in several ways. The user may enter a substance
name or CAS number if a method for a specific chemical is desired, by chemical
group (e.g. volatile organics), or by method name. The user's options are displayed
and described in Figure 3-1. More detailed descriptions are included below.
The FSMC system provides several search options depending upon the information
known about the substances and area to be sampled. The sequence of the search
routines are summarized a$ follows:
1. Select an option in order to enter the chemical name, group, CAS
number, or method name or number.
2. Select each matrix that must be analyzed with this field method by enter-
ing a "Y" after each matrix name.
3. Enter the detection limit to constrain the search to only those
methods capable of analyzing below or equal to this limit for each matrix
selected. Enter "0.0" if no limit is desired.
4 The default units of measure may be changed. Valid units of measure for
the detection limit are PPM (parts per million) and PPB (parts per billion).
5 The system will respond by informing the user how many methods were
found in this search. If there was at least one, a display/print menu will
display the options of viewing the method descriptions.
FIELD SCREENING METHODS CATALOG (FSHC)
USER RETRIEVAL SYSTEM
SEARCH OPTIONS
[1] CLASS OF CHEMICALS
12] COnPOUND/CHENICAL NANE
[31 CAS NUMBER
[41 METHOD NAME OR NUMBER
[81 EXIT
[51 UTILITIES (INSTALL,REINDEX)
SELECT OPTION (8-5): 2
Tuesday October 27, 1987 7:19:89
Figure 3-1
18
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3.1.1 SEARCHING BY CHEMICAL NAME
The user may enter a specific chemical name. If the full name is not available, enter
what you know is correct. The search is designed to look for an embedded character
string within a chemical or method name. The system will match on what the user
has entered if that character string is found anywhere in the name, display what was
found, and then permit the user to select the one desired. See Figure 3-2.
SEARCH FOR A CHEMICAL NAME
ENTER CHEMICAL NAME
BLANKS TO EXIT - NOTE THE RECORD Is FOR NAME CONFIRMATION
RECORD* CAS# CHEMICAL NAME
164 71-43-2 BENZOL
264 85-68-7 BENZYL BUTYL PHTHALATE
265 85-68-7 BENZYL N-BUTYL PHTHALATE
284 91-94-1 BENZIDINE, 3,3'-DICHLORO-
285 91-94-1 3,3'-DICHLOROBENZIDINE
286 92-87-5 BENZIDINE
291 95-50-1 0-DICHLOROBENZIDINE
292 95-50-1 1,2-DICHLOROBENZME
299 98-95-3 NITROBENZENE
300 98-95-3 NITRBBENZOL
ENTER RECORD # TO SELECT CORRECT NAME:
(Enter 0 to return to the MAIN MENU)
Figure 3-2
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3.1.2 SEARCHING BY CHEMICAL ABSTRACT SERVICES (CAS)NUMBER
The user must enter a Chemical Abstract Services (CAS) Number, including the
dashes, and not including preceding zeros. The system will respond by displaying all
chemical synonyms with that CAS number so that the user can verify the entry. One
chemical name is then selected to continue the search. See Figure 3-3.
Valid CAS Numbers Invalid CAS Numbers
7440-43-9 7429905
7143-2 0057-74-9
SEARCH FOR CAS NO.:188-41-4
ETHYLBENZENE
ENTER SEARCH PARAHATERS
(Enter [Yl for each Matrix desired)
AIR(Y/N) 3 SOIL(Y/N) Q UATER(Y/N)
DETECTION LIMIT KE PP2
(8 for no limit)
Is this correct tY/Nl? Q
[11 DISPLAY or [21 PRINT HEADING ONLY
[31 DISPLAY or [41 PRINT HEADING ft SUHNARY
[51 DISPLAY or (61 PRINT COMPLETE HETHOD(S)
Methods found SELECT DISPLAY/PRINT (1-6, fl TO EXIT) Q
Figure 3-3
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3.1.3 SEARCHING BY CHEMICAL CLASS
The user may request a search by one of five chemical class. These classes are
shown in Figure 34.
FIELD SCREENING METHODS CATALOG (FSHC)
SEARCH BY CLASS OF CHEMICALS
[1] - Aromatics [4] - Base kid
- Chlorinated Hydrocarbons -BNA
- Gasoline - Coal Tar Volatiles
- Hydrocarbons - Polynuclear Aromatics(PNAs)
- Volatile Organics - Polcyclic Aromatics
- Unsaturated Hydrocarbons Hydrocarbons (PAHs)
- Semi-volatiles
[2] - Aroclors [5] - Heavy metals
- PCB - Inorganics
- Metals
[3] - Insecticides
- Pesticides
SELECT CHEMICAL CLASS (1-5, 0 to exit) 0
Figure 3-4
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3.1.4 SEARCHING BY METHOD NAME OR NUMBER
The user may enter a specific method name. If the full name is not known, enter a
character string that you know is correct. The search is designed to look for an
embedded character string within a method name. The system will match on what
the user has entered, display what was found, and then permit the user to select the
one desired.
If the method number is known, the user can reduce typing and search time by
entering the number instead of the name. See Figure 3-5.
SEARCH FOR A FULL OR PARTIAL METHOD NAME
ENTER METHOD HAtlE OR NUMBER (BLANKS TO EXIT)
Enter ALL to select ALL Methods
ENTER SEARCH PARAMETERS
(Enter EV1 for each Matrix desired)
AIR(¥/H) Q SOILCV/H) J
DETECTION LIMIT •Rlil PPJ
(8 for no Unit)
Is this correct [Y/N1? Q
[1] DISPLAY or [21 PRINT HEADING ONLY
131 DISPLAY or [41 PRINT HEADING * SUMMARY
15] DISPLAY or [61 PRINT COMPLETE NETHOD(S)
5 Methods found SELECT DISPLAY/PRINT (1-6, 8 TO EXIT) |
Figure 3-5
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3.1.5 SEARCHING BY THE SAMPLE MATRIX
The user may select specific matrices (air, soil and water) in order to constrain the
search. The user must enter a "Y" for each matrix desired. The middle portion of
Figure 3-5 displays the matrix options.
3.1.6 SEARCHING BY DETECTION LIMIT VALUES AND UNITS
if the user requires a certain detection limit or "sensitivity" level on which to search
a method, the user may enter a value and units for each matrix selected. Only the
methods that are valid at that detection limit or less will be selected. If a "0.0" Is
entered for any matrix, ail methods for that matrix will be selected, regardless of the
detection limit. The default units of measure may be changed by the user. Valid units
of measure for the detection limit are PPM (parts per million) and PPB (parts per
billion).
The middle portion of Figure 3-5 displays the detection limit option. The example
shows a detection limit minimum for air (10.0 PPM) and for water (50.0 PPB).
23
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4.0 DISPLAYING OR PRINTING REPORTS
If a search has been successful and one or more methods have been selected, a
DISPLAY/PRINT menu presents the option to display the method(s) on the screen or
to print them on an attached printer. This menu is shown in the bottom portion of
Figure 3-5 and summarized in the following table.
Option Number Result
f Display Method Headings Only
2 Display Method Heading and Summary
3 Display Complete Method Listing
4 Print Method Headings Only
5 Print Method Heading and Summary
6 Print Complete Method Listing
After selecting one or more methods to print or display, the user may elect to print
the detection limit table for each method. These tables will Include all the sub-
stances for which each method may be applied. When the printing is complete, the
DISPLAY/PRINT menu reappears. At this point you can choose to repeat the
DISPLAY/PRINT process or exit to the main menu and conduct another search.
When a user selects options 3, or 6, methods selected for display or printing will
produce fully detailed method descriptions. In order to view or print Headings only or
Headings and Summaries, choose option 1 or 4 and 2 or 5 respectively.
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5.0 FSMC SYSTEM REQUIREMENTS
5.1 SOFTWARE CHARACTERISTICS
The two sided 5 I/4 inch diskettes are the only software required to run the FSMC
system. Users are encouraged to make backup copies of these two diskettes.
Although users may freely copy the system diskettes, only users of registered copies
will receive software and documentation revisions. To obtain additional copies of the
FSMC system, contact the FSMC Coordinator at the address provided in the
Executive Summary and Appendix C of this manual.
The FSMC system was developed by COM Federal Programs Corporation using
dBASE iii Pius version 1.1, a product of Ashton-Tate Inc. The source code was
compiled using Clipper, a product of Nantucket Software, Inc. and will run on most
IBM compatible computers under MS-DOS. The FSMC system does not require a
copy of dBASE iii Pius to run, and will execute faster than if it were uncompiled
running under dBASE III.
5.2 HARDWARE REQUIREMENTS
The following are the minimal computer hardware requirements needed to run the
FSMC system. The system has been tested on Compaq DeskPro-386, Compaq
Portable-2, Telex PC, IBM PC clones, and Tandon machines.
* IBM compatible computer with 512K of available RAM, a monochrome or
color monitor.
Two floppy disk drives or one floppy disk drive and one hard disk drive.
A printer if printed reports are desired.
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APPENDIX A
FIELD METHOD LISTING
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LISTING OF METHODS
PRIMARY METHODS
FM-I Field Atomic Absorption Analysis 1
FM-2 X-Ray Fluorescence in Laboratory for Heavy Metals 4
FM-3 X-Ray Fluorescence for Heavy Metals (On-site) 6
FM-4 Air Monitoring for Volatile Organic Compounds Using
Programmed Thermal Desorption and GC 8
FM-5 Volatile Organic Compound Analysis Using GC with
Automated Headspace Sampler 10
FM-6 Headspace Technique Using an Ion Detector for VOC Analysis. 12
FM-7 Headspace Technique Using an OVA for VOCs 14
FM-8 Headspace Analysis Using HNU for Total Volatile Organics ... 16
FM-9 Headspace Technique Using a Mobile GC for VOCs 18
FM-10 Passive Soil Gas Sampling Using Industrial Hygiene Samplers 20
FM-11 Soil Gas Sampling Using Mini-Barrel Sampler 22
FM-12 Soil Gas Sampling Using a One-Liter Syringe 24
FM-13 Soil Gas Sampling Using Direct Injection - Stopper 26
FM-14 Soil Gas Sampling Using a Perforated Tube 28
FM-15 Soil Gas Sampling Using Tenax Tubes 30
FM-16 Soil Gas Sampling for Downhole Profiling. 32
FM-17 Soil Gas Sampling Direct Injection - Auger 34
FM-18 PC6 Analysis Using a Gas Chromatograph in an On-Site
Laboratory - Hexane/Methanol/Water Extraction 36
FM-19 PCB Analysis Using a Gas Chromatograph in an On-Site
Laboratory - Hexane Extraction. 38
FM-20 PCB Analysis Using a Gas Chromatograph in an On-Site
Laboratory - Hexane/Methanol 40
FM-21 PCB Analysis Using a Gas Chromatograph in an On-Site
Laboratory - Hexane/Acetone Extraction 42
FM-22 Pesticide Analysis Using a GC with ECD - Hexane/Methanol
Extraction 44
FM-23 Pesticide Analysis Using Isothermal GC with ECD - Hexane
Extraction 46
FM-24 Phenol Determination by Liquid-Liquid Extraction and GC Analysis ... 48
FM-25 PAH Analysis Using GC with Heated Column 50
FM-26 Total PNA Analysis Using an Ultraviolet Fluorescence
Spectrophotometer. 52
METHODS UNDER DEVELOPMENT
FM-D1 Trace Atmospheric Gas Analyzer (TAGA) 54
FM-D2 Use of Bonded Sorbents for Pesticide Analysis 58
FM-D3 Use of Bonded Sorbents for Semi-Volatile Analysis 60
FM-D4 Immunoassays for Trace Organic Analysis 62
FM-D5 Use of Fiber Optic Sensors in Environmental Monitoring 64
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Method FM-I: FIELD ATOMIC ABSORPTION ANALYSIS
Summary: Atomic absorption (AA) spectroscopy for metals analysis in field laboratory
with the minimum detectable concentrations commonly below 1 ug/kg for metals
such as Au, Ag, Cu, Cd, and Pb. Tungsten furnace requires a maximum of only 500
W of power and can be run off a portable generator.
Method description: Low mass tungsten furnace is used to atomize samples, making
power requirements compatible with field lab use. Dry-ash-atomize timing and tem-
perature controls must be set for element being analyzed; final ashing temperature is
adjustable between 1000°C and 1000°C; atomizing temperature is variable to
2500%. Sample is prepared by procedures similar to those used in other AA tech-
niques. Place 10 ul liquid sample by pipette onto atomizer. Analysis results are
displayed in about 90 seconds.
Applications: Mobile field analysis for trace metals.
Limitations: Requires 1 10/220 volt electrical connection. Sample preparation required.
Instrumentation used: Scintrix AAZ-2 Zeeman Modulated Atomic Absorption
Spectrophotometer.
PERFORMANCESPECIFICATION
Sensitivity (Detection Limits): 0.1 mg/kg for most metals. Detection limits are obtained
by taking 3 times the standard deviation from 14 determinations on a standard.
Selectivity: Zeeman technique used to reduce background interference.
Accuracy: Not generally available. Whenever possible, comparative results are presented
in the user's Application Manual.
Precision/Repeatability: In general better than 10%. Measurements are based on 14
determinations of a metal standard which lies in the middle of the linear working
range. For example, the RSD for 8 ng/ml copper was 3%, for 1.0 ng/ml of cadmium
was 8!! and for 20 ng/ml lead was 7!!.
Comments: Portable generator can be used for power. Argon gas is used for cooling
the furnace (eliminating need for water) and as a purge gas. Argon-hydrogen and
helium are also used as purge gases based on specific applications. For each ele-
ment being analyzed, a specific cathode lamp is required.
USE
Location Used: Field experience mainly related to mining, beginning to be used in haz-
ardous waste work.
EPA Site Number (CERCLIS): Not Applicable.
Matrix: Water and Soil.
Preparation, Maintenance and Cleanup: Monochromator adjustment required to analyze
for each element. Filament replacement in the furnace required after "hundreds" of
firings. Argon gas used for flushing; 75 kg tank replacement in about 200 hours.
Analysis Time: 2 minutes/sample after sample preparation.
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Capital Cost: $20,000 - $30,000.
Calibration: Three (3) standard solutions covering the entire working concentration range
of the element being analyzed are used and prepared fresh daily. The standard solu-
tions and a blank is run at the start of each day, and one standard is used to verify
calibration three times a day.
Comments: Easily set up for field work in mobile or stationary field laboratory. Zeeman
correction compensates somewhat for design compromise in optics and furnace re-
quired for portability. Hazardous waste site experience is limited.
Protocol
Available:
Yes
SOURCE
Technical Contact: Dr. John D. Kinrade
Affiliation: Scintrex Limited
Telephone: (416) 669-2280
Prepared: 09/29/87
BIBLIOGRAPHY
Becker, D.L., and Carter, M.H., "Equipment Available for Sample Screening and On-Site
Measurements, Appendices", TDD-HO831 1-04, U.S. EPA, May 30, 1984 (Draft)
Kinrade J.D. et. al., "Applications Manual for the Scintrex AAZ-2 Zeeman Modulated
Absorption Spectrophotometer" Scintrex Limited, Concord, Ontario, Canada October
1986
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METHOD FM-2: X-RAY FLUORESCENCE (XRF) IN LABORATORY FOR HEAVY METALS
SUMMARY: Rapid screening of most metals (46) in soil and water in field laboratory to
minimum of 20 mg/kg in soil. Conventional methods have better sensitivity and preci-
sion. Simultaneous detection (of the 18 elements analyzed for) is one of the greatest
advantages of the system.
METHOD DESCRIPTION: Uses a flux of high energy x-rays to bombard sample causing
elements in sample to emit characteristic wavelengths, The instrument separates the
elements' wavelengths into a spectrum. Concentration of elements present is directly
proportional to energies being produced. Technique used to screen soil and water
samples. Soil sample preparation includes drying sample and grinding to a fine
powder, Aqueous sample preparation includes concentrating the metallic
cations by filtering through strong acid ion exchange paper. Sample pH must be below 2
to ensure that metal Ions are in cationic form. When anionic forms such as arsenate,
etc. are present, base ion exchange is required. Region VIM method uses portable
XRF analyzer which offers less sensitivity and detects fewer metals than this method.
APPLICATION: Rapid screening in laboratory for chromium, barium, cobalt, silver, ar-
senic, antimony, selenium, thallium, mercury, tin, cadium, lead, copper, nickel, zinc,
manganese, iron, and vanadium.
LIMITATIONS: Does not have sensitivity or precision of atomic absorption or other con-
ventional methods. Lithium, beryllium, aluminum, and boron not detected using this
method.
INSTRUMENTATION USED: Kevex 7000 X-Ray Fluorescence Spectrometer.
PERFORMANCE SPECIFICATION
DETECTION LIMIT: Is element specific. For critical elements such as lead, it is 20 mg/kg
in soil and 600 ug/l in water. For 18 elements tested, the range was from 20 to 50
mg/kg in soil and 100 to 600 ug/l in water.
SELECTIVITY: Elements may be identified by looking at various emission x-rays (i.e., K-
alpha, K-beta, etc.). Spectra are stored on computer disc for later printout and direct
identification of each element.
ACCURACY: Four samples analyzed for lead by CLP had values of 80, 180, 130 and
910 mg/kg. The range of values for the same samples analyzed by XRF were IOO-
300, 100-200, 95-120 and 800-900 mg/kg, respectively.
PRECISION/REPEATABILITY: Duplicate samples show good repeatability.
COMMENTS: XRF is non-destructive; samples can be stored for future reference after
analysis.
USE
LOCATION USED: Sudbery, MA; 1985 (Non-CERCLA).
EPA SITE NUMBER (CERCLIS): Non-CERCLA
MATRIX: Soil and Water.
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PREPARATION, MAINTENANCE AND CLEANUP: Soil samples (dried, 60 mesh-screened)
are placed directly into sample cup; aqueous samples are ion exchanged by passing
through a resin-coated filter paper. XRF spectrometer must be set up and pro-
grammed. Maintenance of the spectrometer includes checking probe for cleanliness
and dryness and checking source decay. Standards are prepared using 1,000 mg/kg
AA standard solutions for Ag, Ba, Mn, Ni, Sn, Zn, Se and Pb. Standards can be
prepared separately or as multi-element mixtures and can be used up to 5 months.
ANALYSIS TIME: 10-30 minutes for sample preparation. Analysis time is less than 10
minutes.
CAPITAL COSTS: $80,000.00
CALIBRATION: Standards required at concentrations of 1000, 500, 250, and 125 mg/kg
for soil and 2, 1, 0.5 and 0.25 ug/l plus a blank for water samples. Run all standards
at beginning of each day and run a set every fourth hour of analysis or after all
samples have been analyzed, whichever is more frequent. Additional standards must
be prepared and used to cover the entire working range of required analyses.
COMMENTS: Spectrum displayed on video screen and stored in computer disk. Used
routinely in Region I. Sample quantity needed for analysis is 1g of soil or 40 ml for
water.
PROTOCOL AVAILABLE: Yes.
SOURCE
TECHNICAL CONTACT: Dr. Thomas Spittler
AFFILIATION: U.S. EPA Region I Laboratory
TELEPHONE: (617)861-6700
PREPARED: April 7, 1987
BIBLIOGRAPHY
Furst, G.A., Spittler, T. and Tillinghust, V., "Screening For Metals at Hazardous Waste
Sites: A Rapid Cost-Effective Technique Using X-Ray Fluorescence," Management of
Uncontrolled Hazardous Waste Sites, Washington, D.C. November 4-6, 1985.
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METHOD FM-3: X-RAY FLUORESCENCE (XRF) FOR HEAVY METALS (ON-SITE)
SUMMARY: Good for on-site screening of some metals in soil to minimum of 15 mg/kg.
Sample matrix may cause accuracy problems. Uses portable XRF analyzer.
METHOD DESCRIPTION: Uses flux of high energy X-rays to bombard sample, causing
elements in sample to emit energy at characteristic wavelengths. Instrument separates
wavelengths produced into a spectrum that contains energy peaks characteristic of ele-
ments present. Concentration of each element present Is directly proportional to the in-
tensity of energy produced for that element. This technique has been used to screen soil
and sediment samples for concentrations of lead, zinc, copper, arsenic, iron, and chro-
mium. Sample preparation includes drying a 5-gram sample and grinding it to a fine
powder. The XRF analyzer must be programmed and calibrated before samples are
screened.
APPLICATION: Rapid on-site screening for lead, zinc, copper, arsenic, iron, and
chromium
LIMITATIONS: Method does not have the sensitivity or precision of atomic absorption or
other conventional methods. Cadmium, manganese, barium, and mercury may be de-
tected, but only at high concentrations due to spectral overlap of other elements.
Sample matrix effect may cause significant accuracy problems and can never be elimi-
nated fully. (Matrix effects include non-homogeneity, surface conditions, and spectral
interferences).
INSTRUMENTATION USED: XRF 840 analyzer electronic unit; HEPS sample probe,
either Cm-244 or Am-241 radioisotope, or both.
PERFORMANCE SPECIFICATION
DETECTION LIMIT: 15 mg/kg for arsenic, to 140 mg/kg for iron but dependent on site-
specific matrix and calibration techniques.
SELECTIVITY: Elements may be identified by looking at various emission X-rays (i.e., K-
alpha, K-beta).
ACCURACY: Student's t-test and Wilcoxin's test show agreement between XRF and CLP
data at a 95% confidence level for As, Cu, Pb, Zn, and Fe. (Number of samples ranged
from 26-45.)
PRECISION/REPEATABILITY: Coefficient of variation = + 20% at detection limit and .+
5% at higher values for all elements tested.
COMMENTS: Detection limit is directly related to the total number of x-rays counted and
the number of x-rays due to interferences and background. Average RPD is about 27%;
18% may be due to sample non-homogeneity, 6% to instrument error and 3!! due to the
grinding process. Laboratory XRF analyzer offers better sensitivity performance.
USE
LOCATION USED: Smuggler Mountain Site, Aspen, Colorado, 1985
-------
EPA SITE NUMBER (CERCLIS): COD980806277
MATRIX: Soil
PREPARATION, MAINTENANCE AND CLEANUP: The XRF analyzer must be set up and
programmed. Maintenance includes checking the probe for cleanliness and dryness and
checking for source decay.
ANALYSIS TIME: 10-30 minutes for sample preparation, depending on moisture content
of the soil. Actual analysis averages 5 minutes per sample.
CAPITAL COSTS: $50,000
CALIBRATION: Sample calibration includes measurements of pure element calibratior,
standards, measurements of site specific samples with known analyte concentrations,
input of calibration standard concentrations, and calculation of calibration coefficients.
Midpoint standards should be rechecked after five samples, if deviation of standards is
greater than 3%, recalibrate instrument.
COMMENTS: XRF is non-destructive; the samples can therefore be stored for future ref-
erence after analysis, Personnel training is required. Data reporting format is either
direct LCD read-out or paper printout if interfaced with a printer.
PROTOCOL AVAILABLE: Yes
SOURCE
CONTACT NAME: Richard Chappell
AFFILIATION: COM INC.
TELEPHONE: (303)458-1311
PREPARED: April 6, 1987
BIBLIOGRAPHY
Chappell, R.W., Davis, A.O. and Olsen, R.L., "Portable X-Ray Fluorescence as a
Screening Tool for Analysis of Heavy Metals in Soils and Mine Waste." Management of
Uncontrolled Hazardous Waste Sites, Washington, D.C. December 1-3, 1986.
Chappell, R.W. and Olsen, R.L., EPA Memorandum, "XRF Field Analysis of Smuggler
Mountain Soil Samples," January 13, 1986.
Columbia Scientific industries Corporation, "Operating instructions X-MET 840 Portable
XRF Analyzer", March 1985.
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METHOD FM-4: AIR MONITORING FOR VOLATILE ORGANIC COMPOUNDS USING
PROGRAMMED THERMAL DESORBER (PTD) AND GC
SUMMARY: Air monitoring of volatile organics as a time-weighted average to ug/l range.
Time consuming. Requires field laboratory.
METHOD DESCRIPTION: Uses a field sampling pump, programmed thermal desorber,
and a GC to evaluate volatile organic contaminants in air samples as a time-weighted
average. Identification and quantitation is done by comparing peak retention times and
heights of peaks with standards. Sample acquisition involves collecting an adequate
sample (usually 10-30 liters) of ambient air using a Tenax or activated carbon tube at-
tached to a pump. The sample is thermally desorbed in the PTD. Two samples are with-
drawn from the PTD and analyzed on the GC. The first sample is usually a small volume
"preliminary" sample, and the second is a larger volume sample, based on results from
the first.
APPLICATION: Air monitoring as a time-weighted average for low molecular weight vola-
tile organic compounds; aromatics; unsaturated hydrocarbons; chlorinated hydrocarbons;
ketones; alcohols, etc.
LIMITATIONS: Time consuming; samples take 4-8 hours to collect. Desorption efficiency
is less than 100%. Pre-packed Tenax tubes may be contaminated. Packing own tubes is
recommended but requires laboratory and chemist,
INSTRUMENTATION USED: Century Systems Programmed Thermal Desorber,
Model 132 A.
Century Systems (Foxboro) Organic Vapor Analyzer or other comparable GC or GC/MS
(e.g., Photovac, Finnigan, etc.).
PERFORMANCE SPECIFICATION
DETECTION LIMIT: 1.0 ug/l using the Photovac or Finnigan GC/MS for most volatile or-
ganics; or 500 ug/l using Foxboro OVA for most volatile organics.
SELECTIVITY: Good separation of peaks,
ACCURACY: 99% recovery of eleven spiked vinyl chloride samples using freshly packed
coconut charcoal tubes; lower recovery In other tests possibly related to spiking method.
PRECISION/REPEATABILITY: Standard deviation of spiked vinyl chloride samples was
approximately 10%.
COMMENT: Recoveries varied according to type and condition of carbon tube used and
number of components in sample. With 8 components, recovery ranged from 3-106%;
for 4 components, recovery range was 63-135%.
USE
LOCATION USED: Has been used at 30-50 locations in New England and elsewhere.
-------
EPA SITE NUMBER (CERCLIS): Not Available
MATRIX: Air
PREPARATION, MAINTENANCE AND CLEANUP: Tubes are prepared by thermally de-
sorbing in PTD and cleaned to background levels (less than 1 ug/l). If tubes are dirty or
contaminated they may have to be cleaned and repacked or replaced.
ANALYSIS TIME: 4-8 hours for sample collection; 5 minutes desorbing;
5 minutes analysis time.
CAPITAL COSTS: $5,990 for Model 132A PTD; $5,200-$6,325 for OVA
CALIBRATION: Calibration determined by peak heights and retention times for stan-
dards. Run standards as for GC or GC/MS.
COMMENTS: The Interpretation of results requires a trained chemist. Method is used on
average 2-3 times per year in Region I.
PROTOCOL AVAILABLE: Yes.
SOURCE
TECHNICAL CONTACT: Dr. Thomas Spittler
AFFILIATION: U.S. EPA Region I Laboratory
TELEPHONE: (617) 861-6700
PREPARED: April 7, 1987
BIBLIOGRAPHY
Spittler, T.M., Siscanaw, R.J. and Lataille, M.M., "Correlation between Field GC.
Measurement of Volatile Organics and Laboratory Confirmation of Collected Field
Samples Using the GC/MS." National Conference on Management of Uncontrolled
Hazardous Waste Sites, November 29 -
December 1, 1982, Washington, D.C.
Chapman H. and Clay P., Field Investigation Team (FIT) Screening Methods and Mobile
Laboratories Complementary to Contract Laboratory Program (CLP). TDD-HQ-8507-01,
October 17, 1986.
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METHOD FM-5 VOLATILE ORGANIC COMPOUND (VOC) ANALYSIS USING GC WITH
AUTOMATED HEADSPACE SAMPLER
SUMMARY: Rapid determination of VOCs to 10 ug/l in water and 10 ug/kg in soil.
Requires field laboratory. Results are tentative. Method yet to be used in field.
METHOD DESCRIPTION: Requires a field laboratory with an automated headspace sam-
pler interfaced to a GC equipped with a PID and ECD in series to screen VOCs in soil
and water. Identification and quantitation by comparison of standard peak retention times
and peak areas with sample. Method for water consists of transferring 1 ml of water
sample to a 3 ml reaction vial. For soil, method consists of transferring 1 gram of
sample to 3 ml reaction vial. Add 1 ml of surrogate standard to each sample. Set
headspace sampler temperature at 6OoC. Load sampler and analyze samples.
APPLICATION: Good for most VOCs to low ug/kg ranges; halogenated hydrocarbons,
chlorinated hydrocarbons, aromatics, etc.
LIMITATIONS: Complex samples give co-eluting peaks. Results, especially for soil, are
semi-quantitative. Method has not been used in the field.
INSTRUMENTATION USED: Perkin-Elmer 2000 with HNU PID detector and Tracer Hall
detector. Hewlett Packard Model 19395A automated headspace sampler.
PERFORMANCE SPECIFICATION
DETECTION LIMIT: 10 ug/l for most VOCs in water. 20 ug/l for some halogenated aro-
matics. 10 ug/kg for most VOCs in soil.
SELECTIVITY: Peaks are separate, occasional overlapping peaks.
ACCURACY: At low concentrations (1O-50 ug/l) good correlation to GC/MS data. At
higher levels, there is a discrepancy between data sources by a factor of two. Bias
ranged from high to low with increasing concentrations.
PRECISION/REPEATABILITY: Not available.
COMMENTS: This method was developed by Region IV and until recently was not used
as a quantitative method.
USE
LOCATION USED: Not used in field.
EPA SITE NUMBER (CERCLIS): Not applicable
MATRIX: Air (Headspace above soil, sediment, or water)
PREPARATION, MAINTENANCE AND CLEANUP: Column and detector cleaning and re-
conditioning almost nonexistent because of the nature of headspace analysis. Samples
must equilibrate in sampler 1 hour before analysis.
10
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ANALYSIS TIME: 30-40 nin/sample
CAPITAL COST: Approximately $20,000 for Perkin-Elmer GC with PID and ECD.
Approximately $8,000 for Hewlett Packard headspace sampler.
CALIBRATION: 3-point standard calibration curve necessary to accurately quantify com-
pounds detected by GC. Single point calibration is adequate for semiquantitative data.
Standard is known quantity of organic vapor in equilibrium with air with an aqueous or-
ganic solution.
COMMENTS: The interpretation of results requires a trained chemist. This method has
been used in Region IV laboratory but has yet to be used in the field.
PROTOCOL AVAILABLE: Yes.
SOURCE
TECHNICAL CONTACT: William Loy
AFFILIATION: U.S. EPA Region IV ESD.
TELEPHONE: (404) 546-3386
PREPARED: April 16, 1987
BIBLIOGRAPHY
Screening Method for Volatile Organic Compounds, EPA Region IV Mobile Laboratory
Protocol, January 1987.
11
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METHOD FM-6: HEADSPACE TECHNIQUE USING AN ION DETECTOR FOR VOC
ANALYSIS
SUMMARY: Analysis of soil, water, and air samples for identification and quantitation of
most VOCs to ug/l range. The ion detector is a GC/MS system. Requires field laboratory.
Soil results are semi-quantitative.
METHOD DESCRIPTION: Used to screen water, soil and sediment samples for volatile
organic compounds (VOC) on an ion trap detector- a gas chromatograph/mass spectral
(GC/MS) system - in a field laboratory. GC separates the compounds and Introduces
them into MS which provides positive identification of peaks. Quantitation is determined
by peak areas on GC. Method Involves collecting desired sample in a 40 ml vial, prepar-
ing sample (if soil) and sampling the vapor headspace above solution. It is then analyzed
on ion trap detector. Air is screened directly by collecting sample and injecting it into GC
for analysis.
APPLICATION: Good for most VOCs to 1 ug/l concentrations; unsaturated hydrocarbons,
halogenated hydrocarbons, aromatics, etc. Mass spectrum good for more positive identi-
fication of compounds.
LIMITATIONS: Results for soil are semi-quantitative. High initial cost.
INSTRUMENTATION USED: Finnigan Ion Trap Detector (ITD) 700 series with
IBM PC/XT
PERFORMANCE SPECIFICATION
DETECTION LIMIT: 1 ug/l for most VOCs
SELECTIVITY: Excellent identification capabilities even in the presence of co-eluting
peak.
ACCURACY: SIX-point calibration curve yielded 0.964 correlation coefficient.
PRECISION/REPEATABILITY: Six-point calibration curve showed 20% relative standard
deviation.
COMMENT: Performance specifications were taken from headspace of water samples.
USE:
LOCATION USED: Adamstown, Maryland; Well Water Analysis, August 1986.
EPA ID NUMBER: Non-CERCLIS
MATRIX: Air (Headspace above soil, sediment, and water)
PREPARATION, MAINTENANCE AND CLEANUP: Columns and detector must be cleaned
and reconditioned occasionally. Care must be taken not to saturate the column with con-
centrated samples.
12
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ANALYSIS TIME: 10-20 minutes/sample
CAPITAL COST: Approximately $40,000 for ITD with IBM PC/XT
CALIBRATION: Standards necessary to identify and quantify compounds. The standard
is a known quantity of an organic vapor, which is in equilibrium with either air or an
aqueous or water-organic solution. Minimum of three points should be used to develop
calibration curve.
COMMENTS: The interpretation of results requires a trained chemist. Method has seen
limited use.
PROTOCOL AVAILABLE: No
SOURCE:
CONTACT NAME: James Jerpe
AFFILIATION: EPA Region iii Central 'Laboratory
TELEPHONE: (301)266-9180
PREPARED: April 23, 1987
BIBLIOGRAPHY
Chapman, H. and Clay, P., "Field investigation Team (FIT) Screening Methods and
Mobile Laboratories Complementary to Contract Laboratory Program (CLP), n TDD-HQ-
8507-1, October 17, 1986, (Draft).
13
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METHOD FM-7: HEADSPACE TECHNIQUE USING AN OVA (FID) - VOLATILE
ORGANIC COMPOUNDS
SUMMARY: Rapid analysis of total VOCs or identification of individual components in
soil, water, or air. OVA is portable. Soil results are semi-quantitative. Field instruments
give better sensitivity.
METHOD DESCRIPTION: Used to screen water, soil, and sediment samples on an
OVA- a portable GC equipped with a flame ionization detector. Method involves collect-
ing samples in a 40 ml vial, preparing sample if it is soil or sediment, and sampling the
vapor headspace above the aqueous solution. The vapor sample is analyzed by the OVA.
Air may be screened directly by injecting it into the OVA. Identification and quantitation
determined by comparing the peaks of standards to samples. A modification of this
method involves placing the probe directly above the soil sample or inserting the probe
directly into a shallow bore hole.
APPLICATION: Analysis for low molecular weight total volatile organic concentration or
for identification of specific constituents with the use of proper standards.
LIMITATIONS: Measures volatile organics only. Highly volatile organics such as methane
tend to skew analysis for total VOCs. Light VOCs (e.g., vinyl chloride) are rapidly eluted
from column and are difficult to detect. Response given in methane equivalent. OVA op-
erates at ambient temperatures; therefore for reproducibility, surrounding temperatures
must remain constant.
INSTRUMENTATION USED: Century Systems (Foxboro) Organic Vapor Analyzer (Model
128).
PERFORMANCE SPECIFICATION
DETECTION LIMIT: 500 ug/l for most volatile organics.
SELECTIVITY: Early peaks tend to overlap. Later peaks easily identifiable.
ACCURACY: Calibration error (for benzene) ranged from 25% of value at detection limit
(0.74 mg/kg) to 14% at higher concentrations (165 mg/kg).
PRECISION/REPEATABILITY: Coefficient of variance = l-4% for five standard samples
of benzene and carbon tetrachloride. Duplicate samples show good agreement.
COMMENT: Performance specifications are for air; results for soil/sediment semi-
quantitative.
USE
LOCATION USED: Ottadi & Gross (Kingston Steel Drum); Kingston, NY 1980.
EPA SITE NUMBER (CERCLIS): NHD990717647
MATRIX: Air (Headspace above soil, sediment, and water)
14
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PREPARATION, MAINTENANCE AND CLEANUP: Columns must be cleaned every 3
months. Recharge batteries after use.
ANALYSIS TIME: 20 samples per hour.
CAPITAL COSTS: $7,000.
CALIBRATION: Standards necessary to identify and quantify compounds detected by
GC. The standards are run before screening field samples.
COMMENTS: The interpretation of results requires a trained chemist. The column can
easily be saturated by concentrated samples, resulting in an inoperable unit. Method Is
routinely used in Region I.
PROTOCOL AVAILABLE: Yes
SOURCE
TECHNICAL CONTACT: Dr. Thomas Spittler
AFFILIATION: U.S. EPA Region I Laboratory
TELEPHONE: (617)861-6700
PREPARED: April 7, 1987
BIBLIOGRAPHY
Quimby, J.M., Cibulskis, R.W. and Gruenfeld, M., "Evaluation and Use of a Portable Gas
Chromatograph For Monitoring Hazardous Waste Sites. "National Conference on
Management of Uncontrolled Hazardous Waste Sites,
November 29 - December 1, 1982, Washington, D.C.
15
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METHOD FM-8: HEADSPACE ANALYSIS USING HNU (PID) FOR TOTAL VOLATILE
ORGANICS
SUMMARY: Portable instrument that gives rapid analysis of total organic vapor con-
centrations in water, soil, and sediment to 100 ug/l benzene equivalent.
METHOD DESCRIPTION: Used to screen water, soil, and sediment samples for total or-
ganic vapor concentration. HNU is a portable photoionization detector that requires inter-
nal electronic calibration as well as calibration to a known standard. After sample is
collected, it can be analyzed by inserting probe of HNU into headspace of jar.
Alternative procedures to place probe directly above soil or insert probe into a shallow
hole.
APPLICATION: Measures total organic vapor concentration. Response to VOC varies
with probe used. Insensitive to methane. May detect unsaturated hydrocarbons, chlorin-
ated hydrocarbons, aromatics, nitrogen and sulfur compounds, aldehydes, ketones, alco-
hols, acids, and others.
LIMITATIONS: Not able to identify Individual compounds. Total response reported as
benzene equivalent. High ambient humidity causes erratic responses (usually low).
INSTRUMENTATION USED: HNU Systems PI 101 Portable Photoionizer. Available probes
include 9.5 ev, 10.2 ev and 11.7 ev.
PERFORMANCE SPECIFICATION
DETECTION LIMIT: 100 ug/l for most volatile organics. Linear operating range for most
compounds is IOO-60,000 ug/l. Useful range extends to 200,000 ug/l.
SELECTIVITY: Depends on probe.
ACCURACY: Not tested.
PRECISION/REPEATABILITY: 1% at Full Scale Deflection. Duplicate samples show good
agreement.
COMMENTS: Three probes are available that vary in sensitivity to organic compounds.
One probe (9.5 ev) detects aromatics and large molecules. The 10.7 ev probe detects
the above compounds plus vinyl chloride, MEK, TCE and other 2-4 carbon compounds.
The 11.7 ev probe detects the above compounds plus halocarbons, methanol, and other
single carbon compounds.
USE:
LOCATION USED: Ottadi & Gross (Kingston Steel Drum); Kingston, NY, 1980.
EPA SITE NUMBER (CERCLIS): NHD990717647
MATRIX: Air (Headspace above soil, sediment, and water)
PREPARATION, MAINTENANCE AND CLEANUP: Recharge battery after use. Clean light
source window every few weeks,
16
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ANALYSIS TIME: Response given in less than 5 seconds
COST: $5,000.00
CALIBRATION: Zero electronically at start of day. Check periodically. Use calibration gas
prior to each use.
COMMENTS: Easy to train personnel in usage. Used fairly regularly.
PROTOCOL AVAILABLE: No.
SOURCE
TECHNICAL CONTACT: Or. Thomas Spittler
AFFILIATION: U.S. EPA Region I Laboratory
TELEPHONE: (617)861-6700
PREPARED: April 13, 1987
BIBLIOGRAPHY
Becker, D.L. and Carter, M.H., "Equipment Available for Sampling and On-Site
Measurements." U.S. EPA, Document Number HQ-831104, May 30, 1984.
17
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METHOD FM-9 HEADSPACE TECHNIQUE USING A MOBILE GC FOR VOLATILE
ORGANICS (VOCS)
SUMMARY: Analysis of soil, water, and air samples for identification and quantitation of
most VOCs to 0.5 ug/l range. Soil results are semi-quantitative, Depending on GC used,
is portable or requires field laboratory.
METHOD DESCRIPTION: Used to screen water, air, soil, and sediment samples on a GC
with a.PID, FID or ECD. Method involves collecting desired sample in a 40 ml vial, pre-
paring sample if soil or sediment, and sampling and analyzing vapor headspace above
aqueous solution. Air screened directly by collecting sample and injecting into GC for
analysis. Identification and quantitation is determined by comparing peak retention times
and areas of standard solution to samples.
APPLICATION: Good for most VOCs to low concentrations; halogenated methanes and
ethanes, chlorinated hydrocarbons, aromatics, etc; arsine, phosphine, hydrogen sulfide,
and carbon disulfide.
LIMITATIONS: GC and sample need to be at same temperature in an area free of or-
ganic vapor. For reproducibility, surrounding temperature must remain constant, Complex
samples give co-eluting peaks. Identifications are considered tentative for soil.
INSTRUMENTATION REQUIRED: Photovac Model 10AIO equipped with PID and 4 foot
SE-30 column; AID 511 equipped with FID or ECD and 3-foot SE-30 column; Shimadzu
GC Mini-2 and GC Mini-3 with FID and 6-foot SP-1000 and AT-1000 column; HNU Model
GC-301 with PID or FID and Standard SE-column.
PERFORMANCE SPECIFICATION
DETECTION LIMIT: 1 ug/l for aromatics; 40 ug/l for some chlorinated hydrocarbons.
SELECTIVITY: Peaks are separate, good selectivity.
ACCURACY: 27-32% RPD (Standard Deviation) (70 TCE and PCE samples).
PRECISION/REPEATABILITY: Duplicate samples show very good agreement.
COMMENTS: Results given for Photovac, the most common GC used. Others give simi-
liar results.
USE
LOCATION USED: Norwalk Harbor, Conn. Winter 1981
EPA SITE NUMBER (CERCLIS): Non-CERCLA
MATRIX: Air and headspace above soil, sediment, and water.
PREPARATION, MAINTENANCE AND CLEANUP: Optional backflush valve allows for
flushing of contaminants from column. Column conditioning done every third month by
heating to 100% and flushing with helium.
18
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ANALYSIS TIME: 10-20 minutes.
CAPITAL COSTS: Photovac: $14,000.00
AID 511: $5,020.00
Shimadzu: $4,100.00-$5,200.00
HNU-301: $6,350.00
CALIBRATION: Standard necessary to identify and quantify compounds detected by GC.
Standard is a known quantity of organic vapor in equilibrium with air or an aqueous or
organic solution. Standards run before screening field samples and after every 5
samples..
COMMENTS: The interpretation of results requires a trained chemist. The column can
easily be saturated by concentrated samples, resulting in an inoperable unit. Used
routinely.
PROTOCOL AVAILABLE: Yes
SOURCE
TECHNICAL CONTACT: Dr. Thomas Spittier
AFFILIATION: U.S. EPA Region I Laboratory
TELEPHONE: (617)861-6700
PREPARED: April 7, 1987
BIBLIOGRAPHY
Chapman, H. and Clay, P., "Field investigation Team (FIT) Screening Methods and
Mobile Laboratories Complementary to Contract Laboratory Program (CLP)," TDD HQ-
8507-01, October 17, 1986. (Draft).
Clark, A.E., Latailie, M. and Taylor, E.L., "The Use of a Portable PID Gas
Chromatograph for Rapid Screening of Samples for Purgeable Organic Compounds in
the Field and in the Lab," U.S. EPA Region I Laboratory,
June 29, 1983.
Morin, S.O., "Development and Application of an Analytical Screening Program to
Superfund Activities," Management of Uncontrolled Hazardous Waste Sites, Washington,
D.C. November 4-6. 1985.
19
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METHOD FM-IO: PASSIVE SOIL GAS SAMPLING USING INDUSTRIAL HYGIENE
SAMPLERS
SUMMARY: Passive sampling for volatile organics as a way to detect and estimate
ground water contamination. Concentrations obtained by calculation. Site conditions
affect results. Field laboratory or off-site analysis possible.
METHOD DESCRIPTION: Passive sampling using open, inverted l-quart metal cans con-
taining an activated carbon organic vapor monitor are buried at one-foot depths in area
to be sampled, exposed for a time determined by sampling rate for target chemical and
anticipated soil concentrations of target chemical (8 hours to 1 month), followed by sol-
vent desorption in off-site or field laboratory and GC analysis (with ECD, PID or FID).
Soil gas concentration of chemical by volume is calculated using results of analysis,
sample exposure time, and sampling rate for chemical of interest.
APPLICATION: Assessment of VOC ground water contamination plume by soil gas
sampling.
LIMITATIONS: Does not provide ground water contaminant concentrations directly; is an
indirect method. Site conditions affect method.
INSTRUMENTATION USED: Activated carbon organic vapor monitors (#3500, 3M, St.
Paul, MN). Various GCs and column configurations have been successfully used includ-
ing the HP 5710 GC/ECD, the AID GC/ECD and the HNu 301 GC/FID/PID.
PERFORMANCE SPECIFICATION
DETECTION LIMIT: Depends on GC used, local conditions, and exposure time.
SELECTIVITY: Volatile organics; depends on GC method used.
ACCURACY: Correlation of 0.93 between this technique and grab samples obtained ear-
lier; correlation of 0.79 with ground water monitoring results.
PRECISION/REPEATABILITY: Based on closely spaced samples. 12% RSD
over 27'.
COMMENTS: Need to demonstrate, precision and correlation with ground water
contamination at each site. Test precision using closely spaced samplers, and evaluate
correlation with ground water data by regression analysis.
USE
LOCATION USED: Pittman Lateral, Henderson, NV (Numerous other locations).
EPA SITE NUMBER (CERCLIS): Non-CERCLA
MATRIX: Soil
PREPARATION, MAINTENANCE AND CLEANUP: Solvent desorption required before GC
analysis.
20
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ANALYSIS TIME: Sample collection time varies depending on analytical sensitivity, ex-
pected concentration of contaminant, etc. Sample processing involves solvent desorption
(1/2 hour) and GC analysis (15-30 min/sample).
CAPITAL COST: Not available
CALIBRATION: Check validity of method under site conditions.
COMMENTS: One of several soil gas sampling methods that may be applicable under
various circumstances. Clay layers and horizons with
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METHOD FM-11: SOIL GAS SAMPLING USING MINI-BARREL SAMPLER
SUMMARY: Method to collect soil gas samples when low concentration expected. Soil
aliquots are directly removed and prepared. Headspace gas is withdrawn and injected
into GC. Analysis can be performed using portable GC, field and/or off-site laboratories.
METHOD DESCRIPTION: A coring tool is used along with an auger or backhoe to collect
the sample. Samples are forced into screw-cap vials by a sampling extruder. Deionized/
distilled water is added to the vial, which is then heated, agitated, and samples are with-
drawn for GC analysis.
APPLICATIONS: Suited for low-concentration contaminants with low vapor pressures or
where sample contaminants need to be concentrated in a headspace to be within detec-
tion limits of the analytical instrument.
LIMITATIONS:
INSTRUMENTATION USED: Mini-barrel borehole sampler and sample extruder.
PERFORMANCE SPECIFICATION
DETECTION LIMITS: Suited for low-concentration contaminants.
SELECTIVITY: Volatile organics.
ACCURACY: Not Known
PRECISION/REPEATABILITY: Not Known
COMMENTS: Clay layers and horizons with <5% air-filled porosity reduce effectiveness
of soil gas sampling. Compare with other sampling techniques to determine applicability
at each site.
USE
LOCATION USED: Not available
EPA SITE NUMBER (CERCLIS): Not applicable
MATRIX: Soil.
PREPARATION, MAINTENANCE AND CLEANUP: N/A
ANALYSIS TIME: N/A
CAPITAL COST: Not Available
PROTOCOL AVAILABLE: Yes.
22
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SOURCE
TECHNICAL CONTACT: Andrew Hafferty
AFFILIATION: Ecology and Environment, Inc.
TELEPHONE: (206) 624-9537
PREPARED: May 6, 1987
BIBLIOGRAPHY
Chapman, H., and Clay, P., Field Investigation Team (FIT) Screening Methods and
Mobile Laboratories Complementary to Contract Laboratory Program (CLP), TDD-HQ-
8507-01, October 17, 1986 (Draft).
23
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METHOD FM-12: SOIL GAS SAMPLING USING A ONE-LITER SYRINGE
SUMMARY: Rapid sampling of soil gas for on-site analysis to determine contaminant
plume; repeated sampling not possible once auger removed. GC analysis can be per-
formed in a field laboratory.
METHOD DESCRIPTION: Sample is obtained as follows: drill hole using hollow-stem
auger; lower a length of Teflon tubing attached to a l-liter, gas-tight syringe to the de-
sired sampling depth. Condition Teflon line by drawing a 500 ml air sample, detach and
evacuate the syringe, reattach and draw 1-liter sample, which is injected Into a purge
and trap unit for concentration and GC analysis.
APPLICATION: Soil sampling for GC analysis to aid in contaminant plume delineation.
LIMITATIONS: Relatively long analysis time; no repeated sampling once auger is re-
moved; variation in injection rate can lead to VOC breakthrough in the purge and trap
unit.
INSTRUMENTATION USED: Sampling: l-liter, gas-tight syringe, syringe pump. Analysis:
GC with a purge and trap unit.
PERFORMANCE SPECIFICATION
DETECTION LIMIT: Sensitivity improved over other sampling techniques by sample con-
centration (0.2-0.02 ug/l for TCE).
SELECTIVITY: Volatile organics; depends on GC method used for analysis.
ACCURACY: High correlation with other sampling techniques: Correlation coefficients
were 0.68 with direct injection auger; 0.88 with soil headspace; 0.87 with direct Injection-
stopper; 0.90 with Tenax tube.
PRECISION/REPEATABILITY: N/A
COMMENTS: Sensitivity depends on GC used; concentrating techniques overcome some
field GC limitations. Clay layers and horizons with <5% air-filled porosity reduce effec-
tiveness of soil gas sampling. Method should be tested at each site by comparing to
results of other sampling techniques.
USE
LOCATION USED: Puget Sound, WA, 1986.
EPA SITE NUMBER (CERCLIS): Not Available
MATRIX: Soil.
PREPARATION, MAINTENANCE AND CLEANUP: Syringes and tubing must be cleaned
(e.g., using vacuum heated syringe cleaner following sample injection); nitrogen gas
flushing. Decontamination of auger & syringes required for reuse.
24
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ANALYSIS TIME: Drilling borehole- 15-30 min; sample collection- 1 min; GC
analysis- 30 minutes.
CAPITAL COSTS: Syringe ($30-40); pump($IOO-500); Both are reusable.
GC$4,100-$20,000,
CALIBRATION: N/A
COMMENTS: Simple sample collection. May perform better than Direct Injection - Auger
sampling when most appropriate analytical equipment used. Allows adjustment of sam-
pling area for further investigation based on immediate results.
PROTOCOL AVAILABLE: No.
SOURCE
TECHNICAL CONTACT: John Ryding
AFFILIATION: C.C. Johnson & Malhotra
TELEPHONE: (303) 433-6966
PREPARED: May 6, 1987
BIBLIOGRAPHY
Jowise, P. P., Villnow, J. D., Gorelik, L. I., Ryding, J. M., "Comparative Analysis of Soil
Gas Sampling Techniques," Management of Uncontrolled Hazardous Waste Sites,
Washington, D.C., December 1-3, 1986, p. 193-199.
25
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METHOD FM-13: SOIL GAS SAMPLING USING DIRECT INJECTION - STOPPER
SUMMARY: Sampling of VOCs in soil gas to determine ground water contaminant
plume. Requires probe installation for equilibration and repeated sampling. Analysis can
be performed using portable GC and/or field laboratory.
METHOD DESCRIPTION: A 12-17-foot borehole is drilled using a hollow-stem auger (8"
O.D.). A sample probe is inserted, borehole walls are allowed to collapse as the auger is
pulled. The hole is sealed with a bentonite-slurry plug, the probe is sealed with a stopper
and screw cap. Samples are collected by syringe after a 2-day equilibration period and
analyzed by a GC.
APPLICATION: Delineation of extent of contamination; long-term sampling of true soil
gas concentrations.
LIMITATIONS: Probe installation required.
INSTRUMENTATION USED: Auger for drilling, gas-tight syringes for sampling; GC for
analysis.
PERFORMANCE SPECIFICATION
DETECTION LIMIT: 0.2 ug/l for TCE in one study.
SELECTIVITY: Volatile organics; depends on GC method used.
ACCURACY: Results correlated well with results from other sampling methods at same
locations: Correlation coefficients were 0.78- direct injection-auger; 0.87- one-liter
method; 0.73- headspace method; 0.98- Tenax.
PRECISION/REPEATABILITY: Field variability - 33% RSD for 42 samples.
COMMENTS: Occasional leaks in stoppers increased variability. Water contamination ac-
curately reflected; however, number of samples was small and correlation may be
misleading. Sensitivity depends on GC used. Clay layers and horizons with <5% air-filled
porosity reduce effectiveness of soil gas sampling. Compare to other sampling methods
to assess applicability to a particular site.
USE
LOCATION USED: Puget Sound, WA, 1986.
EPA SITE NUMBER (CERCLIS): Not Available
MATRIX: Soil.
PREPARATION, MAINTENANCE AND CLEANUP: Determine appropriate drilling depth by
use of test holes (need to drill below surface soils to bypass competing adsorption sinks)
or by combined experience and assessment of site factors. Auger and syringe
decontamination required. Periodic direct mixing of probe contents needed before sam-
pling to provide equilibrium conditions along probe length. Minimal sample preparation
required before analysis.
26
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ANALYSIS TIME: 15-30 minutes to drill boreholes; 2 days for sample probe equilibration;
1 minute to collect sample.
CAPITAL COST: Syringes ($30-40) probes ($100) plus drilling equipment
GC: $4,100 - $20,000
CALIBRATION: Purge syringes with nitrogen and check for contamination by injecting
carrier gas samples Into GC. Periodic mixing of probe contents.
COMMENTS: Long-term changes in soil gas concentration will not be evident without
mixing of probe contents.
PROTOCOL AVAILABLE: Yes.
SOURCE
TECHNICAL CONTACT: John Ryding
AFFILIATION: C.C. Johnson & Malholtra
TELEPHONE: (303) 433-6966
PREPARED: May 6, 1987
BIBLIOGRAPHY
Jowise, P.P., Villnow, J.D., Gorelik, LI., and Ryding, J.M., "Comparative Analysis of Soil
Gas Sampling Techniques," Management of Uncontrolled Hazardous Waste Sites,
Washington, D.C., December 1-3, 1986, p.193-199.
27
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METHOD FM-14: SOIL GAS SAMPLING USING A PERFORATED TUBE
SUMMARY: Grab or composite soil gas samples obtained using pipe with perforated tip
driven into ground. Analysis can be performed using portable GC, field laboratory and/or
off-site laboratory.
METHOD DESCRIPTION: A non-reactive rod or pipe with a perforated tip is driven into
the ground to the desired sampling depth. A pump is used to withdraw soil gas through
Teflon tubing, from which grab samples can be taken using a syringe, or composite
samples obtained by adding Tenax or other adsorbent material in the collection line
along with a flow meter to measure air volume sampled. A water trap is used in some
applications.
APPLICATION: Sampling of VOCs in the soil pore spaces in the unsaturated zone to
assess extent of contamination.
LIMITATIONS: Aerobic degradation of hydrocarbons may occur in some areas at shallow
sampling depths. Sample leakage from probe or syringe possible.
INSTRUMENTATION USED: Perforated pipe, Teflon tubing, gas-tight glass syringe,
vacuum pump.
PERFORMANCE SPECIFICATION
DETECTION LIMIT: Not Known
SELECTIVITY: Volatile organics; affected by GC method used.
ACCURACY: Not Known
PRECISION/REPEATABILITY: Not Known
COMMENTS: Clay layers and horizons with < 5!! air-filled porosity reduce effectiveness
of soil gas sampling. Precision and ground water correlation must be demonstrated for
each site. Determine applicability to each site by comparing to other sampling
techniques.
USE
LOCATION USED: Tucson International Airport.
EPA SITE NUMBER (CERCLIS): CR811018010
MATRIX: Soil.
PREPARATION, MAINTENANCE AND CLEANUP: Flushing of sampling equipment with
nitrogen gas is effective in preventing contamination. Inject carrier gas samples into GC
to check for contamination. Draw air through soil gas probes and inject into GC to check
for contamination. Teflon may be subject to carry-over from high liquid or gas-phase
concentrations.
28
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ANALYSIS TIME: NA
CAPITAL COST: Sampling probes ($100) each; syringes ($30-40), Sampling pump ($100-
500). All are reusable. GC: $4,100 - $20,000
CALIBRATION: Pump should be calibrated if used for composite samples.
COMMENTS: One of several soil gas sampling methods that may be applicable under
various circumstances.
PROTOCOL AVAILABLE: Yes.
SOURCE
TECHNICAL CONTACT: Andrew Hafferty
AFFILIATION: Ecology and Environment, Inc.
TELEPHONE: (206) 624-9537
PREPARED: May 6, 1987
BIBLIOGRAPHY
Chapman, H., and Clay, P., Field Investigation Team (FIT) Screening Methods and
Laboratories Complementary to Contract Laboratory Program, TDD-HQ-8507-01, October
17, 1986 (Draft)
Marrin, D.L., Thompson, G.M., Investigation of Volatile Contaminants in the Unsaturated
Zone Above TCE Polluted Groundwater, EPA Project I.D. CR811018010, October 10,
1984.
29
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METHOD FM-15: SOIL GAS SAMPLING USING TENAX TUBES
SUMMARY: Sampling (long-term and time-averaged) of soil gas for on-site analysis to
determine volatile organic contaminant plume. Requires use of sampling probe and pre-
conditioning of Tenax tubes. Analysis can be performed in a field laboratory or offsite
laboratory.
METHOD DESCRIPTION: Stainless steel desorption tubes packed with Tenax are
suspended inside a stoppered sampling probe and connected to a pump. Three liters of
soil gas are drawn through each tube, concentrating the contaminant on the adsorbing
material. In a field laboratory, contaminants are driven off thermally and analyzed using a
GC.
APPLICATION: Soil sampling to aid in contaminant plume delineation, especially where
very low concentrations expected.
LIMITATIONS: Sampling probe installation necessary. Tenax tubes must be precondi-
tioned. Sampling requires lengthy pumping. Pre-packed Tenax tubes often contaminated;
recommend packing own tubes, but requires laboratory and chemist.
INSTRUMENTATION USED: Tenax-filled desorption tubes; calibrated air pump; thermal
desorber; gas-tight syringe.
PERFORMANCE SPECIFICATION
DETECTION LIMIT: Sensitivity improved over other sampling techniques by sample con-
centration; calculated 0.02 ug/l forTCE (10x below detection limit of GC used).
SELECTIVITY: Volatile organic contaminants; depends on GC method used for analysis.
ACCURACY: High correlation with other sampling techniques direct:
injection-auger- 0.80; headspace sampler- 0.84; one-liter technique- 0.90; direct in-
jection - stopper- 0.98. Also, high correlation with concentrations in water (0.80 & 0.99
In two sample groups). Percent recovery is unknown.
PRECISION/REPEATABILITY: RSD = 24% for 10 samples from a single location over a
4-week period. For three sets of triplicate samples from different locations, RSDs were
5%, 10%, and 44%, varying inversely with concentration.
COMMENTS: Variation in results is mainly due to the nature of soil gas sampling rather
than the subsequent analysis unless contaminant concentrations are very low. Correlation
with ground water contaminant concentrations may be misleading. Sensitivity depends on
GC used; concentrating method overcomes some limitations of field ,GC. Clay horizons
with <5% air-filled porosity reduce effectiveness of soil gas sampling. Should be com-
pared with other sampling techniques to determine its applicability at a particular site.
USE
LOCATION USED: Puget Sound, WA, 1986.
EPA SITE NUMBER (CERCLIS): Not Available
30
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MATRIX: Soil.
PREPARATION, MAINTENANCE AND CLEANUP: Preconditioning and assembly of Tenax
tubes necessary (solvent extraction with methanol, then hexane; heating in N2 at-
mosphere). Cleanup required for reuse.
ANALYSIS TIME: Drilling borehole- 15-30 minutes; installing sampling probe- 10 min-
utes; sample collection- 45 minutes; analysis- 25 minutes.
CAPITAL COST: Tenax tubes ($50-75); probes ($100); sampling pump ($100-500) Gas
Chromatograph: $4,100 - $20,000
CALIBRATION: Sampling pump requires calibration, using a "dummy" Tenax tube and
Buck Calibrator before and after sample collection.
COMMENTS: Allows long-term and time-averaged sampling. Comparatively easy sample
collection. May not show long-term changes in soil gas concentration unless probe con-
tents mixed to provide equilibrium along probe length before sampling. Provided more
information about widespread, low-level contamination than Direct Injection - Auger
method but no more detailed plume map. Allows more complete desorption than acti-
vated carbon and is easier to clean for reuse. Samples can be refrigerated for later
analysis.
PROTOCOL AVAILABLE: No.
SOURCE
TECHNICAL CONTACT: John Ryding
AFFILIATION: C.C. Johnson & Malhotra
TELEPHONE: (303) 433-6966
PREPARED: May 6, 1987
BIBLIOGRAPHY
Jowise; P.P., Vilinow, J.D., Gorelik, L.I., Ryding, J.M., "Comparative Analysis of Soil Gas
Sampling Techniques, "Management of Uncontrolled Hazardous Waste Sites,
Washington, D.C. December 1-3, 1986, p. 193-199.
31
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METHOD FM-16: SOIL GAS SAMPLING FOR DOWNHOLE PROFILING
SUMMARY: Soil gas samples are collected from borehole through Teflon tubing to deter-
mine vertical contamination gradient. Soil temperature increase due to boring may in-
fluence results. Analysis can be performed using portable GC or field laboratory.
METHOD DESCRIPTION: A Teflon collection hose with attached collection chamber low-
ered into a borehole, and a sample is withdrawn by pumping for analysis. Gas-tight
syringe is used to take sample from a septum fitting on the pump. Grab or composite
samples can be taken.
APPLICATIONS: Used to determine vertical contamination gradient, identify "hot spots,"
predict emission rates, and assess migration pathways as determined by soil type and
stratigraphy.
LIMITATIONS: Uncontrolled variables include soil temperature influenced by heat gener-
ated by the auger and surface area of the soils.
INSTRUMENTATION USED: Custom fabricated downhole Isolation flux chamber, Teflon
line, gas-tight syringe.
PERFORMANCE SPECIFICATION
DETECTION LIMITS: Function of injection volume and detector sensitivity. 0.2 ug/l for
TCE in one study.
SELECTIVITY: Volatile organics.
ACCURACY: Not Known
PRECISION/REPEATABILITY: Not Known
COMMENTS: Sensitivity depends on GC used. Clay layers and horizons with <5% air-
filled porosity reduce effectiveness of soil gas sampling. Precision and ground water cor-
relation must be demonstrated at each site. Compare with other sampling methods to
determine applicability to the site.
USE
LOCATION USED: Not Available
EPA SITE NUMBER (CERCLIS): Not Available
MATRIX: Soil.
PREPARATION, MAINTENANCE, AND CLEANUP: Equipment decontamination required;
purge syringes with nitrogen gas and check for contamination by GC analysis; check soil
probes by drawing air through and analyzing. Teflon may be subject to carry-over from
high liquid or gas-phase concentrations.
ANALYSIS TIME: 40 min/sample.
32
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CAPITAL COST: Syringes ($30-40); sampling pump ($100-500). Both are reusable.
CALIBRATION: N/A
COMMENTS: One of several soil gas sampling methods; each has advantages under
various circumstances.
PROTOCOL AVAILABLE: Yes.
SOURCE
TECHNICAL CONTACT: Andrew Hafferty
AFFILIATION: Ecology and Environment, Inc.
TELEPHONE: (206) 624-9537
PREPARED: May 6, 1967
BIBLIOGRAPHY
Chapman, H., and Clay, P., "Field Investigation Team (FIT) Screening Methods & Mobile
Laboratories Complementary to Contract Laboratory Program (CLP)," TDD-HQ-8507-01,
October 17, 1986 (Draft).
33
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METHOD FM-17: SOIL GAS SAMPLING USING DIRECT INJECTION - AUGER (DIA)
SUMMARY: Rapid sampling technique for soil gas analysis to aid in ground water plume
determination. Repeated sampling not possible once auger is pulled. Analysis can be
performed using a portable GC and/or field laboratory.
METHOD DESCRIPTION: A 12'-17'-foot borehole is drilled using a hollow-stem auger (8"
O.D.). When desired sampling depth is reached, a 500 ml gas-tight, side port syringe is
lowered and filled. Syringe contents are injected directly into a GC.
APPLICATION: Delineation of extent of contamination; rapid soil gas sampling.
LIMITATIONS: No repeated sampling. Lack of control of sampling environment.
INSTRUMENTATION USED: Auger for drilling and 500 ml gas-tight, side port syringe for
sampling; GC for analysis.
PERFORMANCE SPECIFICATION
DETECTION LIMIT: Heat generated by drilling raises sampled concentration of contami-
nants; however, fewer DIA samples found contaminant, possibly indicating less sensitivity
than other soil sampling methods. 0.2 ug/l for TCE in one study, based on capability of
GC used for analysis.
SELECTIVITY: Volatile organics; depends on GC method used.
ACCURACY: Results correlated well with results from other sampling methods at same
locations: Correlation coefficients were 0.68 for one-liter method; 0.72- headspace
method; 0.78- direct injection-stopper; 0.80- Tenax.
PRECISION/REPEATABILITY: Not Known.
COMMENTS: May not accurately reflect ground water conditions due to quick nature of
sampling. GC used will affect detection limits. Clay layers and horizons with <5% air-
filled porosity reduce effectiveness of soil gas sampling. Compare method to other sam-
pling techniques to determine its applicability to a particular site.
USE
LOCATION USED: Puget Sound, WA, 1986.
EPA SITE NUMBER (CERCLIS): Not Available
MATRIX: Soil
PREPARATION, MAINTENANCE AND CLEANUP: Determine appropriate drilling depth by
use of test holes (need to drill below surface soils to bypass competing adsorption sinks)
or by combined experience and assessment of site factors. Decontamination of auger
and syringes required.
ANALYSIS TIME: 15-30 minutes to drill borehole; 1 minute for sample collection.
34
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CAPITAL COSTS: Syringes: ($30-40); GC: $4,100 - $20,000.
CALIBRATION: Purge syringes with nitrogen and check for contamination by injecting
carrier gas samples into GC.
COMMENTS: Sample collection relatively easy. Minimal sample preparation required
before analysis.
PROTOCOL AVAILABLE: Yes.
SOURCE
TECHNICAL CONTACT: John Ryding
AFFILIATION: CC. Johnson & Malhotra
TELEPHONE: (303) 433-6966
PREPARED: May 6, 1967
BIBLIOGRAPHY
Jowise, P.P., Villnow, J.D., Gorelik, L.I., and Ryding, J.M., "Comparative Analysis of Soil
Gas Sampling Techniques," Management of Uncontrolled Hazardous Waste Sites,
Washington, D.C., December 1-3, 1986., p. 193-199.
35
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METHOD FM-18: PCB ANALYSIS USING A GAS CHROMATOGRAPH IN AN ON-SITE
LABORATORY- HEXANE/METHANOL/WATER EXTRACTION
SUMMARY: Rapid determination of major Aroclors to 200 ug/kg in soil. Accurate to
100,000 ug/kg, then underestimates by 60%. Requires field lab. Appropriate extraction
solvent should be determined by laboratory testing prior to field use.
METHOD DESCRIPTION: Requires a field laboratory with a GC and linearized electron
capture detector for PCB analysis of soil samples. Identification is done by comparing
peak retention time with external standards. Quantitation is determined by comparing
peak heights and volumes of the standard and sample. Sample preparation consists of
mixing 0.8 gram of soil with with a 1:4:5 ratio of distilled water/methanol/hexane. An
optional step Is to dry and grind sample before extraction. Agitate sample and let sit,
allowing hexane layer to separate. Transfer hexane layer to a test tube containing sul-
furic acid and mix. This step is optional, as it is used to eliminate matrix interferences.
Withdraw sample from hexane layer for GC analysis.
APPLICATION: Simple and rapid determination of polychlorinated biphenyls. Method
most appropriate for Aroclors 1242, 1248, 1254 and 1260, but good for 1016, 1221, and
1232.
LIMITATIONS: Above 100,000 ug/kg, concentrations are underestimated by 60%. Results
are approximations.
INSTRUMENTATION USED: Analytical instrument Development Corp. (AID) Model 511-06
GC equipped with ECD and a 4-foot SE-30 stainless column.
PERFORMANCE SPECIFICATION
DETECTION LIMIT: 200 ug/kg
SELECTIVITY: Compounds give characteristic multiple peaks, good selectivity.
ACCURACY: Recovery of Aroclor 1242 spike = 80%-105%. Based on results of 300
samples, accuracy Is equivalent to CLP below 100,000 ug/kg; determination above
100,000 ug/kg are biased low (about 40% of the CLP determined value).
PRECISION/REPEATIBILITY: Relative Standard Deviation (RSD) of 4 samples = I0%-
12%.
COMMENTS:
USE
LOCATION USED: Extensively used; sites include Washburn, ME; Norwood, MA.
EPA SITE NUMBER (CERCLIS): Not Available
MATRIX: Soil.
PREPARATION, MAINTENANCE AND CLEANUP: Care should be taken not to contami-
nate column. Before run, column should be at thermal equilibrium.
36
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ANALYSIS TIME: 5-10 samples/hr
CAPITAL COST: $7,245.00
CALIBRATION: Calibration determined by peak heights and retention times of PCB stan-
dards. Standards and blanks should be run every tenth sample.
COMMENTS: This method has been used often in Region I.
PROTOCOL AVAILABLE: Yes.
SOURCE
TECHNICAL CONTACT: Dr. Thomas Spittler
AFFLILIATION: U.S. EPA Region I Laboratory.
TELEPHONE: (617)861-6700
PREPARED: 4/9/67
BIBLIOGRAPHY
Spittler, T. M., "Field Measurement of PCBs in Soil and Sediment Using a Portable Gas
Chromatograph." Proceedings of 4th National Conference on Management of Hazardous
Waste Sites. Washington, DC, October 31-November 2, 1963.
Fowler, B.A. and Bennett, J.T. "Screening For Characterization of PCB-Containing Soils
and Sediment."
37
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METHOD FM-19: PCB Analysis 'Using a Gas Chromatograph in an On-site Laboratory -
Hexane Extraction.
SUMMARY: Rapid determination of major Aroclors to 25 ug/l in water and 2,500 ug/kg in
soil. Requires field laboratory. Appropriate extraction solvent should be determined by
laboratory testing prior to field use.
METHOD DESCRIPTION: Requires field laboratory with GC and linearized ECD for PCB
analysis of water and soil samples. Identification is done by comparing peak retention
times with external standards. Quantitation is determined by comparing peak heights and
volumes of the standard and sample. Sample preparation for water consists of adding
1.5 ml hexane to 15 ml of water, mixing and separating hexane layer. Sample prepara-
tion for soil consists of mixing 2 grams of soil with 2 grams sodium sulfate. Then 10 ml
of hexane is added to sample, mixed with an ultrasonic probe and hexane layer sepa-
rated. The hexane layer is ready for GC analysis.
APPLICATION: Simple and rapid determinations of polychlorinated biphenyls (PCBs).
Also determines pesticides. (Testing based on Aroclor 1260).
LIMITATIONS: Results are semi-quantitative. Has not been used in the field.
INSTRUMENTATION USED: Hewlett-Packard 5880 with ECD.
PERFORMANCE SPECIFICATION
DETECTION LIMITS: 25 ug/l in water and 2,500 ug/kg in soil.
SELECTIVITY: Compounds give characteristic, multiple peaks; good selectivity.
ACCURACY: Not available.
PRECISION/REPEATABILITY: Not available.
COMMENTS: This method was developed by Region IV to provide semiquantitative data.
Until recently, not used as a quantitative method.
USE
LOCATION USED: Field Mobile Laboratory in Florida
EPA SITE NUMBER (CERCLIS): N/A
MATRIX: Soil and Water
PREPARATION, MAINTENANCE AND CLEANUP: Precautions should be taken not to
contaminate column. Occasional cleaning and reconditioning of column and detector
required.
ANALYSIS TIME: 20-25 min/sample
CAPITAL COST: $20,000.00
38
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CALIBRATION: Calibration determined by peak area and retention time of PCB
standard.
COMMENTS: A much less expensive GC/ECD could be used.
PROTOCOL AVAILABLE: Yes.
SOURCE
TECHNICAL CONTACT: William Loy
AFFILIATION: EPA Region IV, ESD.
TELEPHONE: (404) 546-3386
PREPARED: April 15, 1987
BIBLIOGRAPHY
"Screening Method For Extractable Organic Compounds," EPA Region IV, Mobile
Laboratory Protocol, January 1987.
39
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METHOD FM-20: PCB ANALYSIS USING A GAS CHROMATOGRAPH IN AN ON-SITE
LABORATORY- HEXANE/METHANOL
SUMMARY: Rapid determination of major Aroclors to 200 ug/kg in soil and 200 ug/l in
water. Requires field laboratory. Appropriate extraction solvent should be determined by
laboratory testing prior to field use.
METHOD DESCRIPTION: Requires a field laboratory with GC and linearized electron cap-
ture detector for PCB analysis of soil samples. Identification is done by comparing peak
retention times with external standards. Quantitation is determined by comparing peak
heights and volumes of the standard and sample. Sample preparation for water consists
of adding 1 ml hexane to 100 ml of water, mixing sample, and separating hexane layer.
This step Is repeated once. Add 1 ml sulfuric acid to hexane extract and mix. Sample is
ready for GC analysis. Sample preparation for soil consists of mixing 1 to 2 grams soil, 2
ml methanol, and 10 ml hexane. Separate hexane layer, add 1 ml sulfuric acid to ex-
tract, and mix. Hexane extract is ready for GC analysis.
APPLICATION: Simple and rapid determination of polychlorinated biphenyls. Method
most appropriate for Aroclor 1232, 1242, 1248, 1254, 1260.
LIMITATIONS: Results are approximations,
INSTRUMENTATION USED: Analytical Instrument Development Corp. (AID) Model 51 1-06
with ECD and 4-ft SE-30 column; or Shimadzu Mini-2 with ECD and 4-ft OV-1 column.
PERFORMANCE SPECIFICATION
DETECTION LIMIT: 200 ug/l in water
100 ug/kg in soil
SELECTIVITY: Compounds give characteristic multiple peaks, good selectivity.
ACCURACY: Average Percent Recovery = 104% (Range 65%-193%).
PRECISION/REPEATABILITY: Average Relative Standard Deviation = 14%; range 5.0%-
42%.
COMMENTS: The percent recovery decreases as PCB concentration increases.
USE
LOCATION USED: Beaver Creek, Oregon 1985
EPA SITE NUMBER (CERCLIS): Not Available
MATRIX: Soil and Water
PREPARATION, MAINTENANCE AND CLEANUP: Care should be taken not to contami-
nate column. Column should be at thermal equilibrium before running.
ANALYSIS TIME: 5-10 samples/hr
40
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CAPITAL COST: AID-51 1 $7,245.00
Shimadzu
Mini-2
$4520.00
CALIBRATION: Calibration determined by peak heights and retention times of PCB stan-
dards. Standards and blanks should be run every tenth sample.
COMMENTS: Used regularly in Region X.
PROTOCOL AVAILABLE: Yes.
SOURCE
TECHNICAL CONTACT: Hunt Chapman
AFFILIATION: Ecology and Environment, Inc.
TELEPHONE: (703) 522-6065
PREPARED April 9, 1987
BIBLIOGRAPHY
Chapman, H. and Clay, P., "Field Investigation Team (FIT) Screening Methods and
Mobile Laboratories Complementary to Contract Laboratory Program (CLP)," TDD-HQ-
8507-01, October 17, 1986. (Draft),
41
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METHOD FM-21: PCB ANALYSI'S USING A GAS CHROMATOGRAPH IN AN ON-SITE
LABORATORY- HEXANE/ACETONE EXTRACTION
SUMMARY: Rapid determination of major Aroclors down to 2,000 ug/kg in soil. Requires
field laboratory. Method was not tested for all PCBs. Appropriate extraction solvent
should be determined by laboratory testing prior to field use.
METHOD DESCRIPTION: Requires field laboratory with a gas chromatograph (GC) and
linearized electron capture detector (ECD) for PCB analysis of soil samples. Identification
is done by comparing peak retention times with external standards. Quantitation is deter-
mined by comparing the peak heights and volumes of the standard and sample. Sample
preparation consists of mixing 10-15 grams of soil with a UV grade 1:1 hexane/acetone
solution, followed by extraction. Florisil "SepPak" used to adsorb interferences from so-
lution. Extract from SepPak then screened by GC analysis.
APPLICATION: Simple and rapid determination of polychlorinated biphenyls; Aroclor
1232, 1242, 1248, 1254, and 1260.
LIMITATIONS: Method was not tested for all PCBs.
INSTRUMENTATION USED: Hewlett Packard (HP) Model 5840-A Gas Chromatograph
with one glass column; or HP Model 5880-A Gas Chromatograph with one glass column;
with AID 511 or Shimadzu Mini-2 with Electron Capture Detector
PERFORMANCE SPECIFICATION
DETECTION LIMIT: 2,000 ug/kg
SELECTIVITY: Peaks are separate; good selectivity.
ACCURACY: Approximately + 5!! of true value. Mean recovery of soil spike = 97%-98%
(Tested for eleven soil spikes).
PRECISION/REPEATABILITY: One sample run in triplicate gave standard deviation of
0.231. Two duplicate samples differed by 2-18%. Relative standard deviation (RSD) of
soil spike was + 14% (eleven samples).
COMMENTS: Samples below the detection limit can be concentrated and re-run.
USE
LOCATION USED: G.E Moreau, Schenectady N.Y.; Modified at Wide Beach, N.Y
EPA SITE NUMBER (CERCLIS): NYD980528335
MATRIX: Soil
PREPARATION, MAINTENANCE AND CLEANUP: After a week of continuous use,
columns and detectors have to be cleaned and reconditioned, requiring one and a half
days of down time.
42
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ANALYSIS TIME: 30 minutes per sample.
CAPITAL COSTS: $18,000.00
CALIBRATION: Calibration determined by the peak heights and retention times of PCB
standards. Standards and method blanks are run after every tenth sample.
COMMENTS: This method has had very limited use.
PROTOCOL AVAILABLE: No.
SOURCE
TECHNICAL CONTACT: Lisa Gatton Vidulich
AFFILIATION: U.S. EPA Region II Monitoring Management
Branch
TELEPHONE: (201) 321-6676
PREPARED: April 17, 1987
BIBLIOGRAPHY
A Rapid Procedure for the Determination of Polychlorinated Biphenyls in Soils. Draft.
U.S. EPA Region II.
43
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METHOD FM-22: PESTICIDE ANALYSIS USING A GC WITH
ECD- HEXANE/METHANOL EXTRACTION
SUMMARY: Rapid determination of most pesticides to 100 ug/l in water and to 20 ug/kg
In soil. Low recovery of some pesticides. Field laboratory required.
METHOD DESCRIPTION: Requires field laboratory with GC and linearized ECD for pesti-
cide analysis in soil and water. Identification and quantitation is determined by compar-
ing peak retention times and peak areas, respectively, of the standard and sample.
Sample preparation for water consists of adding 1 ml hexane to 100 ml of water, mixing,
and separating hexane layer. This step is repeated once. Sample preparation for soil
consists of mixing 1 to 2 grams of soil, 2 ml methanol and 10 ml hexane, and separating
the hexane layer. 1 ml sulfuric acid is added to the extract and mixed. If pesticide is
sensitive to acidification, this step is omitted. Hexane extract is ready for GC analysis.
APPLICATION: Simple and rapid determination of most pesticides except for endrln
ketone and methoxychlor. Also determines PCBs.
LIMITATIONS: Poor spike recoveries for some pesticides. Method requires testing before
use. Results are semi-quantitative.
INSTRUMENTATION USED: Analytical Instrument Development Corp. (AID) model 511-06
with ECD and 4 ft SE-30 column; or Shimadzu Mini-2 with ECD and 4 ft OV-1 column.
PERFORMANCE SPECIFICATION
DETECTION LIMITS: 100 ug/l in water and 20 ug/kg in soil.
SELECTIVITY: Compounds give separate peaks, good selectivity.
ACCURACY: 3 water matrix spikes of 13 compounds: recovery = 8%-107%.
3 soil matrix spikes of 13 compounds: recovery = 26%-200%.
PRECISION/REPEATABILITY: Relative Standard Deviation (RSD) of 13 compounds in
water, in triplicate, RSD = 1.5%-34.2%; 13 compounds in soil, in triplicate, RSD =
7.6%-54.9%.
COMMENTS: Recoveries are given before and after acidification
USE
LOCATION USED: Beaver Creek, Oregon 1985.
EPA SITE NUMBER (CERCLIS): ORD095016887
MATRIX: Soil and Water
PREPARATION, MAINTENANCE AND CLEANUP: Column should be at thermal equilib-
rium before running. Column and detector require occasional cleaning and
reconditioning.
44
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ANALYSIS TIME: 30-45 min/sample
CAPITAL COST: AID 511 with ECD $7,245.00 Shimadzu Mini-2E with
ECD $4,520.00
CALIBRATION: Calibration determined by peak retention times and areas of PCB stan-
dards. Standards and method blank should be run every tenth sample.
COMMENTS: Used fairly regularly in Region X.
PROTOCOL AVAILABLE: Yes.
SOURCE
TECHNICAL CONTACT: Hunt Chapman
AFFILIATION: Ecology and Environment, Inc.
TELEPHONE: (703) 522-6065
PREPARED: April 15, 1987
BIBLIOGRAPHY
Chapman, M. and Clay, P. "Field Investigation Team (FIT) Screening Methods and
Mobile Laboratories Complementary to Contract Laboratory Program (CLP), " TDD-HQ-
8507-01, October 17, 1986 (Draft).
45
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METHOD FM-23: PESTICIDE ANALYSIS USING ISOTHERMAL GC WITH
ECD- HEXANE EXTRACTION
SUMMARY: Rapid determination of pesticides to 5 ug/l in water and 500 ug/kg in soil.
Requires field lab. Many other compounds detected with pesticides on GC.
METHOD DESCRIPTION: Requires field laboratory with GC and linearized ECD for pesti-
cide analysis in soil and water. Identification and quantitation is determined by compar-
ing peak retention times and peak areas of the standard and sample. Sample
preparation for water consists of mixing 15 ml of water with 1.5 ml hexane and separat-
ing hexane layer. Sample preparation for soil consists of mixing 2 grams soil with 2
grams sodium sulfate. To this, 10 ml hexane is added, mixed with an ultrasonic probe,
and hexane layer separated. The hexane layer is ready for analysis.
APPLICATION: Simple and rapid determination of pesticides. Also detects PCBs.
LIMITATIONS: Results are semi-quantitative. Has not been used in the field. Detects
phosphorus, nitrogen, sulfur, and oxygen compounds along with pesticides.
INTRUMENTATION USED: Hewlett-Packard Model 5880 with ECD.
PERFORMANCE SPECIFICATION
DETECTION LIMIT: 5 ug/l in water and 500 ug/kg in soil.
SELECTIVITY: Compounds give separate peaks, many compounds detected; usually
good selectivity.
ACCURACY: Not available.
PRECISION/REPEATABILITY: Not available.
COMMENTS: This method was developed by Region IV to provide tentative identification
of compounds and semiquantitative data. Until recently not used as a quantitative
method.
USE
LOCATION USED: Field Mobile Laboratory in Florida
EPA SITE NUMBER (CERCLIS): Not Applicable.
MATRIX: Soil and water
PREPARATION, MAINTENANCE AND CLEANUP: Precautions should be taken not to
contaminate column. Occasional cleaning and reconditioning of column and detector
required.
ANALYSIS TIME: 20-25 minisample.
CAPITAL COST: $20,000.00
46
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CALIBRATION: Calibration determined by peak areas and retention times of pesticide
standards.
COMMENTS: A much less expensive GC/ECD could be used.
PROTOCOL AVAILABLE: Yes.
SOURCE:
TECHNICAL CONTACT: William Loy
AFFILIATION: EPA Region IV ESD
TELEPHONE: (404) 546-3386
PREPARED: April 15, 1987
BIBLIOGRAPHY
"Screening Method For Extractable Organic Compounds", EPA Region IV Mobile
Laboratory Protocol, January 1987.
47
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METHOD FM-24: PHENOL DETERMINATION BY LIQUID-LIQUID EXTRACTION AND GC
ANALYSIS
SUMMARY: Detection of phenols in water to 100 ug/l and soil to 25 ug/kg. Requires
field laboratory and chemist.
METHOD DESCRIPTION: Uses liquid-liquid extraction with GC analysis to determine phe-
nols in soil and in water. The procedure for soil analysis entails taking 2-3 grams of soil
and extracting with methanol. The procedure for water analysis consists of taking 20 ml
of water, adjusting the pH to 2, and extracting with methanol. Extract for both soil and
water Is reacted with pentafluorobenzyl bromide and potassium carbonate in presence of
hexacyclooctadecane catalyst to form pentafluorobenzyl (PFB) phenol derivative. PFB de-
rivative is exchanged into hexane using liquid-liquid extraction. An aliquot of hexane solu-
tion is injected Into GC for analysis. Identification and quantitation by comparison of
retention time and peak height and volume to standard (response factor determination
required). Method is a modification of EPA method 604.
APPLICATION: Determination of phenol concentrations in soil and water; 2,4-dimethyl
phenol, phenol, 2-chlorophenol, 2-nitrophenol, 2,4-dichlorophenol, 4-chloro-3-
methylphenol, 2,4,6-trichlorophenol and pentachlorophenol.
LIMITATIONS: Liquid-Liquid extraction procedure is a difficult process and can best be
performed by a trained chemist.
INSTRUMENTATION USED: Shimadzu GC Mini-2 Gas Chromatograph with ECD and
Shimadzu Chromatopac C-RSA Data Processor.
PERFORMANCE SPECIFICATION:
DETECTION LIMITS: Detection limit for pentachlorophenol in water = 100 ug/l and in
soil = 25 ug/kg
SELECTIVITY: Separate peaks, easily identifiable. Other compounds may appear on
chromatograph.
ACCURACY: Spike recoveries In soil (6 replicates of 8 compounds) = 102%-127%.
Spike recoveries in water (6 replicates of 8 compounds) = I.O%-88%.
PRECISION/REPEATABILITY: Relative Standard Deviation (RSD) for 6 replicates of 8
compounds in soil = 15.3%-44.4%. RSD for 6 replicates of 8 compounds in water =
19.6% to 56.2%.
COMMENTS: Recoveries for water samples were acceptable for pentachlorophenol (88%,
CLP limits = 9-103%) and phenol (25.8%, CLP limits = 12-89%).
USE
LOCATION USED: Not Available
EPA SITE NUMBER (CERCLIS): Not Applicable
48
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MATRIX: Water and Soil
PREPARATION, MAINTENANCE AND CLEANUP: Column cleaning and reconditioning re-
quired occasionally. Column can be saturated easily by concentrated samples.
ANALYSIS TIME: 20-40 min/sample, depending on column length
CAPITAL COST: $4520 Shimadzu GC with ECD
CALIBRATION: Standards necessary to identify and quantify compounds. Calibration Is
done using mixed standard solutions of known concentrations. A minimum of three stan-
dard solutions should be used for calibration.
COMMENTS: Interpretation of results requires a trained chemist. Used occasionally in
Region X.
PROTOCOL AVAILABLE: Yes
SOURCE
TECHNICAL CONTACT: John Ryding
AFFILIATION: C.C. Johnson & Malhotra
TELEPHONE: (303) 433-6966
PREPARED: April 22, 1987
BIBLIOGRAPHY
McGinnis, Roger, "Screening Method for Acid Extractables (Phenols) in Soil and Water,"
EPA Document No. TDD-R1O-8601 -04, September, 1986.
49
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METHOD FM-25: PAH ANALYSIS USING GC (FID) WITH HEATED COLUMN
SUMMARY: Detects PAHs in water and in soil to ppm range. GC may give overlapping
peaks, hindering identification. Has trouble determining naphthalene.
METHOD DESCRIPTION: Requires a field laboratory with a gas chromatograph able to
heat column above ambient temperatures for polycyclic aromatic hydrocarbon (PAH) de-
termination. Identification and quantitation is done by comparing peak retention times
and peak areas between standards and samples. Procedure for water analysis consists
of extracting contaminants from 100 ml water sample into 1 ml methylene chloride by
vortex mixing. Procedure for soil analysis consists of mixing 2-3 grams of soil with 6 ml
methylene chloride and separating methylene chloride. Extraction step for soil and water
is repeated, and extracts are combined. The methylene chloride is passed through a
silica gel column to remove potential interferences before GC analysis. Method is a
modification of EPA method 610.
APPLICATION: Rapid identification and quantitation of polycyclic aromatic hydrocarbons.
LIMITATIONS: Possible co-eluting peaks (e.g., phenanthrene and anthracene). Method
gives poor spike recovery for naphthalene. Does not detect many semi-volatlles.
INSTRUMENTATION USED: Shimadzu Mini-2F or Shimadzu Mini-3 GC (FID) with 6 foot
glass quantitation and confirmation column
PERFORMANCE SPECIFICATION
DETECTION LIMITS: 500-1000 ug/l in water and 50-500 ug/kg in soil for PAHs.
SELECTIVITY: Peaks usually separate and give good selectivity. Occasional co-eluting
peaks.
ACCURACY: Spike recovery for 12 different compounds in soil: 67%-129% (naphthalene
excluded, 14% recovery).
PRECISION/REPEATABILITY: Relative Standard Deviation (RSD) for 12 different com-
pounds in soil: 7.8%-55.7%.
COMMENTS: None
USE
LOCATION USED: J.H. Baxter, Washington, 1986
EPA SITE NUMBER (CERCLIS): WAD009265521
WAD053823019
MATRIX: Soil and Water
PREPARATION, MAINTENANCE AND CLEANUP: Columns and detectors require occa-
sional cleaning and reconditioning.
ANALYSIS TIME: 60 min/sample
50
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CAPITAL COST: Shimadzu Mini-2F- $4,100.00; Mini-3- $5,200.00
CALIBRATION: Retention times and peak areas of standards must be obtained for the
compounds of interest. Standards are used to generate a three-point calibration curve.
COMMENTS: Used fairly regularly in Region X.
PROTOCOL AVAILABLE: Yes.
SOURCE
TECHNICAL CONTACT: Hunt Chapman
AFFILIATION: Ecology and Environment, Inc.
TELEPHONE: (703) 522-6065
PREPARED: April 14, 1987
BIBLIOGRAPHY
Chapman, H. and Clay, P., "Field Investigation Team (FIT) Screening Methods and
Mobile Laboratories Complementary to Contract Laboratory Program (CLP)," EPA
Document Number TDD-HQ-8507-01, October 17, 1986. (Draft).
51
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METHOD FM-26: Total PNA Analysis using an Ultraviolet Fluorescence
Spectrophotometer
SUMMARY: Rapid, semi-quantitative determination of total polynuclear aromatics (PNAs)
in soil and water to 10.0 ug/l in water and 1,000 ug/kg in soil; field laboratory required.
METHOD DESCRIPTION: Requires a field laboratory with UV fluorescence spectropho-
tometer. The compounds' concentrations will determine the amount of a particular
wavelength of light absorbed. Method consists of measuring a set amount of soil or
water, a one-step extraction followed by UV fluorescence spectrophotometric analysis.
Analysis occurs at ambient temperature; constant temperature preferable. Sodium sulfate
is added to soil samples and is used as an absorbent for water extract samples to clean
up the sample. Acetonitrile is used for soil extraction and hexane for water extraction.
Quantitation is done by a seven-point calibration curve.
APPLICATION: Simple and rapid determination of total PNAs.
LIMITATIONS: Does not identify individual PNA compounds. Must be validated for each
site due to potential matrix interferences.
INSTRUMENTATION USED: Perkin-Elmer Model LS-5 Fluorescence spectrometer with
chart recorder.
PERFORMANCE SPECIFICATION
DETECTION LIMIT: 10.0 ug/l in water, 1,000 ug/kg in soil.
SELECTIVITY: Dependent upon matrix interference. Where used, only PNAs were
detected.
ACCURACY: Spike recoveries for napthalene/acenapthene for soil (10 samples) and
water (6 samples) were 63%-100% and 81%-101% respectively. Spike recoveries for
phenanthrene for soil (10 samples) and water (6 samples) were 66%-130% and 93%-
111 %, respectively.
PRECISION/REPEATABILITY: Relative Standard Deviation (RSD) for phenanthrene for
water (6 samples) and soil (10 samples) were 0.6%-11% and 0.6%-13%, respectively.
RSD for napthalene/acenaphthene for water (6 samples) and soil (10 samples) were
1.2%-10% and 0%-l 2.7%, respectively.
COMMENTS: Specifications shown based on data from two sites. Calibration curves ex-
trapolated to non-linear response regions will give high concentrations (> 100% recover-
ies of spikes). Results were within an order of magnitude of GC/MS results, which is
considered acceptable for screening.
52
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USE
LOCATION USED: Southern Maryland Wood Treating Plant. Summer 1986.
EPA SITE NUMBER (CERCLIS): MDD980704852
MATRIX: Soil and water.
PREPARATION, MAINTENANCE AND CLEANUP: UV Fluorescence cells should be
cleaned occasionally.
ANALYSIS TIME: 20-30 samples/day
CAPITAL COST: $16,300.00
CALIBRATION: Standards were made of seven commonly occurring PNAs. Calibration
curve was from 0.01 g/l to 0.1 g/l and 0.1 g/l to 1.0 g/l, with four points for each curve.
COMMENTS: Can be operated by trained technician.
PROTOCOL AVAILABLE: No.
SOURCE
TECHNICAL CONTACT: Stacie Popp
AFFILIATION: Roy F. Weston, Inc.
TELEPHONE: (215)692-3030
PREPARED: April 10, 1987
BIBLIOGRAPHY
Motwani, J.N., Popp, S.A., Johnson, G.M. and Mindock, R.A., "Field Screening
Techniques Developed Under the Superfund Program," Management of Uncontrolled
Hazardous Waste Sites, Washington, D.C., December 1-3, 1986.
53
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METHOD FM-DI: TRACE ATMOSPHERIC GAS ANALYZER (TAGA)
(METHOD UNDER DEVELOPMENT)
SUMMARY: Quick characterization and monitoring of many organic compounds, using
MS/MS. Capable of analyzing direct air samples for most organics at the ppb level, and
performing rapid GS/MS/MS analyses of soils. Capable of real-time screening of ambient
air for target compounds (1/2 order of magnitude accuracy), but the quantitative data
reduction (increase of accuracy) to include the calculation of error bars requires addition
time. Some interferences possible with hydrocarbons and chlorinated solvents; lacks
isomer specificity; requires frequent recallbration; standard QA/QC procedures not
compatible. Analyses are performed in specially build mobile laboratory.
METHOD DESCRIPTION: Triple quadrupole MS/MS analyzes polar and non-polar com-
pounds in ambient air using direct sampling. The MS/MS uses the ambient air as its
chemical ionization reagent gas. Chemical ionization of target compounds achieved by
charge transfer, hydride abstraction, halide abstraction, hydride-halide abstraction, proto-
nation, and/or adduct formation. Ionization is determined by the compound class being
analyzed and the instrument source being used. In tandem mode, preselected ions are
fragmented and analysed to produce characteristic mass spectra; specific fragment ions
can be sought. In single mass analyzer mode, scans all ions produced. For air analyses,
chromatographic separation is not compatible with the existing software. Some type of
parallel GC sampling is recommended for compound confirmation. Ion signals obtained
in the tandem mode can be used to directly calculate air concentration.
APPLICATION: For air and soil gas samples - instant (real-time) screening and monitor-
ing of concentration changes over time (e.g., plume tracking and characterization) for
polar and nonpolar compounds including amines, nitrogen and sulfur containing hete-
rocyclic compounds, oxygenated hydrocarbons, halogenated hydrocarbons, aromatics,
C5 and larger hydrocarbons, and sulfur containing hydrocarbons. Also capable of quanti-
tation but more analytical control and data-reduction time needed. For soil analyses -
capable of "dilute and shoot" GC/MS/MS analyses for any GC compatible compound
present in mg/kg concentrations (e.g., PCBs and chlorinated pesticides) and "rapid
cleanup and shoot" GC/MS/MS analyzes for any compound present in ug/kg concentra-
tions (e.g., TCDD).
LIMITATIONS: Lacks isomer specificity for air analyses. Hydrocarbons and chlorinated
solvents can yield ions of equal mass and similar structures, resulting in cross interfer-
ences. Dirty samples can yield spectra with fragments from more than one parent struc-
ture. Not as stable as normal GC/MS (2- to 3-fold drift in sensitivity over a day is
possible). The sampling system is not totally compatible with classical QA/QC procedures
(direct sampling of audit cyclinders and replicate analyses) but TAGA specific QA/QC
procedures are currently being developed and refined by the ERT and NYDEC.
Difference in ionization and the use of an initial mass filtering will result in MS/MS
spectra being different than the MS spectra contained in standard EPA/NIH standard
spectral libraries.
The use of the sample matrix as the chemical ionization reagent gas can result in poten-
tial matrix affects. The current instrument software does not support QA/QC criteria
being applied to quantitative results obtained during air analyses. Quantitative software
utilizing QA/QC criteria is currently being developed by the ERT and by NYDEC. Similar
54
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software development is also being proposed by Battelle and by Sciex, the instrument
manufacturer. For all analyses - because of its cryogenic vacuum pump the instrument
can only be used for a maximum of sixteen hours a day. However, typical analysis days
rarely exceed fourteen hours.
INSTRUMENTATION USED: TAGA 6000E Triple Quadrupole Mass Spectrometer/Mass
Spectrometer; three quadrupoles are RF-coupled: sources in use are Atmospheric
Pressure Chemical lonization (APCI) and Low Pressure Chemical lonization (LPCI).
PERFORMANCE SPECIFICATION
DETECTION LIMIT: 1-10 ug/l for most non-polar organics in air; 0.02-1.7 ug/kg for
dioxins in soil (0.02 ug/kg for 2,3,7,8-TCDD); 25 ug/l for phenols and other such polar
compounds in air; 1 mg/kg for PCB and chlorinated pesticides In soil (without cleanup).
SELECTIVITY: Compounds may be identified by comparing spectral peaks; but lacks
isomer specificity in air analyses. Also, during air analyses certain non-isomeric com-
pounds will form isomers upon ionization (e.g., isopropanol and acetone, 1,2-
dichloroethane and vinyl chloride, and methylene chloride and chloroform).
ACCURACY: Variation of less than 20% between spiked PCB and TCDD samples in
different soil types.
PRECISION/REPEATABILITY: Standard deviation of 0.68 with a mean of 5.5 ug/l dioxin
(repeated analyses of well homogenized soil). Relative standard deviation of 22% for
nine spiked soil samples for PCBs.
COMMENTS: Flash chromatography can be used as a gross cleanup step before MS/MS
when interferences are likely, e.g., isobaric compounds with overlapping collision-induced
dissociation spectra or compounds that react preferentially with the reagent gas.
Accurate quantification difficult In air samples if >IO,000 ug/l methane is present.
Because of the possibilities of self-chemical ionization and source chemistry saturation,
quantitation in the mg/l range is suspect. The quantitation of many compounds in air is
very sensitive to changes in the absolute humidity of the air sampled, especially with the
APCI source. Quantitation of polar compounds by the APCI source is very sensitive to
the presence of ammonia and mg/l levels of amines. LPCI is required source for most
environmental sampling.
USE
LOCATION USED: Oceanside, NJ; Utica, NY; and numerous other sites.
EPA SITE NUMBER (CERCLIS): Not Available
MATRIX: Air, (ambient and indoor) soil, water, soil gas and incinerator wastes.
PREPARATION, MAINTENANCE AND CLEANUP: Soil sample preparation for dioxin
analysis typically consists of a single-step extraction, a rapid dual mini-column cleanup (8
samples every 3-4 hours), and flash gas chromatography (temperture program at 25 C
/min.). Soil preparation for PCBs and chlorinated pesticides at mg/kg concentrations
55
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consists of single-step extraction, extract dilution, and flash chromatography ("dilute and
shoot"). Water analyses consist of extraction and flash chromatography of the extract.
Air analyses typically consist of sampling the air directly from a 1.5-2 liter/second sample
stream.
ANALYSIS TIME: Dioxin- 15-20 minutes for non-isomer specific analyses; 30-45 minutes
for TCDD; complete screening of chemical classes in air- 30 minutes; complete set of
air analyses for a set of target compounds- 1-10 seconds depending on the number of
compounds.
CAPITAL COSTS: $500,000 for MS/MS; $800,000 in fully outfitted van.
CALIBRATION: For GC/MS/MS analyses- uses conventional GC calibration methods.
For air analyses two different calibration techniques are used: 1) A motorized syringe
drive expels headspace vapor from syringe containing solid or liquid. Vapor from syringe
is mixed with air at 2 liters/minute in the temperature-controlled (1OOoC) mixing tee.
Relative concentration in the stream is calculated based on vapor pressure and flow
rates. Overall calibration accuracy is + 30%. 2) Certified gas standard cylinders (25 - 50
ppm(v)) can also be serially diluted directly into the sampled air stream to generate cali-
bration concentrations in the range of 5 - 100 ppb(v). This method has an overall calibra-
tion accuracy of + 10% but is limited only for compounds which can be maintained at
stable concentrations in gas cylinders.
For air analyses the instrument should be calibrated for each target compound at least
twice daily. In addition, for many target compounds (e.g., tetrachloroethyiene, chlorinated
aromatics, and oxygenated solvents) the calibrations should be periodically checked
throughout the day.
COMMENTS: Requires high level of expertise and experience on the part of the analyst.
Calibration is simple, and method is relatively fast, cost-effective, and applicable to many
compounds. Calibration accuracy depends on accuracy of literature value of vapor
pressure vs. temperature and on setting of flow rates. Use of ambient air as reagent gas
means that as air changes, calibrations change.
PROTOCOL AVAILABLE: Available upon request for TCDD. Air protocols currently under
revision to incorporate ERT developed software and ERT/NYDEC developed QA/QC
procedures. Onsite consultation available from ERT.
SOURCE
TECHNCIAL CONTACT: Tom Pritchett/Dr. S.H. MO
AFFILIATION: EPA ERT/NYDEC
TELEPHONE: (201) 321 -67387(518)457-7454
PREPARED: April 29, 1987
BIBLIOGRAPHY
Engels, J.W., Kerfoot, H.B., and Arnold, D.F., Survey of Mobile Laboratory Capabilities
and Configurations, EPA 600/X-84-170, U.S. Environmental Protection Agency, July 1984.
56
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Ben-Hur, D., Smith, J.S., and Urban, M.J., Application of Mobile MS/MS to Hazardous
Waste Site Investigation, 5th National Conference on Management of Uncontrolled
Hazardous Waste Sites, November 7-9, 1984.
Becker, D.L, Carter, M.L. Equipment Available for Sample Screening and On-Site
Measurements, Appendices TDD# HQ-8311-04, EPA Contract 68-01-6699, NUS
Corporation, May 30, 1984 (includes EPA report and company literature).
57
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METHOD FM-D2: USE OF BONDED SORBENTS FOR PESTICIDE ANALYSIS
(METHOD UNDER DEVELOPMENT)
SUMMARY: Method is faster than traditional liquid-liquid extraction. Determines pesticide
concentration in water to I ug/l. Requires field laboratory and trained chemist.
METHOD DESCRIPTION: Uses bonded phase extraction column with GC and ECD to
determine pesticide concentrations in water. The procedure involves passing 100 ml of
filtered ground water through a cyclohexyl-bonded phase extraction column with 1 ml
ethylacetate as the elution solvent. The extract injected into GC for analysis.
Identification and quantitation are performed by comparing peak heights and areas to
standards.
APPLICATION: Determination of pesticide concentrations in water.
LIMITATIONS: Possible interferences from other electron capturing species.
INSTRUMENTATION USED: Varian Model 3700 GC equipped with a nickel electron cap-
ture detector and a glass capillary column.
PERFORMANCE SPECIFICATION
DETECTION LIMITS: 1 ug/l for most pesticides
SELECTIVITY: Separate peaks, compounds usually easily identified. Occasional interfer-
ences from other electron capturing species.
ACCURACY: Spike recoveries for 5 replicates of 9 compounds = 79%-105%
PRECISION/REPEATABILITY: Coefficient of variation for 5 replicates = H7,
COMMENTS: Performance data are available for recovery as a function of solvent,
column, flow rate and type of water.
USE
LOCATION USE: Not Available
EPA SITE NUMBER (CERCLIS): Not Applicable
MATRIX: Water
PREPARATION, MAINTENANCE AND CLEANUP: Columns are disposable. Columns are
conditioned prior to use with methanol followed by water or buffer. After the sample has
been added, interferences are washed off the column with distilled 'water, and the
sample eluted by a solvent.
ANALYSIS TIME: Sample preparation = 10-15 min; analysis = 20-30 minutes.
CAPITAL COST: $4,000.00 - $20,000.00 for GC
CALIBRATION: Standards were made of high purity solvents with various concentrations
of seven pesticides. This is used to spike water samples. The spikes were used for
identification and quantitation.
58
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COMMENTS: Interpretation of results requires a trained chemist. Columns must not be
allowed to dry out prior to adding sample.
PROTOCOL AVAILABLE: No
SOURCE
TECHNICAL CONTACT: Patricia Gardner
AFFILIATION: Analytlchem International
TELEPHONE: l-(800) 42 1-2825
PREPARED: April 22, 1987
BIBLIOGRAPHY
Andrews, J.S. and Good, T. J., "Trace Enrichment of Pesticides Using Bonded-Phase
Sorbents," American Laboratory, April 1982.
59
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METHOD FM-D3: USE OF BONDED SORBENTS FOR SEMI-VOLATILE ANALYSIS
(METHOD UNDER DEVELOPMENT)
SUMMARY: Method is faster than traditional liquid-liquid extraction. Determines most
PAHs and phenols in water to 20 ug/l. Poor recovery of phenol (<27%). Analysis can be
performed in a field laboratory.
METHOD DESCRIPTION: Uses bonded phase extraction column with GC/MS analysis to
determine polycyclic aromatic hydrocarbons (PAHs) and phenols concentrations in water.
The procedure involves passing 50-100 ml of filtered ground water through a cyclohexyl-
bonded phase extraction column with a solvent, methanol or acetonitrile and methylene
chloride, and injecting an aliquot directly into GC for analysis. Response factors were
developed using standard mixtures and used to convert mass spectra to quantities
based on area of internal standard base peak.
APPLICATION: Determination of concentrations of many phenols and PAHs plus ben-
zothrophene, dibenzofuran, and some nitrogen heterocycles.
LIMITATIONS: Possible interferences from other electron capturing species. Does not
detect some phenols and nitrogen heterocycles (e.g., phenol and 2,4-dimethyipyridine).
INSTRUMENTATION USED: Finnigan OWA 1020 computerized capillary gas
chromatograph/quadrupole mass spectrometry system (GC/MS) with 30-m fused silica
column.
PERFORMANCE SPECIFICATION
DETECTION LIMITS: Less than 20 ug/l for most phenols and PAHs.
SELECTIVITY: Separate peaks, easily identifiable
ACCURACY: Spike recovery for phenolic compounds (except phenol) = 80%-105%.
Spike recovery for PAHs and other neutral compounds = 51%-111 %, for nitrogen hete-
rocycles = 3%-197%, for phenol = 0%-27%.
PRECISION/REPEATABILITY: Standard Deviation (SD) of five replicates: Phenols (except
phenol) SD = 5.2%-25.8%. PAHs and neutral compounds; SD = 2.3%-15.8%. Nitrogen
heterocycles; SD = 4.4%-32.2%.
COMMENTS: Performance data given for method using acetonitrile and methyl chloride
solvent.
USE
LOCATION USED: Not Available
EPA SITE NUMBER (CERCLIS): Not Applicable
MATRIX: Water
PREPARATION, MAINTENANCE AND CLEANUP: Columns are not reusable and must be
discarded.
80
-------
ANALYSIS TIME: Sample preparation = 10-15 min, analysis = 20-30 min/sample
CAPITAL COST: $85,000 - $100,000 for GC/MS; $1 - extraction column
CALIBRATION: Standards are made of high purity solvents with 0.0001 ug/l of various
contaminants added. These standards are used to spike water samples to obtain various
concentrations. The spikes are used for identification and quantitation.
COMMENTS: Interpretation of results requires a trained chemist. Capital cost varies de-
pending on the GC/MS purchased. HPLC analysis is alternative to GC/MS.
PROTOCOL AVAILABLE: No
SOURCE
TECHNICAL CONTACT: Patricia Gardner
AFFILIATION: Analytichem International
TELEPHONE: l-(800) 421-2825
PREPARED: April 21, 1987
BIBLIOGRAPHY
Rostad, C.E., Pereiru, W.E., and Rutcliff, SM., "Bonded-Phase Extraction Column
Isolation of Organic Compounds in Ground Water at a Hazardous Waste Site," Analytical
Chemistry, Vol. 58, No. 14, p. 2856-2860. December 1984.
Chladek, E and Marano, R.S. "Use of Bonded Phase Silica Sorbents for the Sampling of
Priority Pollutants in Wastewaters," Journal of Chromatographic Science, Vol. 22, p. 313-
320. August 1984.
61
-------
METHOD FM-D4: I MM UNO ASSAYS FOR TRACE ORGANIC ANALYSIS
(METHOD UNDER DEVELOPMENT)
SUMMARY: Alternative (inexpensive and simple) analytical technique incorporating mono-
clonal antibodies for the quantitative measurement of organic chemicals in ground water
& other media. Method for individual chemicals in varying stages of development;
development nearly complete for pentachlorophenol. Preliminary data indicates sensitivi-
ties equal to GS or HPLC methods.
METHOD DESCRIPTION: Developmental stage technique which is a competitive inhibition
enzyme immunoassay (EIA) that incorporates monoclonal antibodies produced via ceil
fusion (hybridoma) technology. The EIA steps include the addition of reagents (e.g., anti-
bodies) and samples/standards to a microtiter plate, a 3-hour incubation, and spectra-
photometric analysis of microtiter plate. A colorimetric reaction indicates the
concentration of target compound by reference to a standard curve.
APPLICATION: inexpensive, rapid and high volume anlysis of organic compounds in
aqueous media. Solid phase or oily samples must be extracted into polar solvents prior
to introduction into the assay. Antibodies can distinguish stereoisomers.
LIMITATIONS: Limited field studies to date. Antibodies methods cannot detect organic
compounds of molecular weight less than 100 atomic units.
INSTRUMENTATION USED: Automated spectrophotometer (microtiter plate reader) IBM
compatible personal computer, printer and software package.
PERFORMANCE SPECIFICATION
DETECTION LIMIT: 25 ug/l for pentachlorophenol without sample concentration; depends
upon binding strength of antibody for target compound and is compound specific.
SELECTIVITY: Each assay is highly selective for a single compound with minor or no
cross-reactivity. Antiboides can also be developed which exhibit broad cross-reactivity
with compounds of similar structure.
ACCURACY: Not available
PRECISION/REPEATABILITY: Not available; preliminary results show + 10-20%
variability between samples.
COMMENTS: Each sample must be tested in triplicate to provide statistically valid
results. Performance data is being compiled in conjunction with US EPA-EMSL Las
Vegas.
USE
LOCATION USED: Mobile laboratory and laboratory setting.
EPA SITE NUMBER (CERCLIS): N/A
MATRIX: Water, soil
62
-------
PREPARATION, MAINTENANCE AND CLEANUP: Antibodies recognize and bind to spe-
cific chemical structures, so sample cleanup & purification may not be critical in many
cases. Sample preparation for soil samples requires extraction (or solvent exchange) into
a polar solvent prior to introduction into the immunoassay. Aqueous samples can usually
be analyzed directly or concentrated using reverse phase adsorbtion columns.
ANALYSIS TIME: 4 hours per plate (up to 24 samples per plate); several plates may be
run concurrently.
CAPITAL COSTS: $22,000 for complete system, including spectrophotometer, computer
(can purchase without), software, printer, plate washer, micropipetters.
CALIBRATION: Prepare a standard curve & controls along with samples. The standard
curve is developed using known concentrations of the target compound & occupies 18
wells on the plate.
COMMENTS: Immunoassays are simple to perform; Highly trained operators not needed.
Methods under development for dioxin, (2,3,7,8-TCDD) pesticides, PCBs, benzene,
phenol,etc. Studies to compare method to other methods will be performed.
PROTOCOL AVAILABLE: Yes
SOURCE
TECHNICAL CONTACT: Joseph Paladino, Product Manager
AFFILIATION: Westinghouse Bio-Analytic Systems Company
TELEPHONE: (412)722-5602
PREPARED: May 19, 1987
BIBLIOGRAPHY: Technical Product Description (Corporate
Literature), personal conversation
63
-------
METHOD FM-D5 USE OF FIBER OPTIC SENSORS IN ENVIRONMENTAL MONITORING
(METHOD UNDER DEVELOPMENT)
SUMMARY: In situ monitoring technique for various contaminants to ug/l concentrations
in ground water, air, & soil. Few fully developed applications, but appears to offer signifi-
cant advantages over conventional sampling techniques.
METHOD DESCRIPTION: Optical fibers are used either as a "light tube" in remote fiber
spectroscopy mode (RFS) or as a "sensor" in fiber optical chemical sensing mode. RFS
provides light transmission over large distances with low light loss; transmission depends
on the core having a higher index of refraction than the cladding. Configurations include
use of laser-induced fluorescence, absorption spectroscopy, raman spectroscopy, & mul-
tivariate spectral analysis. A fiber optical chemical sensor (FOCS) unit includes a
chemical-specific sensor & can operate in at least three modes: fluorescence, absorption
& refraction. A FOCS can respond to a class of compounds or a single species.
APPLICATION: In situ, real-time monitoring of environmental contamination. Particularly
suited for inaccessible or hazardous situations (e.g., ground water, spill cleanup
monitoring).
LIMITATIONS: A different FOCS is needed for each pollutant to be monitored, increasing
development costs (but many can be bundled In a
-------
USE
LOCATION USED: Henderson, NV
EPA SITE NUMBER (CERCLIS): Non-CERCLA
MATRIX: Water, air, soil
PREPARATION, MAINTENANCE AND CLEANUP: Reuse of FOCS requires cleanup (e.g.,
for organic chloride FOCS, bleach the fluorescent reaction product by raising the source
power).
ANALYSIS TIME: NA
CAPITAL COSTS: RFS: Low developmental cost but high operational and equipment
cost. FOCS: Individual FOCS elements should cost less than $25. Instruments would
cost from $500 to $10,000 depending on configuration (e.g., spectrometer or refractome-
ter, single or multi-channel, etc.).
CALIBRATION: FCCS: Experiments are run with each type of FOCS to produce a cali-
bration curve using precalibrated solutions.
COMMENTS: Limited field experience with most FRS and FOCS applications. Research
& commercialization effort underway by several agencies and companies.
PROTOCOL AVAILABLE: No
SOURCE
TECHNICAL CONTACT: Steve Simon
AFFILIATION: Lockheed Engineering and
Management Services Co, Inc.
TELEPHONE: (702) 734-3285
PREPARED: May 18, 1987
BIBLIOGRAPHY
Eccles, L.A., Simon, S.J., and Klainer, S.M., In Situ Monitoring at Superfund Sites with
Fiber Optics, U.S. EPA, Environmental Monitoring Systems Laboratory, Las Vegas, NV,
EPA/600/X-87/156, June 1987.
Milanovick, F.P., Klainer, S.M., and Eccles, L.A., "Remote Detection of Organochlorlides
with a Fiberoptic Based Sensor." Analytical Instrum., 1986, 15 [2], 137.
Milanovick, F.P., Klainer, S.M., and Eccles, L.A., "Remote Detection of Organochlorides
with a Fiber Optic Based Sensor II. A Dedicated Portable Fluorimeter." Analytical
Instrum., 1986.
65
-------
-------
APPENDIX B
HISTORICAL PRECISION AND ACCURACY
DATA CLASSIFIED BY MEDIA
BY ANALYTICAL LEVEL
-------
HISTORICAL PRECISION AND ACCURACY TABLES
Introduction
Table B-l WaterLevel III ( Other than CLP RAS)
Table B-2 WaterLevel III (SW-846)
Table B-3 Water: Level IV
Table B-4 Soillevel I
Table B-5 Soillevel II
Table B-6 Soillevel III
Table B-7 Soillevel IV
Table B-8 Air: Level I
Table B-9 Air: Level II
Table B-10 Air: Level III
Table B-11 Other Media: Level III
-------
INTRODUCTION
The data in this Appendix have been compiled to assist the reader in selecting an ana-
lytical method appropriate for each data use. The methods are classified by media and
by analytical levels defined as follows:
Level I - field screening or analysis using portable instruments. Results are
often not compound specific and not quantitative but results are available in
real-time.
Level II - field analysis using more sophisticated portable analytical instru-
ments; in some cases, the instruments may be set up in a mobile or onsite
laboratory. There is a wide range in the quality of data that can be gener-
ated. Quality depends on the use of suitable calibration standards, reference
materials, and sample preparation equipment: and the training of the opera-
tor. Results are available in real-time or several hours.
Level III - all analyses performed in an offsite analytical laboratory using
standard, documented procedures. The laboratory may or may not be a CLP
laboratory.
Level IV - CLP routine analytical services (RAS). All analyses are performed
in an offsite CLP analytical laboratory following CLP protocols.
Precision and accuracy data are presented in tabular fashion. Footnotes to each table
cite the sources of the data and the concentration or concentration range at which the
precision and accuracy were determined. When no concentration is cited no concentra-
tion information was available in the source material.
Precision is a measure of the variability in repeated measurements of the same sample
compared to the average value. Precision is reported as % Relative Standard Deviation
(RSD). The lower the % RSD, the more precise the data.
-------
TABLE B-l. HISTORICAL PRECISION AND ACCURACY DATA/WATER"
LEVEL III ANALYTICAL TECHNIQUES - METHODS OTHER THAN CLP RAS METHODS
ANALYTES
Benzene
Bromodichloronae thane
Bromofonn
METHOD
(TECHNIQUE)
624
(GC/MS)
8240
(GC/MS)
624
(GC/MS)
501.1
(PURGE & TRAP GC/MS)
501.2
(EXTRACTION GC/MS)
624
(GC/MS)
501.1
(PURGE & TRAP GC/MS)
501.2
(EXTRACTION GC/MS)
CONCENTRATION
RANGE
11 ug/1
480 ug/1
5-100 ug/1
8 ug/1
480 ug/1
0.9 ug/1
550 ug/1
1.8 ug/1
170 ug/1
9 ug/1
400 ug/1
4.8 ug/1
550 ug/1
6 ug/1
170 ug/1
PRECISION
% RSD
16
21
21
28
18
66
34
61
23
32
30
44
41
14
15
ACCURACY
% BIAS
0
-16
12
-8.8
-6.7
0
-3.8
33
-19
-23
10
-27
7.5
-23
1.8
-------
TABLE B-l. HISTORICAL PRECISION AND ACCURACY DATA/WATER3
(continued)
LEVEL III ANALYTICAL TECHNIQUES- METHODS OTHER THAN CLP RAS METHODS
ANALYTES
Chloroform
Dibromochloromethane
Dioxin
METHOD
(TECHNIQUE)
624
(GC/MS)
501.1
(PURGE & TRAP GC/MS)
501.2
(EXTRACTION GC/MS)
624
(GC/MS)
501.1
(PURGE & TRAP GC/MS)
501.2
(EXTRACTION GC/MS)
613
(GC/MS)
CONCENTRATION
RANGE
4.5 ug/1
300 ug/1
0.9 ug/1
550 ug/1
1.8 ug/1
170 ug/1
8.1 ug/1
360 ug/1
0.8 ug/1
550 ug/1
1.8 ug/1
170 ug/1
21 ng/1
202 ng/1
PRECISION
% RSD
31
14
64
14
68
26
13
19
35
36
37
13
25
21
ACCURACY
% BIAS
2.2
-0.6
44
-0.02
-39
-1.2
-3.1
10
-12.5
4.7
0
0.02
N.A.
N.A.
-------
TABLE B-l. HISTORICAL PRECISION AND ACCURACY DATA/WATER*
(continued)
LEVEL III ANALYTICAL TECHNIQUES - METHODS OTHER THAN CLP RAS METHODS
ANALYTES
Methylene Chloride
Toluene
Trichloroethene
Lead
METHOD
(TECHNIQUE)
624
(GC/MS)
624
(GC/MS)
8240
(GC/MS)
624
(GC/MS)
8240
(GC/MS)
200.7
(ICP)
239.1
(FLAME AA)
239.2
(FURNACE AA)
CONCENTRATION
RANGE
7.2 ug/1
480 ug/1
13.5 ug/1
600 ug/1
25 ug/1
75 ug/1
5.4 ug/1
360 ug/1
25 ug/1
75 ug/1
42 ug/1
47.7 ug/1
12 ug/1
105 ug/1
10 ug/1
234 ug/1
PRECISION
% RSD
78
52
19
31
19
48
39
24
34
5
5.9
6.7
53
19
ACCURACY
% BIAS
-17
-25
15
-14
-10
44
-2.3
5
31
4.4
17
-1.9
-22
-3.1
a Source: Draft Compendium of Information and Performance Data on Routinely Used Measurement Methods (RUMM)
Pilot Phase, RTI/3087/03, prepared for EPA Quality Assurance Management Staff, January 1986.
This document should be consulted for more information on individual analytes.
-------
TABLE B-2. HISTORICAL PRECISION AND ACCURACY DATA/WATER
LEVEL III SW-846 METHODS
Method
Number
ORGANICS:
8010
8020
8030
8040
8060
8080
8090
01 8100
8120
8140
8150
8240
8250
8040
8310
Method Name
Halogenated Volatile Organ! cs
Aromatic Volatile Organics
Acrolein, Acrylonitrile,
Acetonitrile
Phenols
Esters
Organochlorine Pesticides
and PCBs
Nitroaromatics and Cyclic
Ketones
Polynuclear Aromatic
Hydrocarbons
Chlorinated Hydrocarbons
Organophosphorous Pesticides
Chlorinated Herbicides
Volatile Organics
GC/MS Semivolatiles (Packed
Column)
GC/MS Semivolatiles
(Capillary)
Polynuclear Aromatic
Hydrocarbons (HPLC)
(Capillary)
Data
Source
SW
SW
SW
SW
846
846
846
846
EPA 606
SW
SW
SW
SW
SW
SW
SW
846
846
846
846
846
846
846
Range of
Recovery (%)
75.1
77.0
96 -
41 -
82 -
86 -
63 -
NAb
76 -
56.5
NA
95 -
41 -
NA
78 -
- 106.1
- 120
107
86
94
97
71
99
- 120.7
107
143
116
Precision
(%)
2.0
9.4
5.6
7.9
1.3
1.3
3.1
NA
10 -
5.3
NA
9 -
20 -
NA
7.3
- 25.1
- 27.7
- 11.6
- 16.5
- 6.5
- 6.5
- 5.9
0
0
0
MDL
(mg/1)
.03 -
.2 -
.5 -
058 -
0
0
0
.29 -
.29 -
0
0.
0.
2.
3
3
•
4
6
2
•
•
.06/ND
NA
- 25
- 19.9
28
- 145
0
0
0
1
0
.03 - 1.
.1 -
.1 -
.6 -
.9 -
5.
0
200
6.
9
44
NA
- 12.9
0
.03 - 2.
-------
TABLE B-2. HISTORICAL PRECISION AND ACCURACY DATA/WATER
(continued)
LEVEL III SW-846 METHODS
Method
Number
Method Name
Data
Source
Range of
Recovery (%)
Precision
(%)
MDL
(mg/1)
INORGANICS; Metals (ICAP) EPA 200.7 NA 3 - 21.9 (RSD) 1.3 - 75 Mg/1
Metals (FLAME) 7000 Series EPA 200 NA NA 0.01-5
7000 Series Metals (FLAMELESS/GF) EPA 200 NA NA 0.001-0.2 Mg/1
7470 Metals (MERCURY) EPA 245.2 87-125 0.9-4.0 0.0002
9010 Cyanides EPA 335.2 85 - 102 0.2 - 15.2 0.02 Mg/1
9030 Sulfides EPA 376.1 NA NA 1 Mg/1
a. For water only
b. NA = Not Available
NOTES: Method Detection Limit (MDL) as listed on this table is the minimum concentration of a substance
that can be measured and reported with 99% confidence that the value is above zero.
Accuracy, presented as an average percent recovery, was determined from replicate (10-25) analyses
of water and wastewater samples fortified with known concentrations of the analyte of interest or
near the detection limit. In most cases this was less than 10 times the MDL.
Precision data are used to measure the variability of these repetitive analyses reported as a single
standard~deviation or, as a percentage of the recovery measurements. For presentation purposes accuracy,
precision and MDL information is presented as an average range of individual values for every analyte
covered by the procedure. If specific information on a particular compound is required, the specific
analytical method cited should be consulted.
-------
TABLE B-3. HISTORICAL PRECISION AND ACCURACY DATA/WATER*
LEVEL IV ANALYTICAL TECHNIQUES - CLP RAS METHODS
ANALYTES
Volatilesb
Methylene chloride
1,1-Dichloroethene
1,1-Dichloroetheme
Trans-1,2-Dichloroethene
Chloroform
1,2-Dichloroe thane
1,1,1-Trichloroethane
Carbon Tetrachloride
1,1,2,2-Tetrachloroethane
Bromodichloromethane
, 1,2-Dichloropropane
Trans-1,3-Dichloropropene
Trichloroethene
Dibrornochloromethane
1,1,2-Trichloroethane
Benzene
Cis-1,3-Dichloropropene
Bromofonn
Tetrachloroethene
Toluene
Chlorobenzene
Ethyl Benzene
Semiyolatilesd
bis(2-Chloroethyl)ether
2-Chlorophenol
1,3-Dichlorobenzene
1,4-Di chlorobenzene
1,2-Dichlorobenzene
2-Methylphenol
bis(2-Chloroisopropyl)ether
TECHNIQUE
Purge & Trap GC/MS
CONCENTRATION
RANGE
N.A.C
GC/MS
N.A.
PRECISION
% RSD
56
20
13
31
12
13
19
12
11
19
18
31
17
14
11
12
22
16
13
14
14
4
24
29
24
21
29
29
25
ACCURACY
Bie
+36.6
-26.3
-46.4
-21.7
-21.1
+2.4
-41.0
-32.1
-5.8
-13.0
-12.9
-41.2
-22.8
-3.3
-7.0
-3.3
-35.5
+6.5
-42.5
-23.3
-15.9
-31.9
-16
-21
-48
-25
-28
-30
-22
-------
TABLE B-3. HISTORICAL PRECISION AND ACCURACY DATA/WATER*
(continued)
LEVEL IV ANALYTICAL TECHNIQUES - CLP RAS METHODS
CO
ANALYTES
Semivolatilesd
4-Methylphenol
N-Ni t roso-di-n-propylamine
Nitrobenzene
Isophorone
2-Nitrophenol
bi s (2-Chloroethoxy) methane
2,4-Dichlorophenol
1,2,4-Trichlorobenzene
Naphthalene
4-Chloro-3-methylphenol
2,4,6-Trichlorophenol
2-Chlo ronapthalene
Acenapthene
2,4-Dinitrophenol
2,4-Dinitrotoluene
2,6-Dinitrotoluene
4-Chlorophenyl-phenylether
Fluorene
4,6-Dinitro-2-methylphenol
4-Bromophenyl-phenylethe r
Hexachlorobenzene
Pentachlorophenol
Phenanthrene
Fluoranthene
Benzo(b)fluoranthene
Benzo(a)pyrene
TECHNIQIJE
GC/MS
CONCENTRATION
RANGE
N.A.C
PRECISION
% RSD
33
31
32
23
30
34
29
30
44
26
25
24
28
24
34
25
34
25
30
32
36
31
21
42
39
42
ACCURACY
% Bias
-36
+0.3
-23
-8
-21
-2.6
-20
-47
-38
-32
-17
+3.4
-12
-23
-33
-48
+12
-24
-13
-0.1
-42
-24
-28
-15
-10
-29
-------
TABLE B-3. HISTORICAL PRECISION AND ACCURACY DATA/WATER*
(continued)
LEVEL IV ANALYTICAL TECHNIQUES - CLP RAS METHODS
ANALYTES
Metals8
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Maganese
Mercury
Nickel
Potassium
Selenium
Sodium
Thallium
Tin
Vanadium
Zinc
TECHNIQUE
ICP
ICP
Furnace AA
ICP
ICP
ICP
ICP
ICP
ICP
ICP
ICP
Furnace AA
ICP
ICP
Cold Vapor
ICP
ICP
Furnace AA
ICP
Furnace AA
ICP
ICP
ICP
CONCENTRATION
RANGE
1000-3000 ug/1
180-600 ug/1
50-150
800-1500
30-45
25-50
1000-30000
50-150
200-1000
125-250
200-800
30
10000-40000
30-150
5-20
160
10000-20000
50
10000-45000
80-100
160
60-200
50-800
PRECISION
% RSD
9.1
11
9.4
6.8
15
12
6.0
9.8
6.7
6.7
10.4
32
6.6
6.2
18.8
9.0
16.2
8.7
8.7
17.7
N.A.C
7.6
9.1
ACCURACY
% Bias
-4.3
-9.2
-8.3
-3.9
+3.7
-3.3
-1.6
-2.6
-2.9
-1.1
+6.5
-0.7
-2.5
-1.0
-14.4
-2.5
-12.1
-5.7
-2.8
-4.2
-2.5
-0.46
+3.0
a. Source: Quality Control in Remedial Site Investigation: Hazardous and Industrial Solid Waste Testing, Fifth
Volume, ASTM STP 925, C.L. Perket, Ed., American Society for Testing Materials, Philadelphia, 1986.
-------
b. Volatile precision and accuracy data from 26-34 laboratories' results on quarterly blind performance
evaluation samples; 29-152 data points for each compound.
c. N.A. = Not Available.
d. Semivolatile precision and accuracy data from 1985 preaward program data; 22-227 data points for each compound.
e. Metals precision and accuracy data is based on performance evaluation sample results from 18 laboratories;
number of data points is not given.
10
-------
TABLE B-4. HISTORICAL PRECISION AND ACCURACY DATA/SOILS
LEVEL I FIELD SCREENING TECHNIQUES
MEASUREMENT
Resistivity
Terrain
Conductance
Terrain
Conductance
Magnetic Field
Intensity
Subsurface
Lithology
Changes
Subsurface
Lithology
Changes
INSTRUMENT
(TECHNIQUE)
Bison 2390 T/R
(Resistivity meter)
EM 31
( conductivity)
EM 34-3
(conductivity)
EDA - Omni IV
(Magnetometer)
SIR-8
(Ground Penetrating
Radar)
EG+G 1225
(Seismograph)
INSTRUMENT
RANGE
0-1999
millivolts
0-1000
millimhos/meter
0-300
millimhos/meter
18000-11000
gammas
1-81 dielectric
constant
0-2000
milliseconds
INSTRUMENT
PRECISION b
at 1% range setting,
0-5% of full scale
2% of full scale
2% of full scale
0.02 gamma
N/Ad
N/Ad
INSTRUMENT
ACCURACY c
2% of measured
value
5% at 20 millimhos/meter
5% at 20 millimhos/meter
1 gamma at 50000 gammas
at 23° C
N/Ad
0.01%
-------
TABLE B-4. HISTORICAL PRECISION AND ACCURACY DATA/SOIL
(continued)
LEVEL I FIELD SCREENING TECHNIQUES
MEASUREMENT
Total
Volatile
Organics
INSTRUMENT
(TECHNIQUE)
PHOTO VAC
(GC/Photoionization)
FIELD SCREENING
RESULTS in ppm (X)
11.4
22.0
56.0
139
70.0
24.9
60.0
6.6
12.1
8.7
CLP ACCURACY6
RESULTS in ppm (Y) (% Bias)
26.9 -57.6
32.8 -32.9
129.7 -56.8
228.0 & 258.0 -42.8
126.7 -44.8
2823.0 +99.1
53.3 +12.6
0.056 +116.9
0.032 +377.1
0.024 +361.5
a. Source: Manufacturers' manuals unless otherwise cited. Mention of specific models does not constitute an
endorsement of these instruments.
b. Precision refers to reproducibility of meter or instrument reading as cited in instrument specifications.
c. Accuracy refers to instrument specifications unless otherwise cited.
d. N.A. = Not available.
e. Accuracy of PhotoVac field screening results calculated by assuming that CLP results on the same samples
were completly accurate. % Bias = 100 (X-Y). Source of these data is COM project files.
Y
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TABLE B-5. HISTORICAL PRECISION AND ACCURACY nATA/SOILa
LEVEL II FIELD ANALYSIS
LEVEL II FIELD TECHNIQUES
INSTRUMENT FIELD RESULTS
ANALYTES (TECHNIQUE) IN ppm (x)
PCBs HNu 301 6.0
(GC/Electron Capture) 6.0
6.0
9.0
13.0
14.0
14.0
21.0
M 35.0
w 41.0
48.0
50.0
65.0
67.0
92.0
95.0
11
202
269
286
1215
1647
3054
CLP RESULTS
IN ppm (y)
22.0
6.1
510.0
3.9
3.0
3.1
23.5
8.1
7.7
2.1
11.0
460.0
23.1
18.7
75.0
30.0
12.3
99.0
370.0
80.5
640.0
1040.0
9,300
ACCURACY"
% BIAS
-72.7
-1.6
-98.8
+56.7
+333.3
+351.6
-40.5
+159.3
354.5
+1,852
+336.3
-89.1
+181.4
+258.3
22.7
+216.7
-10.6
+104.0
-27.3
+255.3
+90.0
+58.4
-67.2
a. Source: CDM Project files.
b. Source: Accuracy calculated by assuming'that CLP results on the same samples were completely accurate,
% Bias = 100 (x-y)
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TABLE B-6. HISTORICAL PRECISION AND ACCURACY DATA/SOIL*
LEVEL III ANALYTICAL TECHNIQUES - METHODS OTHER THAN CLP RAS METHODS
ANALYTE METHOD CONCENTRATION PRECISION ACCURACY
(TECHNIQUE) RANGE % RSD % BIAS
Dioxins 8280 5 ppb 6-30 N.A.
(HPLC/LRMS) 125 ppb 3-10 N.A.
JAR EXTRACTION GC/MS 1 ppb 20 0
10 ppb 10 -18
a. Source: Draft Compendium of Information and Performance Data on Routinely Used Measurement Methods (RUMM) -
Pilot Phase, RTI/3087/03, prepared for EPA Quality Assurance Management Staff, January 1986. This
document should be consulted for more information on individual analytes.
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TABLE B-7. HISTORICAL PRECISION AND ACCURACY DATA/SOILS3
LEVEL IV ANALYTICAL TECHNIQUES - CLP RAS METHODS
ANALYTES
Volatilesb
Chloroform
1,2-Dichloroethane
Dibromochloromethane
Benzene
Brornaform
2-Hexanone
Toluene
Chlorobenzene
Semivolatilesd
1,4-Dichlorobenzene
Nitrobenzene
isophorone
2-Nitrophenol
2,4-Dichlorophenol
1,2,4-Trichlorobenzene
Penta Chlorophenol
Pyrene
2-Methylnahthalene
bis-(2-Ethylhexyl)phthalate
Phenol
Acenaphthylene
Diethyphthalate
Dioxin6
1,3,7,8-TCCD
TECHNIQUE
Purge & Trap GC/MS
CONCENTRATION
RANGE
N.A.C
GC/MS
N.A.
1-10
PRECISION
% RSD
8.0
13.1
35.0
32.1
16.6
16.6
13.8
21.2
27
21
24
35
31
28
17
25
26
33
38
26
16
15
ACCURACY
-0.1
+11.1
-12.0
-10.3
-12.1
-45.5
+13.7
+13.2
-48
-47
-36
-59
-43
-48
-15
-42
-2
-27
-27
-20
-11.5
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TABLE B-7. HISTORICAL PRECISION AND ACCURACY DATA/SOILS*
(continued)
LEVEL IV ANALYTICAL TECHNIQUES - CLP RAS METHODS
ANALYTES
Metalsb
Aluminum
Cadmium
Calcium
Chromium
Copper
Iron
Lead
Magnesium
Manganese
Mercury
Nickel
Tin
Zinc
TECHNIQUE
ICP
ICP
ICP
ICP
ICP
ICP
Furnace AA
ICP
ICP
Cold Vapor
ICP
ICP
ICP
CONCENTRATION
RANGE (ua/ka)
2-22600
5.5-20
2664-29000
8.5-29600
33-109
5028-113000
11.5-714
2428-7799
73.5-785
1.1-26.5
44-67
N.A.C
19-1720
PRECISION
% RSD
14.4
33.3
N.A.C
7.8
11.2
10.7
9.2
7.5
9.4
25.0
15.0
44.1
5.8
ACCURACY
% Bias
-78.8
+2.9
-4.2
-6.1
-2.5
-27.0
-2.2
-10.6
-15.1
-9.1
-17.0
N.A.°
-6.2
a. Source: Quality Control in Remedial Site Investigation: Hazardous and Industrial Solid Waste Testing, Fifth
Volume, ASTM STP 925, C.L. Perket, Ed., American Society for Testing Materials, Philadelphia, 1986.
b. Volatiles precision and accuracy data is based on 1985 preaward analysis results from laboratories awarded
contracts; 6-14 data points for each compound.
c. N.A. » Not Available.
d. Semivolatiles precision and accuracy data is based on 1985 preaward analysis results; 9-20 data points for
each compound.
e. Dioxin precision for accuracy data is based on results of four performance evaluation samples including 120
data points.
f. Metals precision and accuracy data is based on performance evaluation sample results from 18 laboratories;
number of data points is not given.
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TABLE B-8. HISTORICAL PRECISION AND ACCURACY DATA/AIR*
LEVEL I FIELD SCREENING TEHCNIQUES
ANALYTES
Organics
Organics
Organics
Organics
INSTRUMENT
(TECHNIQUE)
Century OVA-128
(Flame lonization)
HNu PI-101
( Photoionization )
AID - 710
(Flame lonization)
PhotoVac
(GC-Photoion-
ization)
INSTRUMENT
RANGE
0.1 - 1000 ppm
Methane
0.1 - 2000 ppm
Benzene
0.1 - 2000 ppm
Methane
N.A.
INSTRUMENT
SENSITIVITY0
0.1 ppm Methane
0.1 ppm Benzene
0.1 ppm Methane
0.001 ppm
Benzene
INSTRUMENT
PRECISION c
N.A.d
1% of full scale
deflection
N.A.d
N.A.
a. Source: Manufacturers' manuals unless otherwise cited. Mention of specific models does not constitute
an endorsement of these instruments.
b. It is difficult to differentiate between Level I and Level II techniques and instrumentation. Several
instruments may be used at both levels.
c. Sensitivity and precision refer to instrument specifications.
d. N.A. = Not Available.
-------
TABLE B-9. HISTORICAL PRECISION AND ACCURACY DATA/AIR
LEVEL II FIELD TECHNIQUES11
oo
ANALYTES
Organ! cs
Compound-
Specific
Organics,
Compound-
Specific
Organics,
Compound-
Specific
Organics,
Compound-
Specific
Mercury
INSTRUMENT
(TECHNIQUE)
Mi ran IB
(Infrared)
Century OVA-128
(GC/Flame
lonization)
PhotoVac
(GC-Photo-
ionization)
SCENTOR
(Argon lonization
or Electron Capture)
Gold film Mercury
Analyzer
INSTRUMENT
RANGE
Compound Dependent
0-2000 ppm
1-1000 ppm
Methane
N.A.
N.A.
N.A.
INSTRUMENT
SENSITIVITY0
N.A.d
N.A.
0.001 ppm
Benzene
0.001 ppm
Benzene
less than
0.01 ppm
INSTRUMENT
PRECISION c
N.A.d
N.A.
N.A.
N.A.
N.A.
a. Source: Manufacturers' manuals. Mention of specific models does not constitute an endorsement
of these instruments.
b. It is difficult to differentiate between Level I and Level II techniques and instrumentation.
Several instruments may be used at both levels.
c. Sensitivity and precision refer to instrument specifications.
d. N.A. - Not Available.
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TABLE B-10. HISTORICAL PRECISION AND ACCURACY DATA/AIR*
LEVEL III ANALYTICAL TECHNIQUES - METHODS OTHER THAN CLP RAS METHODS
ANALYTES
Benzene
Toluene
Tr i chloroe thene
Vinyl Chloride
Lead
METHOD
(TECHNIQUE)
CRYOGENIC TRAP/GC
TENAX GC/MS
40 CFR 50, APP G
(FLAME AA)
CONCENTRATION
RANGE
3.9 ppb
93 ppb
7.8 ug/m3
4.5 ug/m3
10.8 ppm
3.5 ppb
84 ppb
7.8 ppb
0.6 ug/m3
8.01 ug/m3
PRECISION
4.0
5.1
11
21
5.11
4.1
3.7
6.37
8.6
3.9
ACCURACY
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
N.A.
0
-3.6
a. Source: Draft Compendium of Information and Performance Data on Rountinely Used Measurement Methods (RUMM)
Pilot Phase, RTI/3087/03, prepared for EPA Quality Assurance Management Staff, January 1986. This document
should be consulted for more information on individual analytes.
-------
TABLE B-ll. HISTORICAL PRECISION AND ACCURACY DATA/OTHER MEDIA*
LEVEL III ANALYTICAL TECHNIQUES - METHODS OTHER THAN CLP RAS METHODS
ANALYTE
Lead
METHOD
(TECHNIQUE)
6010
(ICP)
Solid
MEDIUM
Oil Waste
Solid Waste
Sludge
CONCENTRATION
RANGE
1.0 mgAg
-2.5 mg/kg
50 mgAg
75 mg/kg
5 mg/kg
20 mg/kg
PRECISION
% RSD
3.1
22
10
3.7
2
11
ACCURACY
% BIAS
-10
-20
3.4
-0.8
0
55
to a. Source: Draft Compendium of Information and Performance Data on Routinely Used Measurement Methods (RUMM)
0 Pilot Phase, RTI/3087/03 prepared for EPA Quality Assurance Management Staff, January 1986. This
document should be consulted for more information on individual analytes.
-------
APPENDIX C
USER COMMENT FORM
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FIELD SCREENING METHODS CATALOG (FSMC)
USER COMMENT FORM
Your comments and suggestions are important to us. Comments may relate to the
software, user manual, or mini-guide, or may be a request for an addition or correc-
tion to the method descriptions, and additional copies of the system discs. Please
return this form to:
FSMC System Coordinator
Office of Emergency and Remedial Response
Analytical Operations Branch (WH-548-A)
U.S. Environmental Protection Agency
Washington, DC 20480
Please provide the following information so that we may follow up if necessary.
Your name:
Address:
Phone number:
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