M 1
United States
Environmental
Protection
Agency
Office of Water Office of Solid Waste EPA
Regulations and and Emergency 530-SW-87-O05_ET
Standards (WH-552) R.6»P?nse
Washington, D.C. £jK.J?9tO11' D-c-
20460 2046°
&EPA
TECHNICAL REPORT: APPENDIX E
EXPLORATION, DEVELOPMENT, AND PRODUCTION
CRUDE OIL AND NATURAL GAS
ROLE AMD FUNCTION
U.S. Environmental Protection Agency
Region 5, Library (PL42J)
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APPENDIX E
ROLE AND FUNCTION OF THE EPA SAMPLE CONTROL CENTER
TABLE OF CONTENTS
Page
An Introduction to the Sample Control Center
and a Guide to Its Services E-l
Attachment 1
Organics Traffic Report .... . E-19
Attachment 2
Description of Metals Analysis Sheet E-21
Attachment 3
Method 1624 - Volatiles, Volatile Gases and
Water Soluble Compounds Standards' Concentrations .... E-23
Attachment 4
Laboratory Chronicle E-25
Attachment 5
Isotope Dilution Episode Sample Report E-27
Attachment 6
ITD Data Elements E-29
Attachment 7
Methods 1624 and 1625 E-103
Attachment 8
Instructions for Use of Labeled Compounds ... E-225
Attachment 9
Quantitation Reports on Magnetic Tape E-247
Attachment 10
Sample Extract Transmittal Form E-309
Attachment 11
GCMS Raw Data on Magnetic Tape E-315
Attachment 12
Laboratory Results, Metals Analysis form E-321
Attachment 13
SCC Tape Processing Steps E-323
Attachment 14
Quality Assurance Tests of Data Elements
on Quantitation Reports E-329
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U.S ENVIRONMENTAL PROTECTION AGENCY
INDUSTRIAL TECHNOLOGY DIVISION
SAMPLE CONTROL CENTER
An Introduction to the Sample Control Center
and a
Guide to Its Services
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INTRODUCTION
The Industrial Technology Division (ITD) (formerly the Effluent
Guidelines Division) of EPA conducts programs for collection and analysis
of samples from treatment systems in industrial plants. The objective of
this sampling and analysis effort is to determine the presence and to
quantify the levels of pollutants so that ITD can promulgate nationwide
standards and guidelines for control of industrial discharges. Personnel
from EPA Headquarters, EPA Regions, and independent contractors have
been organized to collect and analyze samples on an as-needed basis by
ITD.
The program conducted by ITD generates thousands of sub-samples
and extracts for analysis. In order for analytical results to be valid, it is
imperative that the collection, analysis, data collection, and data quality
assurance processes be conducted in accordance with a carefully controlled
schedule. It presently costs nearly $4,000 to collect, analyze, and quality
assure the results from each sample. Any of the following problems can
cause the data from a sample to be rendered useless and to necessitate
repeating the process and expenditure:
loss of a sample
a delay in processing
unlabeled or mis-labeled containers
lack of control in tracking
violation of the sample holding time
improperly conducted analysis
failure to quality assure the result
ITD has created the Sample Control Center to ensure the orderly
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flow of samples and analytical data through the sampling, analysis, and
quality assurance system, and to insure that the above problems are
minimized.
This guide gives the purposes and objectives of the Sample Control
Center, and an overview of the operations conducted by the Center. For
the most part, these operations are controlled by forms. Throughout this
guide, the names of these forms are shown in boldface type. Where
appropriate, supporting documents are included as attachments to this
guide. These attachments provide the details of the requirements for
operation of the sample control, data collection, and quality assurance
functions that the Center performs.
PURPOSE OF THE SAMPLE CONTROL CENTER
The Sample Control Center was conceived and designed to provide
an efficient mechanism for controlling the logistics of the nationwide
sampling and analysis programs for ITD. Practices and procedures have
been implemented which control sample flow from collection through
analysis and data flow through quality assurance and final reporting.
Much effort has gone into making sure that the amount of control is
sufficient to prevent sample and data misidentification or loss without the
record-keeping becoming self-defeating.
Record-keeping is implemented through the Episode File; sample flow
is controlled through Traffic Reports; analyses are controlled through
Laboratory Chronicles, and data flow and data quality assurance are
controlled through the Data Tracking and Quality Assurance systems.
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The purpose of the Center is to maintain an orderly flow of
samples, analyses, and data, so that ITD objectives are met. The
management of the Center has made every effort to accomplish these
purposes by thoroughly studying the requirements of ITD Management,
ITD Project Officers, EPA Regional Surveillance and Analysis personnel,
ITD sampling contractors and analysis laboratories, and by implementing a
system for reporting and quality assuring gas chromatography-mass
spectrometry data recieved on magnetic tape.
OBJECTIVES OF THE SAMPLE CONTROL CENTER
The objectives of the ITD Sample Control Center are to:
Provide logistical support to everyone involved in the field operation
of the sampling and analysis program.
Insure effective traffic control of all materials.
Insure data integrity.
Provide status of all samples, extracts, and data.
Consolidate and report management information and analysis results
to ITD.
Provide statements of data quality to ITD Project Managers.
Increase the cost efficiency of sampling and analysis programs.
Provide consistent, time-saving procedures for Sampling Contractors,
Regional S&A personnel, EPA Laboratories, and Contract
laboratories.
OVERVIEW OF SAMPLING, ANALYSIS, AND QUALITY ASSUR-
ANCE PROCEDURES
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The Sample Control Center is brought into action when an ITD
Project Officer has need for analysis data to support development of an
Effluent Guideline. The request for analysis generally comes through the
ITD Project Officer responsible for operation of the Center. This Project
Officer is presently W A Telliard. Schedules, laboratory availability, level
of sampling effort, and funding mechanisms are worked out with the
Project Officer, and the sampling and analysis effort can then begin.
To begin the scheduling process, SCC personnel create a permanent
Episode Sample File containing the following scheduling information:
Name and affiliation of the individual requesting the analysis.
The specific analyses requested.
Date of the request.
Responsible ITD Project Officer.
Facility name and location.
Industrial Category.
Scheduled sampling and shipping dates.
Sampling organization, contact, and telephone number.
Number and types of samples to be collected.
The following sub-sections give details of the Sampling, Analysis,
Data Reporting and Quality Assurance activities of the Sample Control
Center which support Project Officers within the Industrial Technology
Division of EPA.
SAMPLING
When an ITD Project Officer initiates a sampling effort for a
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particular location, the Sample Control Center schedules these samples for
shipment to a particular Analysis Laboratory, opens a file on that
sampling Episode, and prepares a packet of material to send to the
Sampler. (An Episode refers to a group of samples collected at a given
plant or location within the same calendar week.) All forms and labels
bear a single identification number which serve as a permanent reference
to collection and analysis of samples at a given sampling point. The
packet normally contains the following:
Episode Number assignments
Laboratory assignments
Sample Volume and Preservative Requirements for special analytes
Traffic Report(s) - With Adhesive Sample Labels
The above items were designed to:
be easy to use
keep writing requirements to a minimum
provide clear guidance and instruction
allow for individualized training
be amended, modified as needed
provide a documented record of events
The Traffic Report is a four-part carbonless form used primarily to
document the dates samples were taken, shipped and received. The top
white copy is returned by the Sampler to SCC. The yellow copy becomes
the Sampler's copy. The bottom two copies are then sent in a Ziploc bag
with the samples to the Analysis Laboratory. Upon receipt of the
samples, the Analysis Laboratory completes the required information on
the Traffic report, returns the pink copy promptly to the Center, and
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retains the gold copy for its records. There are four types of Traffic
Reports currently in use by the center:
Organics Traffic Report
Metals Traffic Report
Asbestos Traffic Report
Generic Traffic Report
The color coding of the copies is alike in all four types and the
information recorded on each is very similar. An example of an Organics
Traffic Report is shown in Attachment 1. This example does not show
the color coding or that the sample numbers are adhesive backed.
Personnel who wish to become familiar with these forms should request a
copy from the Center. The organics, metals, asbestos, and generic forms
were designed to accommodate the differences in the sampling and analy-
sis programs.
The preprinted and prenumbered Adhesive Sample Labels affixed to
the Traffic Reports are secured to sample containers by the Sampler.
Where necessary, the label is protected from attack by water and solvents
with clear cellophane tape which is designed to resist this attack.
The Sampler uses one Traffic Report per day for all samples in a
sampling episode, if possible. If not, more Traffic Reports are used, as
required. If organics and metals samples are collected from the same
point, the Sampler assures that the Organics and Metals Traffic Reports
have the same identification number. A quantity of labels printed with
numbers only are provided so that the Sampler may describe and identify
any additional samples taken. After sampling, the first page (white copy)
of the Traffic Report is mailed to the Sample Control Center, the yellow
copy is retained by the Sampler, and the remaining two copies are sent to
the Analysis Laboratory with the samples. The Sample Control Center
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typically includes two extras.
When Laboratory Chronicles, Additional Sample Labels, and/or
Description of Metals Analysis Sheets are included in the packet, they
are sealed in Ziploc bags and forwarded to the lab(s) with the first
sample shipment.
ANALYSIS
Laboratories analyze samples under analytical contracts with EPA or
under Special Analytical Services (SAS) contracts with the Sample Control
Center through Viar and Company. These contracts specify requirements
for sample analysis including the analytical methods. The Description of
Metals Analysis Sheet identifies the elements to be analyzed by the metals
laboratory. The Center sends the Description(s) to the lab(s) prior to the
first shipment of metals samples. An example of this form is shown in
Attachment 2.
The Sample Control Center interacts in the chemical analysis of
samples only when the laboratory calls with an analytical problem. In
the past, most of these problems have dealt with the analysis of difficult
organic samples. The latest revisions of the methods for analysis of
organics contain provisions for analysis of such difficult samples, so the
number of such calls have been minimized. Nevertheless, in the event
that a laboratory calls with a problem related to the analysis, and Center
personnel cannot answer the question, the Project Officer is contacted
immediately for resolution. Delays in responding to a laboratory's request
for resolution of a problem can delay the analysis and submission of
results.
Volatile Gases and Water Soluble Compounds. EPA Method 1624
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permits analysis of certain "volatile gases and water soluble compounds" at
one of two concentrations. IFB and SAS contracts require the laboratory
to notify the Center at which concentration these compounds will be
calibrated and analyzed. The Method 1624 - Volatiles, Volatile Gases and
Water Soluble Compounds Standards' Concentrations form is used for this
purpose. An example of this form is shown in Attachment 3. This form
must be received by the Center, and the concentrations loaded into the
appropriate table in the computer prior to the time data on tape are
received from the laboratory; otherwise, certain computerized tests of the
data submitted by the laboratories will be failed.
Sample Logistics. Laboratories are required to submit data related to
sample logistics. Each laboratory notes on its copies of the Traffic
Report the dates the samples were received and their condition on receipt.
The pink copy is returned to the Sample Control Center and the gold
copy is retained by the lab.
During organic sample preparation and analysis, dates, technicians'
names and any problems or relevant comments are recorded on the Labo-
ratory Chronicle, shown in attachment 4. Upon completion of analysis,
the white copy of the Laboratory Chronicle is included as part of the
data package and the yellow copy is retained by the lab. The laboratory
is responsible for the analysis and for full compliance with all specifica-
tions in the contract, including those in the quality assurance section of
the analytical method.
DATA REPORTING
Data reporting requirements are project specific, but follow a
general pattern. Data related to sampling and sample tracking are stored
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in the SAMple TRACking (SAMTRAC) system. Data from the analysis of
organics are reported on magnetic tape according to a set of documents
which define the tape specifications and format; all other data (metals,
asbestos, and other special analyses) are reported on data sheets.
Sampling Data. Data from the Project Officer, Traffic Reports and
Laboratory Chronicles related to sampling and sample tracking are entered
into the SAMTRAC system at the Sample Control Center. These data are
accumulated in the Episode Sample File. From this file, various reports
related to the sampling data can be produced. One such report related to
the sampling and analysis of organics is the Isotope Dilution Episode
Sample Report. An up-to-the-minute copy of this report is maintained at
the Sample Control Center. From this report, all plant and sample
specific information can be retrieved. A copy of a page from this report
shown in Attachment 5. The sample stream descriptions and comments
listed on this report are explained more fully in the Data Element
Dictionary.
Organic Data. Prior to 1983, organic data were received on data
sheets. In 1983 ITD began receiving these data on magnetic tape. The
documents which define the tape specifications and format are the:
Data Element Dictionary (ITD Data Elements)
Analytical Methods (presently Methods 1624C and 1625C)
Instructions for Use of Labeled Compounds
[Specifications for] Quantitation Reports on Magnetic Tape
The present revisions of these documents are Attachments 6 thru 9,
respectively.
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Data Element Dictionary. The ITD Data Elements define the data
elements collected and stored in the data base at EPA's National Com-
puter Center (NCC). A "Summary of Data Sources for Collection of
Organic Priority Pollutant Data" is given in the table on pages 6 and 7
of the ITD Data Elements in Attachment 6. This table shows the source
of each data element. Notice that the Sample Number is common to all
data sources; i.e., the Sample Number ties all of the data together.
Analytical Methods. The Analytical Methods are instructions that
laboratories are to follow when they analyze the samples. Methods 1624
and 1625 are isotope dilution GCMS methods for analysis of organic
pollutants. These methods are specified in Invitation for Bid (IFB), Special
Analytical Services (SAS), and other contracts. Methods 1624 and 1625
are shown in Attachment 7.
Instructions for Use of Labeled Compounds. The analysis of organic
compounds by isotope dilution requires the use of stable (non-radioactive)
isotopically labeled compounds. The Instructions for Use of Labeled
Compounds is included in the contract documents, and specifies how the
labeled compounds are to be mixed and spiked into the samples, stan-
dards, and blanks. These instructions are shown in Attachment 8. The
Center supplies labeled compound solutions on an "as needed" basis by the
laboratories. Labeled compound solutions have been synthesized to date by
Merck & Co., Isotopes Division, Quebec, Canada. These solutions are kept
in freezers at the SCC Chemical Repository in Baltimore, and are shipped
as directed by the Center personnel.
After the laboratory completes analysis of a sample or group of
samples, the lab is required to ship data and other deliverables to the
Center, and to other locations specified in the contract or as directed by
the Project Officer.
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Quantitation Reports on Magnetic Tape. Organics data are shipped
to the Center on magnetic tape per the specifications in Quantitation
Reports on Magnetic Tape in Attachment 9. Tapes are received by the
Center, logged-in, and shipped to the NCC in Research Triangle Park,
North Carolina. Data are deblocked and quality assured as described in
the section on "Quality Assurance" below.
Sample Extracts. Other deliverables required by the organics'
contracts include sample extracts and raw GCMS data on magnetic tape.
Sample Extracts are normally shipped to the Repository where they are
stored in freezers for later use. A Sample Extract Transmittal Form is
shown in the contract and accompanies each shipment of extracts.
Requirements for shipment of sample extracts are shown in Attachment
10.
Raw GCMS Data Tapes. Raw GCMS Data Tapes (not to be con-
fused with tapes containing Quantitation Reports) are normally shipped to
Dr John McGuire at EPA's Environmental Research Laboratory in Athens,
Georgia. Specifications for raw data tapes are contained in Attachment 11.
A Tape Transmittal Form, also shown in the Attachment, accompanies
each tape. The extracts and tapes are shipped as directed by the Project
Officer responsible for operation of the Center.
Metals Data. Metals sampling, analysis, and data reporting are
similar to those given above for organic samples; i.e., there are contracts
and methods for analysis of metals and forms for tracking and reporting.
Metals data are reported on data sheets using the Sample Control Center
Laboratory Results, Metals Analysis form. A copy of this form is shown
in Attachment 12, and is included in metals' contracts. The Project
Officer specifies the metals to be analyzed in each sample, and the
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technique to be used.
QUALITY ASSURANCE
The analysis laboratory and the Sample Control Center quality assure
the data received at the Center. All data are to be quality assured by
the analytical laboratories prior to submittal, so the Center's main
function is to check that the laboratory has properly assured the data.
GCMS Data. GCMS data are received in the form of quantitation
reports on magnetic tape and are 100 percent quality assured by the
Center. A Quantitation Report Tape Transmittal Form accompanies each
tape and lists the specific files on that tape. This form is shown at the
back of Attachment 9. When a tape is received at the Center, it is
assigned a tape number and a record is entered in the tape log. The tape
is then forwarded to NCC for processing. The processing steps are shown
in the SCC Tape Processing Steps document in Attachment 13. The
quality assurance process occurs in four major steps:
(1) Tapes are "de-blocked" into individual files. Each file
represents a quantitation report or a piece of a quantitation report for a
given sample, standard, or blank. There can be at most three pieces
(files) which make up a full quantitation report. And because each
sample is divided into three fractions (acid, base/neutral, and volatile), up
to nine files may represent the results of analysis of a single sample.
The de-block report gives errors related to sample and analysis logistics.
The data elements tested are:
The date and time analyzed. This date and time are compared with
the date and time sampled to assure that the holding time for the
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sample (or extract) has not been exceeded.
An instrument identifier. All data are tracked by each specific
GCMS instrument within a laboratory to certain that the
instrument is in calibration when samples are analyzed.
The shift on which the sample was analyzed.
The quantitation report type. This element identifies the analysis as
a Sample, Standard, or Blank.
The EPA Sample Number, or the concentration of the standard.
A single letter code for the fraction.
The concentration/dilution factor (see the Data Element Dictionary
for a detailed definition of this data element).
The date and shift on which the sample was extracted, if appli-
cable.
A standard and blank are required for each set of samples started
through the extraction process on a given shift.
If any of these data elements are missing or incorrect in any file,
that file cannot be processed further until the error is resolved with the
lab. or the proper information deduced from the Tape Transmittal Form.
(2) Each file is submitted for a Level 1 Edit. This edit tests all
data elements specific to a complete quantitation report. Pieces of a
quantitation report are merged for this process. Data are tested against
specifications in Methods 1624 and 1625. Technical data elements tested
are the:
Compound number.
Compound reference number
Quantitation m/z. Scan number.
Retention time.
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Reference compound.
Relative retention time.
Amount.
Unit of measure.
Response factor.
In addition, reference (library) information is tested. Data elements
tested are the:
Library retention time.
Library relative retention time.
Library amount.
Library response factor.
All of the data elements above (technical and library) are literally
tested; i.e., the data fields requiring a number only are tested to
determine if non-numeric characters are present in the field (including
alphabetical characters, symbols, hyphens, etc). The specific tests at Level
1 are given in greater detail in Attachment 14.
A Level 1 Edit Report is produced which shows errors, if any. If
errors are present which will prevent the Level 2 Edit (described below)
from running, they are resolved with the lab before the files are
submitted for Level 2 Edit.
(3) The Level 2 Method Edit verifies the presence and order of
quality assurance sample and field sample analyses.
(4) The Level 2 Final Edit tests all quantitation reports on a tape
against calibration and other data stored for the instrument on which the
samples were analyzed, to verify that the instrument remained in calibra-
tion for all analyses performed. All specifications requiring multiple
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GCMS runs are tested by this edit; for example, if a tape contains
calibration data, calibration linearity over the 5 point calibration is tested.
In addition to reporting results on magnetic tape, Report Form 1,
which is shown in the specifications for "Quantitation Reports on
Magnetic Tape" may be used by the laboratory for reporting results of
hard to analyze compounds. These results supercede- data on tape.
After all tests are passed, and open data items are resolved with the
laboratory, data are merged into a final data file. This file is processed
through the "Data Base Print' program to produce a final report for the
Project Officer. This report lists the results of analyses of all compounds
in all samples, and includes selection of the result at the most dilute level
within the calibration range of the GCMS instrument. Statements of Data
Quality are produced for labeled compound recoveries from samples and
for analysis of standards by the laboratory. These statements are
consistent with those required by the Methods.
CONCLUSIONS
The Sample Control Center is currently managing the collection and
analysis of samples for numerous ITD programs. Among these are Organ-
ics Screening and Verification, Metals, Asbestos, and Residual Waste.
Since the inception of the Center, all interested parties have benefited
from cost efficiency, immediate problem response, rapid data turnaround
and access to computerized sample tracking information. In summary, the
effectiveness of the Sample Control Center as a management tool has been
proven.
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The success of the control system is based on the consistency of
procedures surrounding the use of the reporting forms, the extensive
computerized and manual record-keeping and the constant phone and
written communication among Center, Sampling, Analysis and EPA person-
nel.
Should you have any questions about the operations of the Sample
Control Center or if you would be interested in receiving copies of any
of our reporting instruments, please contact us at (703) 557-5040. Center
personnel would be pleased to be of assistance.
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00
II
w
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ATTACHMENT 1
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USEPA INDUSTRIAL TECHNOLOGY DIVISION
SAMPLE CONTROL CENTER
P.O. BOX 1407
ALEXANDRIA, VA 22313
703/557-5040 / FTS-8-557-5040
EPISODE NO:
RANGE OF SAMPLE NOS:
ORGANICS TRAFFIC REPORT
INDUSTRIAL FIRM SAMPLED:
CITY:
STATE:
INDUSTRIAL CATEGORY:
CONFIDENTIAL: YES NO
SAMPLING OFFICE:
SAMPLER:
SAMPLING DATE
BEGIN:
END:
SHIPPING INFORMATION
SHIP TO:
ATTN:
CARRIER:
AIRBILL NO:
DATE SHIPPED:
SAMPLE POINT DESCRIPTION
SAMPLE TYPE
SAMPLE
NUMBER
RAW WATER I
(CITY. RIVER. WELL)
IN LINE PROCESS
UNTREATED EFFLUENT
(RAW WASTE WATER)
TREATED EFFLUENT
OTHER
(SPECIFY)
ADDITIONAL SAMPLE
DESCRIPTION
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PH LEVEL
SAMPLE POINT FLOW
UNITS-
_ COMPOSITE 1
C (EXTRACTABLE ORQANICS) |
CB COMPOSITE BLANK
ft GRAB
U (EXTRACTABLE ORGANICS) |
VI VOA PRESERVED
... VOA PRESERVED
« (DUPLICATE) 1
V3 VOA UNPRESERVED
... VOA UNPRESERVED
" (DUPLICATE)
VB1 VOA TRIP BLANK
UB. VOA TRIP BLANK
VB* ((DUPLICATE)
OTHER
SPECIFY: 1
WHITE SCO COPY YELLOW SAMPLER COPY PINK LAB COPY FOR RETURN TO SCC GOLD LAB COPY
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ATTACHMENT 2
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Lab Name
DESCRIPTION OF METALS ANALYSIS
Industrial Category
No. of Samples Scheduled_
Sampling Points
Industrial Subcategory
Sample Numbers
Please analyze these metals samples as indicated below.
ICP EMISSION (Elements 1-21) All 21
1. Calcium
2. Magnesium
3.
Hum
Aluminum
5. Manganese
6. Lead
7. Vanadium
8. Boron
9. Barium
10. Beryllium
11. Cadmium
12. Molybdenum
13. TTn
Yttrium
15. Cobalt
16. Chromium
17. Copper
18. Iron
19. Nickel
20. Titanium
21. Zinc
FURNACE AA (Elements 1 - 6) Check specific elements
1. Selenium
2. Thallium
3. Silver
Arsenic
5. Antimony
6. Mercury
Flame Atomic Absorption (Elements 1 - 20) Check specific elements
Calcium
Magnesium
Hum
Aluminum
Manganese
1.
2.
3.
it.
5.
6.
7.
8.
9.
10. Beryllium
II. Cadmium
Vanadium
Boron
Barium
12. Molybdenum
13. Tin
Cobalt
15. Chromium
16. Copper
17. Iron
18. Nickel
19. Titanium
20. Zinc
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ATTACHMENT 3
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METHOD 162* A - VOLATILES
VOLATILE GASES AND WATER SOLUBLE COMPOUNDS
STANDARDS' CONCENTRATIONS
LABf
LAB NAME
LABELED COMPOUND SPIK
COMPOUND
203 - ACRYLON1TRILE-D3
216 - CHLOROETHANE-D5
2*5 - CHLOROMETHANE-D3
246 - BROMOMETHANE-D3
28S - VINYL-D3 CHLORIDE
61* - 2-BUTANONE-4.».*-D3 (MEK)
615 - DIETHYL-DIO ETHER
616 - ACETONE-D6
ING SOLUTION CONCENTRATIONS
CONCENTRATION UG/L
PRIORITY POLLUTANT C
COMPOUND
516 ACETONE
002 ACROLEIN
003 ACRYLONITRILE
0*6 BROMOMETHANE
016 CHLOROETHANE
005 CHLOROMETHANE
515 DIETHYL ETHER
51* METHYL ETHYLKETONE
088 VINYL CHLORIDE
:ALIBRATION CONCENTRATIONS
CONCENTRATION UG/L
10
20
50
100
200
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ATTACHMENT 4
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U.S. EPA INDUSTRIAL TECHNOLOGY DIVISION SAMPLE CONTROL CENTER
ORGANICS SUPERSCREENING LAB CHRONICLE
Sample No.
Lab Name
Industrial Category
SAMPLE DESCRIPTION
Technician Name
Date Extracted
Analyst Name
Date Analyzed
Detail below pertinent infofmation and/or problems
associated with sample preparation and analysis
and the measures taken to overcome those problems.
Use supplementary sheets to continue if necessary
EXTRACTABLE
(BASE/NEUTRAL)
EXTRACTABLE
(ACID)
EXTRACTABLE
(PESTICIDES)
COMPOSITE BLANK
(BASE/NEUTRAL)
COMPOSITE BLANK
(ACID)
COMPOSITE BLANK
(PESTICIDES)
VOA
(Preserved Unpreserved )
\/OA TDID Rl AMW
VvJA 1 Kir DLrMNrx
N/A
f\l/A
Use section below to describe QA/QC samples if received.
QA/QC EXTRACTABLE
(BASE/NEUTRAL)
QA/QC EXTRACTABLE
(ACID)
QA/QC EXTRACTABLE
(PESTICIDES)
QA/QC VOA
(Preserved Unpreserved )
QA/QC EXTRACTABLE
(BASE/NEUTRAL)
QA/QC EXTRACTABLE
(ACID)
QA/QC EXTRACTABLE
(PESTICIDES)
QA/QC VOA
(Preserved Unpreserved )
K 1 / A
N/A
N/A
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- ITD SAMPLE CONTROL CENTER COPY
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ATTACHMENT 5
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RUN DATE : 01/08/87
ISOTOPE DILUTION EPISODE/SAMPLE REPORT
PAGE : 175
PART 2 : EPISODE/SAMPLE
EPISODE SAMPLE
NUMBER NUMBER
TYPE
TYPE DESCRIPTION
SITE SITE DESCRIPTION
LAB ID LAB NAME
NO OF
SAMPLES
1061
01
15056 EP EPA SAMPLE
COMMENT 1 : S376 BRINE
SAMPLE DATE : 062066
PM : 06.000
15056 TB VOA TRIP BLANK
SAMPLE DATE : 062086
PH 2 00.000
(INF)-UNTREATED EFF
(OTH)-OTHER
ACTUAL SAMPLE COUNT :
1062
I
M
00
15057 EP EPA SAMPLE
COMMENT 1 : S380 PIT CONTENTS
SAMPLE DATE > 062366
PH : 07.000
15057 TB VOA TRIP BLANK
SAMPLE DATE : 062366
15056 EP EPA SAMPLE
COMMENT 1 : S360 PIT CONTENTS
COMMENT 2 : 3302 SLUDGE
SAMPLE DATE : 062366
PH : 07.000
02
(OTHI-OTHER
(OTH)-OTHER
(OTHI-OTHER
1063
ACTUAL SAMPLE COUNT :
15059 EP EPA SAMPLE
COMMENT 1 > S376 BRINE
SAMPLE DATE : 062466
PH : 07.000
15059 TB VOA TRIP BLANK
SAMPLE DATE : 062466
01
(SUP)-RAM HATER (SU
(OTH)-OTHER
1064
15060
ACTUAL SAMPLE COUNT :
02
1PLE
COMMENT 1E?* !§BO" PIT CONTENTS
(OTH)-OTHER
-------
ATTACHMENT 6
E-29
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ITD DATA ELEMENT DICTIONARY
NOTE: Pay special attention to the Concentration/Dilution Factor
E-30 10/28/86
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ITD Data Element Dictionary
Following is a brief description of each data element which is to be stored in the
ITD data base. The originating source for the data element is also given. The
complete specification for each data element and an example of its use are given on a
separate page following this summary.
Amount The quantitative measurement of the compound determined by GC or
GC/MS analysis. The amount is computed for the compound using the referenced
internal standard or isotopic diluent and is multiplied by the concentration or
dilution factor to yield final solution concentrations in ug/L.
Amount (Library) The reference amount in the standard and the amount on
which quantitation is based.
Bottle Number A numeric code which uniquely identifies the bottles used for a
particular sample.
Carrier Gas Flow Rate The volumetric (volume/time) rate of flow of the
carrier gas in the gas chromatograph, or the linear gas velocity (distance/time)
when a capillary column is used.
Column Final Hold The final temperature of the gas chromatograph column
and the length of time that it was held.
Column Initial Hold The initial temperature of the gas chromatograph column
and the length of time that it was held.
Column Inside Diameter The internal diameter of the gas chromatograph
column.
Column Length The length of the gas chromatograph column.
E~31 10/28/86
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Column Temperature Program The change in column temperature with respect
to time giving the initial and final column temperatures.
Compound Comment Code A coded value for any optional text that may be
associated with each compound.
Compound Name The name of the compound determined. The compound name
corresponds to the EGD compound number, as given in the "Industrial Technology
Division Compound Code Listing."
Compound Number A numerical code which uniquely identifies each unique
chemical compound, as given in the "Industrial Technology Division Compound
Code Listing."
Compound Order Number A numerical code that establishes the order of
compound determination by the GC/MS. The code is used on the Quantitation
Report to match segments of the compound data within the report.
Compound Type A coded value which identifies a chemical compound as a
priority pollutant (P), or surrogate (S), internal standard (I), or isotopic dilutent
(D).
Concentration/Dilution Factor The ratio of the volume of sample extracted or
diluted to the volume analyzed.
Date Analyzed The date that the sample fraction was analyzed by the
laboratory.
Date Extracted The date that the laboratory extracted the sample for analysis.
Date Sam pled The date the sample was taken by the field sampler.
Episode Comment Code A coded value for comments associated with an
episode.
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10/28/86
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Episode Number The SCC assigned identification code with designates the
specific sampling trip.
Fraction A coded value which designates the compound as either an acid,
base/neutral, volatile, pesticide or dioxin.
Fraction Comment Code A coded value for any optional text that may be
associated with each fraction.
Industrial Category Code The classification of the industrial processes per-
formed by the plant where a sample was taken.
Instrument A coded value assigned by the laboratory that uniquely identifies
each GC/MS instrument within a laboratory. All Calibration, Precision and
Recovery, Standards and Blank Quantitation files will be tracked by this
instrument number within Laboratory. Changing of this instrument number by
the laboratory would necessitate the submittal of new calibration and other
initial QA runs by the laboratory.
Laboratory A numerical code used to identify the specific laboratory where
the sample was analyzed.
Mass to Charge Ratio Designates the quantitation ion. Abreviated as M/Z or
M/E.
Method A coded value which uniquely identifies the method protocol that was
followed during analysis.
Peak Area The area beneath the peak of a mass chromatogram. The peak area
is proportional to the amount of the detected compound at an observed mass to
charge ratio. It is used to compute the concentration of the compound present in
the sample.
PH Level The negative logarithm of the effective hydrogen ion concentration
as expressed in grain equivalents per liter.
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Plant Code A numerical code used to distinguish specific plants which have
been sampled.
Proprietary Indicator A coded value which designates whether or not the
analysis data from a sample is proprietary. Also indicates that confidentiality
papers have been signed.
Quantitation Report Type A coded value that uniquely identifies the particular
type of quantitation report that is being submitted;
Reference Compound A numeric code that is used as a pointer to the internal
standard or isotopic diluent within a quantitation report.
Relative Retention Time The quotient of the retention time of a compound
divided by its internal standard or isotopic diluent.
Relative Retention Time (Library) The relative retention time stored in the
library. The value is based on the analysis of a standard containing both
compounds.
Response Factor The ratio between the response for the sample and a response
for a standard under identical analytical conditions.
Response Factor (Library) The response factor stored in the library. The value
is determined from analysis of a standard.
Retention Time The time it takes the identified compound to eiute from the
gas chromatograph.
Retention Time (Library) The known time it takes an identified compound to
elute from the gas chromatograph. The time is determined from analysis of a
standard.
Sample Comment Code A coded value for any optional text that may be
associated with each sam pie.
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Sample Number The SCC assigned identification code which identifies the indi-
vidual samples.
Sample Point (Site) The specific point within an industrial wastestream where
a sample was taken.
Sample Point Flow The flow rate at the point at which the sample was taken.
Value is recorded from a flow meter or other flow measuring device.
Sample Type A coded value which describes the type of sample.
Scan Number Gives the scan at which the compound was detected by the mass
spectrometer.
Shift The scheduled period of operation of the GC/MS instrument. Operation
is divided into three shifts/day.
Time Analyzed The time that the sample fraction was analyzed by the
laboratory.
Unit of Measure The unit of measurement for the amount.
The following chart shows the source of each data element.
E-35 10/28/86
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SUMMARY OF DATA SOURCES FOR COLLECTION
OF ORGANIC PRIORITY POLLUTANT DATA
COLLECTION SOURCE
. TR2 LAB3
DATA FIELD SAMTRAC1 LC TAPE GENERATED
Amount X
Amount (Library) X
Bottle Number X
Carrier Gas Flow Rate X
Column Final Hold X
Column Initial Hold X
Column Inside Diameter X
Column Length X
Column Temperature Program X
Compound Comment Code X
Compound Name X
Compound Number X
Compound Reference Number X
Compound Type X
Concentration/Dilution Factor X
Date Analyzed X
Date Extracted X
Date Sam pled X
Episode Comment Codes X
Episode Number X
Fraction X
Fraction Comment Code X
Industrial Category Code X
Instrument X
Laboratory X
(1) SAMTRAC - Computerized logistics system at the Sample Control Center.
(2) TR LC - Traffic Reports and Lab Chronicles.
(3) Quantitation Reports on magnetic tape received from analytical laboratories.
E-36 10/28/86
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SUMMARY OF DATA SOURCES FOR COLLECTION
OF ORGANIC PRIORITY POLLUTANT DATA
COLLECTION SOURCE
DATA FIELD
SAMTRAC1 LC TAPE
GENERATED
Mass to Charge Ratio
Method
Peak Area
PH Level
Plant Code
Proprietary Indicator
Quantitation Report Type
Reference Compound
Relative Retention Time
Relative Retention Time (Library)
Response Factor
Response Factor (Library)
Retention Time
Retention Time (Library)
Sample Comment Code
Sample Number
Sample Point (Site)
Sample Point Flow
Sample Type
Scan Number
Shift
Time Analyzed
Unit of Measure
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
(1) SAMTRAC - Computerized logistics system at the Sample Control Center.
(2) TR LC - Traffic Reports and Lab Chronicles.
(3) Quantitation Reports on magnetic tape received from analytical laboratories.
E-37
10/23/36
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NOTES ON TYPE/LENGTH DESCRIPTION
The Type/Length Description for each EGD Data Element represents how each
data field is stored internally in the computer or how each data field is represented on
the quantitation report.
TYPES:
Z
9
X
V
Numeric data only - leading zeroes not printed.
Numeric data only - zeroes printed.
Alpha numeric data.
Implied decimal point.
Explicit decimal point.
LENGTH:
(N) Where N is a positive integer value from 1 to 255, gives the number of data
positions allocated internally by the computer to store this portion of the
data field.
EXAMPLES:
Example 1. 9(7)V9(3)
9
(7)+(3)
V
Numeric data.
10 data positions allocated.
Implied decimal point after 3rd position from the right.
Can also be expressed as 9999999V999.
The number 1,130.31 would be stored internally under this Type/Length des-
cription as:
'0001130310'
E-38
10/23/S6
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NOTES ON TYPE/LENGTH DESCRIPTION (CONT.)
The computer program would also know that there is a decimal point implied
between '0001130' and '310'.
Example 2. X(6)
X - Alphanumeric data.
(6) - 6 data positions allocated.
Can also be expressed as XXXX.
The field 'EPAi' would be stored internally or printed as:
'EPA1'
Example 3. ZZZZZZ9.999
Z - Numeric data - zeroes not printed.
9 - Numeric data - zeroes printed.
Explicit decimial point printed.
6 (Z's) + tf. (9«s) + 1 (.) = 11 data positions allowed.
The field '0000023010' would be printed as:
1 23.010'
E-39 10/28/86
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ELEMENT NAME: AMOUNT
Definition: The quantitative measurement of the compound determined by GC or
GC/MS analysis. The amount is computed for the compound using the referenced
internal standard or isotopic diluent and is multiplied by the concentration or dilution
factor to yield final solution concentration in ug/L.
Input Type/Length
Quantitation Report ZZZZZ9.999
As Stored Internally 9(7)V9(3)
Unit of Measure
Ug/L
Edit Criteria:
Range: 10.000-999,999.999 ug/L
Exam pies:
Volatiles: Concentration (AMOUNT) is reported on the quantitation report in
uG/L. If the sample is diluted to bring a pollutant within the analytical range of
the instrument, the AMOUNT is multiplied by the concentration/dilution factor
(see CONCENTRATION/DILUTION FACTOR).
Semi-volatiles: Concentration (AMOUNT) is reported on the quantitation report
in uG/ML. If the sample or extract is diluted to bring a pollutant within the
analytical range of the instrument, the AMOUNT is multiplied by the concentra-
tion/dilution factor (see CONCENTRATION/DILUTION FACTOR).
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ELEMENT NAME: AMOUNT (LIBRARY)
Definition: The reference amount in the standard and the amount on which quanti-
tation is based.
Input Type/Length
Quantitation Report ZZZZZ9.99
As Stored Internally 9(7)V9(3)
Unit of Measure
The amount is reported as a pure number but must always be accompanied by a
UNIT. See UNIT.
Edit Criteria:
Range: 1.000 - 1000.000 ug/L
Examples: See AMOUNT.
E~41 10/28/86
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ELEMENT NAME: BOTTLE NUMBER
Definition: A numeric code which uniquely identifies the bottles used for a particular
sample. Used as a suffix to the SAMPLE NUMBER.
Input Type/Length
Quantitation Report X(2)
As Stored Internally X(2)
Unit of Measure
Each.
Edit Criteria:
Range: 01-98 for EPA Samples
99 for the TCLP Leachate of an EPA Sample
00 for all Others
Example: See SAMPLE NUMBER.
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ELEMENT NAME: CARRIER GAS FLOW RATE
Definition: The volumetric (volume/time) rate of flow of the carrier gas in the gas
chromatograph for packed columns, or the linear gas velocity (distance/time) for
capillary columns.
Input Type/Length
Quantitation Report X(9)
As Stored Internally X(9)
Unit of Measure
Volatiles (packed column): ML/Min
Semi-vola tiles (capillary column): CM/Sec
Edit Criteria:
Ranges: Voiatiles: 20-40 mL/min; Semi Volatiles: 20-60 cm/sec;
Dioxin: 20-60 cm/sec
E_43 10/28/86
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ELEMENT NAME: COLUMN FINAL HOLD
Definition: The final temperature of the gas chromatograph column and the length of
time that it was held.
Input Type/Length
Quantitation Report X(7)
As Stored Internally X(7)
Unit of Measure
Time: minutes
Temperature: degrees Celsius
Units are understood and not reported.
Edit Criteria:
1. Format: Hold @ temperature ie XXX@XXX
2. Hold Ranges: Volatiles: 0-20 min; Semi Volatiles: 10-20 min; Dioxin: 10-30min
3. Temperature Ranges: Volatiles: 200-250°C; Semi Volatiles: 240-290°C; Dioxin:
200-300°C
Example: 15 Q 280 means that the column was held for 15 minutes.
E-44 10/28/86
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ELEMENT NAME: COLUMN INITIAL HOLD
Definition: The initial temperature of the gas chromatograph column and the length
of time that it was held.
Input Type/Length
Quantitation Report X(7)
As Stored Internally X(7)
Unit of Measure
Time: minutes
Temperature: degrees Celsius
Units are understood and not reported.
Edit Criteria:
1. Format: Hold @ Temp ie XXX@XXX
2. Hold Ranges: Volatiles: 2-4 min; Semi Volatiles: 4-6 min; Dioxin: 0-10 min
3. Temperature Ranges: Volatiles: 25-50°C; Semi Volatiies: 25-35°C; Dioxin: 50-
200°C
Example: 4 (3 30 means that the column was held for 4 minutes at 30°C.
E_45 10/28/86
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ELEMENT NAME: COLUMN INSIDE DIAMETER
Definition: The internal diameter of the gas chromatograph column.
Input Type/Length
Quantitation Report X(6)
As Stored Internally X(6)
Unit of Measure
Millimeter (MM)
Edit Criteria:
Ranges: Volatiies: l-3mm; Semi-Voiatiles: 0.2-0.35 mm;
Dioxin: 0.2-0.35 mm
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ELEMENT NAME: COLUMN LENGTH
Definition: The length of the gas chromatograph column.
Input Type/Length
Quantitation Report X(6)
As Stored Internally X(6)
Unit of Measure
Meters (M)
Edit Criteria:
Ranges: Volatiles: 2.8-3.1 m; Semi-Volatiles: 25-35 m;
Dioxin: 25-65 m
E~47 10/28/86
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ELEMENT NAME: COLUMN TEMPERATURE PROGRAM
Definition: The change in column temperature with respect to time giving the initial
and final column temperatures.
Input Type/Length
Quantitation Report X(iO)
As Stored Internally X(10)
Unit of Measure
Initial temperature: degrees Celsius
Final temperature: degrees Celsius
Rate: degrees Celsius per minute
Units are understood and not reported.
Edit Criteria:
1. Format: Initial Temp - Final Temp (3 Temp Program rate ie XXX-XXX (3 XX
2. Range: 1.5-8.5°C/min
Exam pies:
45-220 @ 8
30-280 <§ 8
10/28/86
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ELEMENT NAME:
COMPOUND COMMENT CODE
Definition: A coded value for any optional text that may be associated with each
compound.
Input
Traffic Report
Laboratory Chronicles
As Stored Internally
Unit of Measure
N/A
Edit Criteria:
Range C001-C999.
Type/Length
X(*)
E-49
10/28/86
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ELEMENT NAME: COMPOUND NAME
Definition: The name of the compound determined. The compound name corresponds
to the EGD compound number.
Input Type/Length
Quantitation Report X(30)
As Stored Internally X(30)
Unit of Measure
N/A
Edit Criteria:
See ITD Compound Code Table, attached as Table 4, for valid names.
Exam pies:
BROMOFORM
1,2-DICHL ORB ENZ ENE-D4
E-50 10/28/86
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ELEMENT NAME: COMPOUND NUMBER
Definition: A numerical code which uniquely identifies each unique chemical com-
pound.
Input Type/Length
Quantitation Report 9(3)
As Stored Internally 9(3)
Unit of Measure
N/A
Edit Criteria:
Must be one of the following codes:
001-129 = Priority Pollutants quantitated by internal standard.
130-199 = Miscellaneous surrogates and internal standards.
200-299 = Priority Pollutant labeled compounds (isotopes) quantitated by
internal standard.
300-399 = Priority Pollutants quantitated by isotope dilution.
WO-429 = Labeled compounds (isotopes) quantitated by internal standard.
500-599 = Non-Priority Pollutant compounds quantitated by internal
standard.
600-699 = Syn Fuel specific and Appendix C labeled compounds (isotopes)
quantitated by internal standard.
700-799 = Syn Fuel specific and Appendix C compounds quantitated by
isotope dilution.
800-829 = Pollutants 100-129 quantitated by isotope dilution.
900-999 = Non-Priority Pollutant Compounds Quantitated by Internal
standard.
See ITD Compound Code Table, attached as Table 4.
E-51 10/28/86
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ELEMENT NAME: COMPOUND ORDER NUMBER
Definition: A numerical code that establishes the order of compound determination
by the GC/MS. The code is used on the Quantitation Report to match the segments of
compound data within the report.
Input Type/Length
Quantitation Report 9(3)
As Stored Internally 9(3)
Unit of Measure
N/A
Edit Criteria:
Range: 001-250
E-52 10/28/86
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ELEMENT NAME:
COMPOUND TYPE
Definition: A coded value which identifies a chemical compound as a priority
pollutant or surrogate.
Input
Generated Based on Compound Number
As Stored Internally
Unit of Measure
N/A
Edit Criteria:
Type/Length
Must be one of the following codes:
CODE
VALUE
D
I
P
S
Isotopic Diluent
Internal Standard
Priority Pollutant
Surrogate
E-53
10/28/86
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ELEMENT NAME: CONCENTRATION/DILUTION FACTOR
Definition: The concentration or dilution ratio of the sample fraction or spike before
analysis.
Input Type/Length
Quantitation Report X(ll)
As Stored Internally 9O)V9<5)
Unit of Measure
Pure number.
Edit Criteria:
Format: two numbers separated by a colon, the first is the pre-extracti on/dilution
amount; the second is the post extraction/dilution amount, e.g., XXXXX:XXXXX.
These numbers are used to form the concentration/dilution ratio (CDR); the number to
the left of the colon becomes the numerator, and the number to the right of the colon
becomes the denominator.
Examples: 1000:1 means that an initial iOOOmL volume of sample was concentrated to
1 mL extract (semi-volatiles); 1:100 means that an inital volume of sample was diluted
with 99 parts of reagent water (volatiles).
Semi-Voiatiles: When a semi-voiatiles fraction (acid or base/neutral) is extracted, the
normal volume of sample is 1 liter (1000 mL). The extract is normally concentrated to
a volume of 1.0 mL. The units on the quantitiation report for semi-volatiles is
UG/ML. Multiplying these units by 1000 mL/L, and dividing the concentration/dilution
ration (CDR) (1000/1) yields the final concentration in the water in ug/L, as given in
the following equation:
Csam (ug/L) = Cext (ug/mL) x 1000 (mL/L) / CDR
E-54 10/28/86
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ELEMENT NAME: CONCENTRATION/DILUTION FACTOR (Continued)
Edit Criteria (continued):
For example, for a 1.0 mL extract containing 67 ug/mL of a pollutant which was
extracted from a 1000 mL water sample:
Csam (ug/mL) = 67 ug/mL x 1000 mL/L / 1000 = 67 ug/L
When a sample volume other than 1000 mL is extracted, the volume is given on the
left hand side of the colon in the concentration/dilution factor. For example, for the
"dilute aliquot" in Method 1625A which employs a 10 mL volume of sample and yields 1
mL of extract, the concentration/dilution factor would be: 10:1, and the CDR would
be 10.
Similarly, when an extract is diluted, the dilute volume is given on the right hand side
of the colon in the concentration/dilution factor. For example, for a 1 1000 mL
sample which yields a final extract volume of 1.0 mL which is then diluted by a factor
of 10, the concentration/dilution factor would be 1000:10, and the CDR would become
1000/10, or 100. Extract volumes other than multiples of 10 of the 1.0 mL extract
volume are prohibited.
For semi-volatiles, the 2,2'-difluorobiphenyl internal standard concentration remains
constant at 100 ug/mL in the extract, regardless of the level of dilution.
Computations of pollutant and labeled compound concentrations become complicated
when the initial volume of sample is other than 1000 mL or 1000 divided by some
multiple of 10, and even more complicated when the final extract volume is not
exactly 1.0, but is close to 1.0 mL (e.g., in the range of 0.5 to 2.0 mL). These
situations are dealt with as follows:
1. When the sample volume is not 1000 mL, but is adjusted to 1000 mL prior
to spike of the labeled compounds and extraction, the concentration for
each pollutant will be (see note below!) adjusted by the CDR, but the final
concentration for the labeled compounds will not be adjusted.
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ELEMENT NAME: CONCENTRATION/DILUTION FACTOR (Continued)
Edit Criteria (continued):
2. When the final extract volume is not exactly 1.0 mL, the concentration for
each pollutant determined by isotope dilution will not be (see note below!)
adjusted by the right hand portion of the concentration/dilution factor
(since the labeled compound compensates the pollutant recovery), but the
concentration (and therefore the recovery) of each labeled compound and
each pollutant with no labeled analog will be adjusted by the right hand
portion of the concentration/dilution factor. Extract volumes of less than
0.5 and in the range of 2.0 to 9.9 mL are prohibited.
NOTE: The adjustments referenced above will be made by the EPA computer after
data are received. In order to minimize the workload for the laboratories, no
adjustments to concentrations are to be made by the laboratories. However, it is
imperative that the 2.2'-difluorobiphenyl concentration be 100 ug/mL in the extract
(as is required by Method 1625), that the compound numbers be correct (so that the
quantitation method, i.e., isotope dilution or internal standard can be identified), and
that the initial volume of sample and final volume of extract be stated correctly in the
concentration/dilution factor, so that the final concentration in the water is computed
properly using the information above. If you are confused by all of this, the simplest
way to avoid these issues is to always use 1000 mL of sample, always concentrate to
1.0 mL, and always spike the 2,2'-difluorobiphenyl such that its concentration in the
extract will be 100 ug/mL.
Finally, the amount of each labeled compound in the water which is extracted shall be
100 ug only. Other amounts are prohibited. This requirement recognizes that the
"sample" may not always be 1000 mL (e.g., the dilute aliquot), but that the water in
the extractor will yield an extract with concentrations of the labeled compounds
identical to those in the precision and recovery standards.
Voiatiles: For volatiles, the labeled compounds and internal standards are spiked into
the 5 mL water sample at each level of dilution. Therefore, the computation of
concentration is applied to the pollutants only (not to the labeled compounds or
internal standards).
E-56 10/28/86
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ELEMENT NAME: CONCENTRATION/DILUTION FACTOR (Continued)
Edit Criteria (continued):
In a way analogous to that for semi-voiatiles, the final concentration of a pollutant in
a sample can be expressed as follows:
Csam (ug/L) = Cdil samp (ug/L) / CDR
For example, for a sample which has been diluted by a factor of 10 with reagent water
and contains 48 ug/L at the dilute level, the concentration/dilution factor is 1:10 and
the CDR is 1/10 or 0.1.
Csam (ug/L) = 48 ug/L / 0.1 = 480 ug/L
NOTE: The "concentration/dilution factor" format was developed to permit use of the
same "units" on quantitation reports, regardless of how much the sample is concen-
trated or diluted. Alternate methods require changing the units depending on the
amount of the dilution.
E-57
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ELEMENT NAME: DATE ANALYZED
Definition: The date that the sample fraction was analyzed by the laboratory.
Input Type/Length
Quantitation Report X(8)
As Stored Internally X(8)
Unit of Measure
N/A
Edit Criteria:
Format: MM/DD/YY, where MM is the month; DD is the day; and YY is the last
two digits of the Gregorian calendar year.
Example: 07/15/83 is July 15, 1983.
E_58 10/28/86
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ELEMENT NAME: DATE EXTRACTED
Definition: The date that the laboratory extracted the sample for analysis.
Input Type/Length
Quantitation Report X(8)
As Stored Internally X(8)
Unit of Measure
N/A
Edit Criteria:
Format: MM/DD/YY, where MM is the month; DD is the day; and YY is the last
two digits of the Gregorian calendar year.
Example: 07/15/83 is July 15, 1983.
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ELEMENT NAME: DATE SAMPLED
Definition: The date the sample was taken by the field sampler.
Input Type/Length
Traffic Report X(8)
As Stored Internally X(8)
Unit of Measure
N/A
Edit Criteria:
Format: MM/DD/YY, where MM is the month; DD is the day; and YY is the last
two digits of the Gregorian calendar year.
Example: 07/15/83 is July 15, 1983.
E-60 10/28/86
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ELEMENT NAME:
EPISODE COMMENT CODE
Definition: A coded value for comments associated with an episode.
Input
Traffic Reports
Laboratory Chronicles
As Stored Internally
Unit of Measure
N/A
Edit Criteria:
Range E001-E999.
Type/Length
E-61
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ELEMENT NAME: EPISODE NUMBER
Definition: The SCC assigned identification code designating the sampling trip.
Input
SAMTRAC
As Stored Internally
Unit of Measure
N/A
Edit Criteria:
1. Numeric
2. Greater than 0119.
Type/Length
E-62
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ELEMENT NAME:
FRACTION
Definition: A coded value which designates the compound as either an acid,
base/neutral, volatile, pesticide or dioxin.
Input
Priority Pollutant Data Sheet
QA/QC Sheet
As Stored Internally
Unit of Measure
N/A
Edit Criteria:
Type/Length
Must be one of the following codes:
CODE
A
B
C
D
P
V
VALUE
Acid Compound
Base/Neutral Compound
Combined Acid Base/Neutral
Dioxin
Pesticide Compound
Volatile Compound
E-63
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ELEMENT NAME:
FRACTION COMMENT CODE
Definition: A coded value for any optional text that may be associated with each
fraction.
Input
Traffic Report/Lab Chronicles
Priority Pollutant Data Sheet
As Stored Internally
Type/Length
Unit of Measure
N/A
Edit Criteria:
Range F001-F999.
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ELEMENT NAME: INDUSTRIAL CATEGORY CODE
Definition: The classification of the industrial processes performed by the plant
where a sample was taken.
Input Type/Length
SAMTRAC 9(3)
As Stored Internally 9(3)
Unit of Measure
N/A
Edit Criteria:
Must be a valid code in the Industrial Category Code Table.
E-65
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ELEMENT NAME: INSTRUMENT
Definition: A coded value assigned by the laboratory that uniquely identifies each
GC/MS instrument within a laboratory. All Calibration, Precision and Recovery,
Standards and Blank Quantitation files will be tracked by this instrument member
within Laboratory. Changing of this instrument number by the laboratory would
necessitate the submittal of new calibration and other initial quantitation runs by the
laboratory.
Input Type/Length
Quantitation Report X(2)
As Stored Internally X(2)
Unit of Measure
N/A
Edit Criteria:
Range: 01-99, AA-ZZ or any two character combination.
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ELEMENT NAME: LABORATORY
Definition: A numerical code used to identify the specific laboratory where the
sample was analyzed.
Input Type/Length
SAMTRAC 9(3)
As Stored Internally 9(3)
Unit of Measure
N/A
Edit Criteria:
Must be a valid code in the Laboratory Code Table.
10/28/86
E-67
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ELEMENT NAME: MASS TO CHARGE RATIO
Definitions Designates the quantitation ion. Abbreviated as M/Z, or M/E.
Input Type/Length
Quantitation Report ZZZ9
As Stored Internally 9(4)
Unit of Measure
N/A
Edit Criteria:
Ranges: Volatiles: 20-250; Semi-Volatiles: 35-450; Dioxin (Selected Ion
Monitoring): 257, 320, 322, 323, 328, 332, and 334.
E-68 10/23/86
-------
ELEMENT NAME: METHOD
Definition: A coded value which uniquely identifies the method protocol that was
followed during analysis.
Input Type/Length
Quantitation Report X(5)
As Stored Internally X(5)
Unit of Measure
N/A
Edit Criteria:
Acceptable Codes:
162* A
1625A
162*5
1625B
162*C
1625C
163*
1635
613
613E
713
E-69 10/28/86
-------
ELEMENT NAME: PEAK AREA
Definition: The area beneath the peak of a mass chromatogram. The peak area is
proportional to the amount of the detected compound at an observed mass to charge
ratio. It is used to compute the concentration of the compound present in the sample.
Input Type/Length
Quantitation Report ZZZZZZZZZZ9.
As Stored Internally 9(10)
Unit of Measure
N/A
Edit Criteria:
E-70 10/28/86
-------
ELEMENT NAME:
PH LEVEL
Definition: The negative logarithm of the effective hydrogen ion concentration as
expressed in grain equivalents per liter.
Input
Traffic Report
As Stored Internally
Unit of Measure
N/A
Edit Criteria:
Type/Length
Z9.999
9(2)V9(3)
E-71
10/28/86
-------
ELEMENT NAME: PLANT CODE
Definition: A numeric code used to distinguish specific industrial plants which have
been sampled.
Input Type/Length
SAMTRAC 9(4)
As Stored Internally 9(4)
Unit of Measure
N/A
Edit Criteria:
Must be a four digit number.
Comment:
1. Plant ID'S are unique within the isotope dilution program.
2. The episode number for the first occurrence of a plant visit is used as the plant's
identification number.
E_72 10/28/86
-------
ELEMENT NAME: PROPRIETARY INDICATOR
Definition: A coded value which designates whether or not the analysis data from a
sample is proprietary. Also indicates that confidentiality papers have been signed.
Input
Traffic Report
Lab Chronicles
As Stored Internally
Unit of Measure
Type/Length
N/A
Edit Criteria:
Must be one of the following codes:
CODE
VALUE
P
N
Proprietary
Not Proprietary
E-73
10/28/86
-------
ELEMENT NAME:
QUANTITATION REPORT TYPE
Definition: A coded value that uniquely identifies the particular type of quantitation
report that is being submitted.
Input
Quantitation Report
As Stored Internally
Type/Length
X(3)
X(3)
Unit of Measure
N/A
Edit Criteria:
CODE
VALUE
BLK
CAL
EPA
FBK
VER
IPR
OPR
1
Laboratory Blank
Calibration
EPA Sample
Field Blank
Calibration Verification for Extraction Methods
Initial Precision and Accuracy
Ongoing Precision and Accuracy
For volatiles, calibration verification and ongoing precision and accuracy tests are
performed using the OPR report.
E-74
10/2S/86
-------
ELEMENT NAME: REFERENCE COMPOUND
Definition: A numeric code that is used as a pointer to the internal standard or
isotopic diluent within a quantitation report.
Input
Quantitation Report
As Stored Internally
Unit of Measure
N/A
Edit Criteria:
Range: 001-250
Type/Length
ZZ9
9(3)
E-75
10/28/86
-------
ELEMENT NAME:
RELATIVE RETENTION TIME
Definition: The quotient of the retention time of a compound divided by its internal
standard or isotopic diluent.
Input
Quantitation Report
As Stored Internally
Unit of Measure
N/A
Edit Criteria:
Type/Length
Z9.999
99V9O)
E-76
10/28/86
-------
ELEMENT NAME:
RELATIVE RETENTION TIME (LIBRARY)
Definition: The relative retention time stored in the library. The value is based on
the analysis of a standard containing both compounds.
Input
Type/Length
Quantitation Report
As Stored Internally
Z9.999
9(2)V9(3)
Unit of Measure
N/A
Edit Criteria:
E-77
10/28/86
-------
ELEMENT NAME: RESPONSE FACTOR
Definition: The ratio between the response for the sample and a response for a
standard under identical analytical conditions. Computed per the following equation:
RF = ASCIS
where
Aj is the PEAK AREA for the compound from analysis of a standard.
Aj_ is the PEAK AREA for the internal standard.
C.c is the concentration of the internal standard.
C,. is the concentration of the compound.
Input Type/Length
Quantitation Report ZZZ9.99
As Stored Internally 9(4)V9(3)
Unit of Measure
N/A
Edit Criteria:
E_78 10/28/S6
-------
ELEMENT NAME: RESPONSE FACTOR (LIBRARY)
Definition: The response factor stored in the library. The value is determined from
analysis of a standard.
Input
Quantitation Report
As Stored Internally
Unit of Measure
N/A
Edit Criteria:
Example: See RESPONSE FACTOR.
Type/Length
ZZZ9.999
9(»)V9(3)
E-79
10/28/86
-------
ELEMENT NAME: RETENTION TIME
Definition: The time it takes the identified compound to elute from the gas
chromatograph.
Input Type/Length
Quantitation Report X(S)
As Stored Internally X(8)
Unit of Measure
N/A
Edit Criteria:
Format: HH:.MM:SS
MM-.5S
SS
Where HH is hours; MM is minutes; S3 is seconds.
E-80 10/23/86
-------
ELEMENT NAME: RETENTION TIME (LIBRARY)
Definition: The known time it takes an identified compound to elute from the gas
chromatograph. The time is determined from analysis of a standard.
Input Type/Length
Quantitation Report X(8)
As Stored Internally X(8)
Unit of Measure
N/A
Edit Criteria:
Format: HH:MM:SS
MM:SS
SS
Where HH is hours; MM is minutes; SS is seconds.
E-81 10/28/86
-------
ELEMENT NAME: SAMPLE COMMENT CODE
Definition: A coded value for any optional text that may be associated with each
sample.
Input
Traffic Reports
Lab Chronicles
As Stored Internally
Unit of Measure
N/A
Edit Criteria:
Range S001-S999.
Type/Length
X(4)
E-82
10/28/36
-------
ELEMENT NAME: SAMPLE NUMBER
Definition: The SCC assigned identification code which identifies the individual
samples. For calibration and performance standards, is used to indicate the nominal
concentration of the standard.
Input Type/Length
Quantitation Report ZZ999
As Stored Internally 9(5)
Unit of Measure
N/A
Edit Criteria:
a. Must be a five digit number.
b. Range: 00001-99999
Examples: 00100 accompanied by a QUANTITATION REPORT TYPE of VER would
define a Calibration Verification standard at a nominal concentration of 100 ug/mL (or
100 ug/L for volatiles).
E-83 10/28/86
-------
ELEMENT NAME:
SAMPLE POINT FLOW
Definition: The flow rate at the point at which the sample was taken. Value is
i
recorded from a flow meter or other flow measuring device.
Input
Traffic Report
As Stored Internally
Unit of Measure
Per 1,000 gallons/day.
Edit Criteria:
Type/Length
X(5)
E-84
10/2S/86
-------
ELEMENT NAME: SAMPLE POINT (SITE)
Definition: The specific point within an industrial wastestream where a sample was
taken.
Input Type/Length
Traffic Report X(l)
Lab Chronicles
As Stored Internally X(l)
Unit of Measure
N/A
Edit Criteria:
Must be a valid code in the Sample Site Table.
E-85 10/28/86
-------
ELEMENT NAME: SAMPLE TYPE
Definition: A coded value which describes the type of sample.
^P"t Type/Length
Traffic Report X(2)
As Stored Internally X(2)
Unit of Measure
N/A
Edit Criteria:
Must be a valid code in the Sample Type Code Table.
E-86 10/2S/86
-------
ELEMENT NAME: SCAN NUMBER
Definition: Gives the scan at which the compound was detected by the mass
spectrometer.
Input Type/Length
Quantitation Report ZZ999
As Stored Internaliy 9(5)
Unit of Measure
N/A
Edit Criteria:
Range: 00001-99999
E-87 10/28/86
-------
ELEMENT NAME: SHIFT
Definition: The scheduled period of operation of the GC/M5 instrument. Operation
is divided into three shifts/day.
Input
Quantitation Report
As Stored Internally
Type/Length
Unit of Measure
N/A
Edit Criteria:
Code Meaning
G Graveyard (0000-0759; Midnight to 3 AM)
D Day (0800 - 1559; 8 AM to 4 PM)
S Swing (1600 - 1159; * PM to Midnight)
10/28/86
-------
ELEMENT NAME: TIME ANALYZED
Definition: The time thtat the sample fraction was analyzed by the laboratory.
Input
Quantitation Report
As Stored Internally
Unit of Measure
N/A
Edit Criteria:
Format: HH:MM:SS
Type/Length
X(8)
X(8)
E-89
10/28/86
-------
ELEMENT NAME:
UNIT OF MEASURE
Definition: The unit of measurement for the amount, as measured in the nominal
sam pie.
Input
Quantitation Report
As Stored Internally
Unit of Measure
Volatiles: UG/L
Semi Volatiles: UG/ml
Dioxin: NG/ML
Edit Criteria:
UG/L
UG/ML
NG/ML
Type/Length
X(5)
X(5)
E-90
10/28/86
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
001
002
003
004
005
006
007
008
009
010
Oil
012
013
014
015
016
017
018
019
020
021
022
023
024
025
026
027
028
029
030
031
032
033
034
035
036
037
038
039
040
041
042
043
044
045
046
047
043
049
050
B ACENAPHTHENE
V ACROLEIN
V ACRYLONITRILE
V BENZENE
B BENZIDINE
V CARBON TETRACHLORIDE
V CHLOROBENZENE
B 1,2,4-TRICHLOROBENZENE
B HEXACHLOROBENZENE
V 1,2-DICHLOROETHANE
V 1,1,1-TRICHLOROETHANE
B HEXACHLOROETHANE
V 1,1-DICHLOROETHANE
V 1,1,2-TRICHLOROETHANE
V 1,1,2,2-TETRACHLOROETHANE
V CHLOROETHANE
V BIS (CHLOROMETHYL) ETHER (NR)
B BIS(2-CHLOROETHYL)ETHER
V 2-CHLOROETHYLVINYL ETHER
B 2-CHLORONAPHTHALENE
A 2,4,6-TRICHLOROPHENOL
A 4-CHLORO-3-METHYLPHENOL
V CHLOROFORM
A 2-CHLOROPHENOL
B 1,2-DICHLOROBENZENE
B 1,3-DICHLOROBENZENE
B 1,4-DICHLOROBENZENE
B 3,3'-DICHLOROBENZIDINE
V 1,1-DICHLOROETHENE
V TRANS-1,2-DICHLOROETHENE
A 2,4-DICHLOROPHENOL
V 1,2-DICHLOROPROPANE
V T-1,3-DICHLOROPROPENE
B 2,4-DIMETHYLPHENOL
B 2,4-DINITROTOLUENE
B 2,6-DINITROTOLUENE
B 1,2-DIPHENYLHYDRAZINE
V ETHYLBENZENE
B FLUORANTHENE
B 4-CHLOROPHENYL PHENYL ETHER
B 4-BROMOPHENYL PHENYL ETHER
B BIS (2-CHLOROISOPROPYL) ETHER
B BIS (2-CHLOROETHOXY) METHANE
V METHYLENE CHLORIDE
V CHLOROMETHANE
V BROMOMETHANE
V BROMOFORM
V BROMODICHLOROMETHANE
V TRICHLOROFLUOROMETHANE (NR)
V DICHLORODIFLUOROMETHANE (NR)
P
P
P
P 0154 Y
P 0056 Y
0053 Y
0078 Y
0184 Y
0047 Y
0112 Y
0180 Y
P 0284 Y
P 0062 Y
0097 Y
0201 Y
0063 Y
P 0083 Y
P 0083 Y
0064 Y
Y
0093 Y
0106 Y
0162 Y
0196 Y
0107 Y
0085 Y
0128 Y
0146 Y
0146 Y
0146 Y
0252 Y
0061 Y
0061 Y
0162 Y
0063 Y
0075 Y
P 0122 Y
P 0165 Y
P 0165 Y
P 0077 Y
P 0106
P 0202
P 0204
P 0248
P 0121 Y
P 0093 Y
P 0084 Y
P 0050 Y
P 0096 Y
P 0173 Y
P 0083 Y
P
P
Y
Y
E-91
-------
LO/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
051
052
053
054
055
056
057
058
059
060
061
062
063
064
065
066
067
068
069
070
071
072
073
074
075
076
077
078
079
080
081
082
083
084
085
086
087
088
089
090
091
092
093
094
095
096
097
098
099
100
V DIBROMOCHLOROMETHANE
B HEXACHLORO-1,3-BUTADIENE
B HEXACHLOROCYCLOPENTADIENE
B ISOPHORONE
B NAPHTHALENE
B NITROBENZENE
A 2-NITROPHENOL
A 4-NITROPHENOL
A 2,4-DINITROPHENOL
A 2-METHYL-4,6-DINITROPHENOL
B N-NITROSODIMETHYLAMINE
B N-NITROSODIPHENYLAMINE
B N-NITROSODI-N-PROPYLAMINE
A PENTACHLOROPHENOL
B PHENOL
B BIS (2-ETHYLHEXYL) PHTHALATE
B BUTYL BENZYL PHTHALATE
B DI-N-BUTYL PHTHALATE
B DI-N-OCTYL PHTHALATE
B DIETHYL PHTHALATE
B DIMETHYL PHTHALATE
B BENZO(A)ANTHRACENE
B BENZO(A)PYRENE
B BENZO(B)FLUORANTHENE
B BENZO(K)FLUORANTHENE
B CHRYSENE
B ACENAPHTHYLENE
B ANTHRACENE
B BENZOCGHI)PERYLENE
B FLUORENE
B PHENANTHRENE
B DIBENZO(A,H)ANTHRACENE
B INDENOC1,2,3-CD)PYRENE
B PYRENE
V TETRACHLOROETHENE
V TOLUENE
V TRICHLOROETHENE
V VINYL CHLORIDE
P ALDRIN
P DIELDRIN
P CHLQRDANE
P 4,4*-DDT
P 4,4'-DDE
P 4,4'-DDD
P ALPHA-ENDOSULFAN
P BETA-ENDOSULFAN
P ENDOSULFAN SULFATE
P ENDRIN
P ENDRIN ALDEHYDE
P HEPTACHLOR
P
P
P
P
P
P
P
P
P
P
P
P
P
P
P
P
P
Y
Y
P 0129 Y
P 0225 Y
P 0237 Y
P OOS2
P 0128
0123 Y
0139 Y
P 0139 Y
P 018
-------
10/30/36 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04 .
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
101
102
103
104
105
106
107
108
109
110
111
112
113
129
130
150
151
152
153
154
155
156
157
158
159
160
161
162
163
164
165
166
167
168
169
170
172
173
174
175
176
177
178
179
130
131
182
183
184
135
P HEPTACHLOR EPOXIDE
P ALPHA-BHC
P BETA-BHC
P 6AMMA-BHC
P DELTA-BHC
P PCB-1242
P PCB-1254
P PCB-1221
P PCB-1232
P PCB-1248
P PCB-1260
P PCB-1016
P TOXAPHENE
D 2,3,7,8-TCDD
V XYLENES
A PHENOL-D5
A PENTAFLUOROPHENOL
V PENTAFLOUROBENZENE
A TRIFLUORO-M-CRESOL
V 2,2-DIFLUOROTETRACHLOROETHANE
B 2-FLUOROBIPHENYL
B 1-FLUORONAPHTHALENE
A 2-FLOUROPHENOL
B 2-FLUORONAPHTHALENE
B PYRIDINE-D5
B ANILINE-OS
B NAPHTHALENE-OS
V TOLUENE-D8
B NITROBENZENE-OS
B 2,2'-DIFLUOROBIPHENYL
V BENZENE-D6
B DECAFLUOROBIPHENYL
V M-DIFLUOROBENZENE
V METHYLENE CHLORIDE-D2
V 1,1,2,2-TETRACHLOROETHANE-D2
V ETHYLBENZENE-D10
V 1,2 DICHLOROETHANE-D4
V 2,2 DICHLOPROPANE-D6
V CHLOROBENZENE-D5
B 1,2 DICHLOROBENZENE-D4
B CHRYSENE D12
B FLUORENE D10
A 2-NITROPHENOL D4
B DI-N-BUTYL-PHTHALATE-D4
B 4-FLUOROANILINE
V BROMOCHLOROMETHANE
V 2-BROMO-l-CHLOROPROPANE
V 1,4-DICHLOROBUTANE
D 2,3,7,3-TCDD-37CL4
V BROMOFLUOROBENZENE
P Y
P Y
P Y
P Y
P Y
P Y
P Y
P Y
P Y
P Y
P Y
P Y
P Y
P 0320 Y
P Y
S Y
S Y
S Y
S Y
S Y
S Y
S Y
S Y
S Y
S Y
S Y
S Y
S Y
S Y
I 0190 Y
S Y
S Y
S Y
S Y
S Y
S Y
S Y
S Y
S Y
S Y
S Y
S Y
S Y
S Y
S Y
I 0128 Y
I 0077 Y
I 0055 Y
I 0328 Y
I 0095 Y
E-93
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
186
187
188
189
201
202
203
204
205
206
207
208
209
210
211
212
213
214
215
216
217
218
219
220
221
222
223
224
225
226
227
228
229
230
231
232
233
234
235
236
237
238
239
240
241
242
243
244
245
246
B DFTPP
P 2'-CHLOROBIPHENYL-D5
P 3' ,4',5'-TRICHLOROBIPHENYL-D5
P 3,3',4,4'-TETRACHLOROBIPHEN-D6
B ACENAPHTHENE-D10
V ACROLEIN-D4
V ACRYLONITRILE-D3
V BENZENE-D6
B BENZIDINE (RINGS-OS)
V CARBON TETRACHLORIDE-13C
V CHLOROBENZENE-D5
B 1,2,4-TRICHLOROBENZENE-D3
B HEXACHLOROBENZENE-13C6
V 1,2-DICHLOROETHANE-D4
V 1,1,1-TRICHLOROETHANE-D3
B HEXACHLOROETHANE-1-13C
V l,l-DICHLOROETHANE-2,2,2-03
V 1,1,2-TRICHLOROETHANE-13C2
V 1,1,2,2-TETRACHLOROETHANE-D2
V CHLOROETHANE-D5
V
B BIS(2-CHLOROETHYL)ETHER-D3
V
B 2-CHLORONAPHTHALENE-D7
A 2,4,6-TRICHLOROPHENOL-3,5-D2
A 4-CHLORO-3-METHYLPHENOL-2.6-D2
V CHLOROFORM-13C
A 2-CHLOROPHENOL-3,4,5,6-D4
B 1,2-DICHLOROBENZENE-D4
B 1,3-DICHLOROBENZENE-D4
B 1,4-DICHLOROBENZENE-D4
B 3,3'-DICHLOROBENZIDINE-D6
V 1,1-DICHLOROETHENE-D2
V TRANS-1,2-DICHLOROETHENE-D2
A 2,4-DICHLOROPHENOL-3,5,6-D3
V 1.2-DICHLOROPROPANE-D6
V T-1,3-DICHLOROPROPENE-1,2-D4
B 2,4-DIMETHYLPHENOL-3,5,6-03
B 2,4-DINITROTOLUENE-3,5,6-D3
B 2,6-DINITROTOLUENE-A,A,A-D3
B 1,2-DIPHENYL-D10-HYDRAZINE
V ETHYLBENZENE-D10
B FLUORANTHENE-D10
B 4-CHLOROPHENYL PHENYL-D5 ETHER
B
B BISC2-CHLQROISOPROPYDETHERD12
B
V METHYLENE CHLORIDE-D2
V CHLOROMETHANE-D3
V BROMOMETHANE-D3
I
S
S
S
Y
Y
Y
Y
Y
N
Y
0198 N
N
N
N
D 0164 Y
0 0060 Y
D 0056 Y
D 0084 Y
D 0192 Y
0 0048 Y
D 0117 Y
0 0183 Y
D 0292 Y
D 0067 Y
D 0102 Y
D 0204
0 0066
D 0084
D 0084
D 0071
D
D 0101
D 0113 N
D 0169 Y
D 0200 Y
D 0109 Y
D 0086 Y
D 0132
D 0152
D 0152
D 0152
D 0258
D 0065
D 0065
D 0167 Y
D 0067 Y
0 0079
D 0125
D 0168
D 0167 Y
D 0082 Y
D 0116
0 0212
D 0209 Y
D N
D 0131 Y
D N
D 0088 Y
D 0053 Y
D 0099 Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
E-94
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
247
248
249
250
251
252
253
254
255
256
257
258
259
260
261
262
263
264
265
266
267
268
269
270
271
272
273
274
275
276
277
278
279
280
281
282
283
284
285
286
287
288
289
290
291
292
293
294
295
296
V BROMOFORM-13C
V BROMODICHLORQMETHANE-13C
V
V
V DIBROMOCHLOROMETHANE-13C
B HEXACHLORO-1,3-BUTADIENE-1
B HEXACHLOROCYCLOPENTADIENE-
B ISOPHORONE-D8
B NAPHTHALENE-08
B NITROBENZENE-05
A 2-NITROPHENOL-3,4,5,6-D4
A 4-NITROPHENOL-2,3,5,6-D4
A 2,4-DINITROPHENOL-3,5,6-D3
A 2-METHYL-4,6-DINITROPHENOL
B
B N-NITROSODIPHENYLAMINE-06
B
A PENTACHLOROPHENOL-13C6
B PHENOL-2,3,4,5,6-05
B BIS(2-ETHYLHEXYL)PHTHALATE
B
B DI-N-BUTYL PHTHALATE-D4
B DI-N-OCTYL PHTHALATE-D4
B DIETHYL PHTHALATE-3,4,5,6-
B DIMETHYL PHTHALATE-3,4,5,6
B BENZO(A)ANTHRACENE-D12
B BENZQ(A)PYRENE-D12
B BENZO(B)FLUORANTHENE-D12
B BENZO(K)PLUORANTHENE-D12
B CHRYSENE-D12
B ACENAPHTHYLENE-D8
B ANTHRACENE-DIO
B BENZO(GHI)PERYLENE-D12
B FLUORENE-D10
B PHENANTHRENE-D10
B
B
B PYRENE-D10
V TETRACHLOROETHENE-1,2-13C2
V TOLUENE-2,3,4,5,6-08
V TRICHLOROETHENE-13C2
V VINYL CHLORIDE-D3
P ALDRIN-13C4
P DIELDRIN-13C4
P
P 4,4'-DDT-D8
P 4,4'-DDE-D8
P 4,4'-DDD-D8
P ENDOSULFAN-I-D4
3C4
13C4
-D2
-D4
04
-D4
D
0
0
D
D
D
D
D
D
D
D
D
D
0
D
D
D
D
D
D
D
0
0
0
D
D
D
D
D
D
D
D
D
D
D
D
D
D
D
0
D
D
D
D
D
D
D
D
D
D
0176
0086
0130
0231
0241
0088
0136
0128
0143
0143
0187
0200
0175
0272
0071
0153
0153
0153
0153
0167
0240
0264
0264
0264
0240
0160
0188
0288
0176
0188
0212
0172
0098
013-6
0065
Y
Y
N
N
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
N
Y
N
Y
Y
Y
N
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
N
N
Y
Y
Y
Y
Y
N
N
N
N
N
N
N
N
E-95
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
297
298
299
301
302
303
304
305
306
307
308
309
310
311
312
313
314
315
316
317
318
319
320
321
322
323
324
325
326
327
328
329
330
331
332
333
334
335
336
337
338
339
340
341
342
343
344
345
346
347
P
P
P
B ACENAPHTHENE
V ACROLEIY
V ACRYLONITRILE
V BENZENE
B BENZIDINE
V CARBON TETRACHLORIDE
V CHLOROBENZENE-
B 1,2,4-TRICHLOROBENZENE
B HEXACHLOROBENZENE
V 1,2-DICHLOROETHANE
V 1,1,1-TRICHLOROETHANE
B HEXACHLOROETHANE
V 1,1-DICHLOROETHANE
V 1,1,2-TRICHLOROETHANE
V 1,1,2,2-TETRACHLOROETHANE
V CHLOROETHANE
V
B BIS(2-CHLOROETHYL)ETHER
V
B 2-CHLORONAPHTHALENE
A 2,4,6-TRICHLOROPHENOL
A 4-CHLORO-3-METHYLPHENOL
V CHLOROFORM
A 2-CHLOROPHENOL
B 1,2-DICHLOROBENZENE
B 1 , 3-DICHLOROBENZENE
B 1,4-DICHLOROBENZENE
B 3,3'-DICHLQROBENZIDINE
V 1,1-DICHLOROETHENE
V TRANS-1,2-DICHLOROETHENE
A 2,4-DICHLOROPHENOL
V 1,2-DICHLOROPROPANE
V T-1,3-DICHLOROPROPENE
B 2,4-DIMETHYLPHENOL
B 2,4-DINITROTOLUENE
B 2,6-DINITROTOLUENE
B 1,2-DIPHENYLHYDRAZINE
V ETHYLBENZENE
B FLUORANTHENE
B 4-CHLOROPHENYL PHENYL ETHER
B
B BIS (2-CHLOROISOPROPYL) ETHER
B
V METHYLENE CHLORIDE
V CHLOROMETHANE
V BROMOMETHANE
V BROMOFORM
P
P
P
Y
Y
D N
D N
D N
P 0154 Y
P 0056 Y
P 0053 Y
P 0078 Y
P 0184 Y
P 0047 Y
P 0112 Y
P 0180 Y
P 0284
P 0062
P 0097 Y
P 0201 Y
P 0063 Y
P 0083 Y
P 0083 Y
P 0064 Y
P N
P 0093 Y
P 0106 N
P 0162 Y
P 0196 Y
P 0107 Y
P 0085
P 0128
0146
0146 Y
0146 Y
P 0252
P 0061
P 0061
P 0162
P 0063
P 0075 Y
P 0122 Y
P 0165 Y
P 0165 Y
P 0077 Y
P 0106 Y
P 0202 Y
P 0204 Y
P N
P 0121 Y
P N
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
P 0084
P 0050
P 0096
P 0173 Y
E-96
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
348
349
350
351
352
353
354
355
356
357
358
359
360
361
362
363
364
365
366
367
368
369
370
371
372
373
374
375
376
377
378
379
330
381
382
383
384
385
386
387
388
389
390
391
392
393
394
395
396
397
V
V
V
V
B
B
B
B
B
A
A
A
A
B
B
B
A
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
V
V
V
V
p
p
p
p
p
p
p
p
p
BROMODICHLOROMETHANE
DIBROMOCHLOROMETHANE
HEXACHLORO-1.3-BUTADIENE
HEXACHLOROCYCLOPENTADIENE
ISOPHORONE
NAPHTHALENE
NITROBENZENE
2-NITROPHENOL
4-NITROPHENOL
2,4-DINITROPHENOL
2-METHYL-4,6-DINITROPHENOL
N-NITROSODIPHENYLAMINE
PENTACHLOROPHENQL
PHENOL
BIS (2-ETHYLHEXYL)
PHTHALATE
DI-N-BUTYL PHTHALATE
DI-N-OCTYL PHTHALATE
DIETHYL PHTHALATE
DIMETHYL PHTHALATE
BENZO(A)ANTHRACENE
BENZO(A)PYRENE
BENZO(B)FLUORANTHENE
BENZO(K)FLUORANTHENE
CHRYSENE
ACENAPHTHYLENE
ANTHRACENE
BENZO(6HI)PERYLENE
FLUORENE
PHENANTHRENE
PYRENE
TETRACHLOROETHENE
TOLUENE
TRICHLOROETHENE
VINYL CHLORIDE
P
P
P
P
P
P
P
P
P
P
P
P
P
P
P
P
P
N
Y
0083 Y
N
N
P 0129 Y
P 0225 Y
P 0237 Y
P 0082 Y
P 0128 Y
P 0123 Y
P 0139 Y
P 0139 Y
P 0184 Y
P 0198 Y
P N
P 0169 Y
P
P 0266
P 0094 Y
P 0149 Y
P N
P 0149 Y
P 0149 Y
P 0149 Y
P 0163
P 0228
P 0252
P 0252
P 0252
P 0228
P 0152 Y
P 0178 Y
0276 Y
0166 Y
0178 Y
N
N
P 0202 Y
P 0166 Y
P 0092 Y
P 0095 Y
P 0062 Y
Y
Y
Y
Y
Y
Y
N
N
N
N
N
N
N
N
N
E-97
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
398
399
400
402
404
429
500
501
502
503
504
505
506
507
508
509
510
511
512
513
514
515
516
517
518
519
520
521
522
523
524
525
526
527
528
529
530
531
532
533
534
535
536
537
538
539
540
541
542
543
P
P
P HEPATACHLOR-13C4
P ALPHA-BHC-D6
P GAMMA-BHC-D6
D 2,3,7,8-TCDD-13C12
A BENZOIC ACID
A HEXANOIC ACID
B B-NAPHTHYLAMINE
B ALPHA-PICOLINE
B DIBENZOTHIOPHENE
B DIBENZOFURAN
B N-DODECANE (N-C12)
B DIPHENYLAMINE
B DIPHENYL ETHER
B ALPHA-TERPINEOL
B STYRENE
B DI-N-BUTYL AMINE
B BIPHENYL
B P-CYMEME
V 2-BUTANONE (MEK)
V DIETHYL ETHER
V ACETONE
B N-DECANE (N-C10)
B N-TETRADECANE (N-C14)
B N-HEXADECANE (N-C16)
B N-OCTADECANE (N-C18)
B N-EICOSANE (N-C20)
B N-DOCOSANE (N-C22)
B N-TETRACOSANE CN-C24)
B N-HEXACOSANE CN-C26)
B N-OCTACOSANE (N-C28)
B N-TRIACONTANE (N-C30)
V P-DIOXANE
B CARBAZOLE
B 1,2,3-TRICHLOROBENZENE
A 2,3,6-TRICHLQROPHENOL
A 2,4,5-TRICHLOROPHENOL
V ALLYL ALCOHOL
V CARBON DISULFIDE
V 2-CHLORO-l,3-BUTADIENE
V CHLORQACETONITRILE
V 3-CHLOROPROPENE
V CROTONALDEHYDE
V 1,2-DIBROMOETHANE (EDB)
V DIBROMOMETHANE
V TRANS-l,4-DICHLORO-2-BUTENE
V 1,3-DICHLOROPROPANE
V CIS-1,3-DICHLOROPROPENE
V ETHYL CYANIDE
P
P
D
D
D
P
P
P
N
N
N
N
N
Y
Y
Y
Y
Y
Y
0 0332
P
P
P 0143 Y
P 0093 Y
P 0184
P 0168
P 0055
P 0169 Y
P 0170 Y
0059 Y
0104 Y
0086 N
P 0154
P 0119
P 0072 Y
P 0074 Y
P 0058
P 0055
P 0055
P 0055
P 0055
P 0055
P 0055 Y
P 0055 Y
P 0055 Y
P 1)055
P 0055
P 0088
P 0167 Y
P 0180 Y
P 0196 Y
P 0196 Y
P 0057 Y
P 0076 Y
P 0053 Y
P 0075 Y
P 0076 Y
P 0070 Y
P 0107 Y
P 0093 Y
P 0075 Y
P 0076
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
P 0075 Y
P 0054 Y
E-98
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
544
545
546
547
548
549
550
551
552
553
554
555
556
557
558
559
560
561
562
563
564
565
566
567
568
569
570
571
572
573
574
575
576
577
578
579
580
581
582
583
584
585
586
587
588
589
590
591
592
593
V ETHYL METHACRYLATE
V 2-HEXANQNE
V IODOMETHANE
V ISOBUTYL ALCOHOL
V METHACRYLONITRILE
V METHYL METHACRYLATE
V 4-METHLY-2-PENTANONE
V 1,1,1,2-TETRACHLOROETHANE
V TRICHLOROPLUORQMETHANE
V 1,2,3-TRICHLOROPROPANE
V VINYL ACETATE
B ACETOPHENONE
B 4-AMINOBIPHENYL
B ANILINE
B 0-ANISIDINE
B ARAMITE
B BENZANTHRONE
B 1,3-BEN2ENEDIOL (RESQRCINOL)
B BENZENETHIQL
B 2,3-BENZOFLUORENE
B BENZYL ALCOHOL
B 2-BROMOCHLQROBENZENE
B 3-BROMOCHLOROBENZENE
B 4-CHLORO-2-NITROANILINE
B 5-CHLORO-O-TOLUIDINE
B 4-CHLOROANILINE
B 3-CHLORONITROBENZENE
B 0-CRESOL
B CROTOXYPHOS
B 2,6-DI-TERT-BUTYL-P-BENZOQINO
B 2,4-DIAMINOTOLUENE
B 1,2-DIBROMO-3-CHLOROPROPANE
B 2,6-DICHLORO-4-NITROANILINE
B l,3-DICHLORO-2-PROPANOL
B 2,3-DICHLOROANILINE
B 2,3-DICHLORONITROBENZENE
B 1,2:3,4-DIEPOXYBUTANE
B 3,3'-DIMETHOXYBENZIDINE
B DIMETHYL SULFONE
B P-DIMETHYLAMINOAZOBENZENE
B 7,12-DIMETHYLBENZ(A)ANTHRACENE
B N,N-DIMETHYLFORMAMIDE
B 3,6-DIMETHYLPHENANTHRENE
B 1 ,3-DINITROBENZENE
B DIPHENYLDISULFIDE
B ETHYL METHANESULFONATE
B ETHYLENETHIOUREA
B ETHYNYLESTRADIOL 3-METHYL ETHE
B HEXACHLOROPROPENE
B 2-ISOPROPYLNAPHTHALENE
Y
Y
Y
Y
P 0069
P 0058
P 0142 Y
P 0074 Y
P 0067 Y
P 0069
P 0058
P 0131 Y
P 0101 Y
P 0075 Y
P 0086 Y
P 0105 Y
P 0169 Y
P 0093 Y
P 0108 Y
P 0185
P 0230
P 0110
P 0110
P 0216 Y
P 0079 Y
P 0111 Y
P 0192
P 0172
P 0106
P 0127 Y
0157 Y
0108 Y
0127 Y
0220 Y
0122 Y
0157 Y
P 0124 Y
P 0079
P 0161
P 0191
P 0055 Y
P 0224 Y
P 0079 Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
0120 Y
Y
Y
P 0256
P 0073
P 0206 Y
P 0168 Y
P 0218 Y
P 0109 Y
P 0102 Y
P 0227 Y
P 0213 Y
P 0170 Y
E-99
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
594
595
596
597
598
599
600
601
602
603
604
605
606
607
608
609
610
611
612
613
614
615
616
617
618
619
620
621
622
623
624
625
626
627
628
629
630
631
700
701
702
703
704
705
706
707
708
709
710
711
B ISOSAFROLE
B LON6IFOLENE
B MALACHITE GREEN
B METHAPYRILENE
B METHYL METHANESULFONATE
B 2-METHYLBENZOTHIOAZOLE
A BENZOIC-D5 ACID
A HEXANOIC ACID-011
B B-NAPHTHYLAMINE-D7
B ALPHA-PICOLINE-D7
B DIBENZOTHIOPHENE-D8
B DIBENZOFURAN-D8
B N-DODECANE-D26 (N-C12)
B DIPHENYLAMINE-D10
B DIPHENYL ETHER-D10
B ALPHA-TERPINEOL-03
B STYRENE-2,3,4,5,6-D5
B DI-N-BUTYL AMINE-D18
B BIPHENYL-D10
B P-CYMENE-D14
V 2-BUTANONE-4,4,4-03 (MEK)
V DIETHYL ETHER-D10
V ACETONE-D6
B N-DECANE-D22 (N-C10)
B
B N-HEXADECANE-D34 (N-C16)
B
B N-EICOSANE-D42 (N-C20)
B
B N-TETRACOSANE-D50 (N-C24)
B
B
B N-TRIACONTANE-D62 CN-C30)
V P-DIOXANE D8
B CARBAZOLE 08
B 1,2,3-TRICHLQROBENZENE 03
A 2,3,6-TRICHLOROPHENOL 02
A 2,4,5-TRICHLOROPHENOL 02
A BENZOIC ACID
A HEXANOIC ACID
B B-NAPHTHYLAMINE
B 2-METHYLPYRIDINE
B DIBENZOTHIOPHENE
B DIBENZOFURAN
B N-OOOECANE (N-C12)
B OIPHENYLAMINE
B DIPHENYL ETHER
B ALPHA-TERPINEOL
B STYRENE
B DI-N-BUTYL AMINE
P 0162 Y
P 0161 Y
P 0330 Y
P 0097 Y
P 0080 Y
P 0149 Y
Y
Y
Y
Y
Y
D N
0 N
D 0150 Y
0 0100 Y
D 0192 Y
D 0176 Y
D 0066 Y
D 0179 Y
D 0180 Y
D 0062
D 0109
0 0096 N
0 0164 Y
D 0130
D 0075
D 0084
D 0064 Y
D 0066 Y
D N
D 0066 Y
0 N
D 0066 Y
D N
D 0066 Y
0 N
D N
0 11066 Y
D 0096 N
D 0175 N
0 0183 N
D 0200 N
D 1)200 N
Y
Y
0143 Y
0093 Y
0184 Y
0168
0055
P 0169 Y
P 0170 Y
P 0059 Y
P 0104 Y
P 0086 N
Y
Y
E-100
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
712
713
714
715
716
717
718
719
720
721
722
723
724
725
726
727
728
729
730
731
829
900
901
902
903
904
905
906
907
908
909
910
911
912
913
914
915
916
917
918
919
920
921
922
923
924
925
926
927
928
B BIPHENYL
B P-CYMENE
V 2-BUTANONE (MEK)
V DIETHYL ETHER
V ACETONE
B N-DECANE CN-C10)
B
B N-HEXADECANE (N-C16)
B
B N-EICOSANE (N-C20)
B
B N-TETRACOSANE (N-C24)
B
B
B N-TRIACONTANE (N-C30)
V P-DIOXANE
B CARBAZOLE
B 1,2,3-TRICHLOROBENZENE
A 2.3,6-TRICHLOROPHENOL
A 2,4,5-TRICHLOROPHENOL
D 2,3,7,8-TCDD
B 3-METHYLCHOLANTHRENE
B 4,4'-METHYLENEBIS<2-CHLOROANI)
B 4,5-METHYLENEPHENANTHRENE
B 1-METHYLFLUORENE
B 2-METHYLNAPHTHALENE
B 1-METHYLPHENANTHRENE
B 2-
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
929
930
931
932
933
934
935
936
937
933
939
940
941
942
943
944
945
946
947
943
TABLE COUNT:
B PRONAMIDE
B PYRIDINE
B SAFROLE
B SQUALENE
B 1,2,4,5-TETRACHLOROBENZENE
B THIANAPHTHENE
B THIOACETAMIDE
B THIOXANTHONE
B 0-TOLUIDINE
B 1,2,3-TRIMETHOXYBENZENE
B 2,4,5-TRINETHYLANILINE
B TRIPHENYLENE
B TRIPROPYLENEGLYCOL METHYL ETHE
B 1,3,5-TRITHIANE
A BENZOIC ACID
A P-CRESOL
A 3,5-DIBROMO-4-HYDROXYBENZONITR
A 2,6-DICHLOROPHENOL
A HEXANOIC ACID
A 2,3,4,6-TETRACHLOROPHENOL
570
P 0173 Y
P 0079 Y
P 0162
0069
0216
P 0134 Y
P 0075 Y
P 0212
P 0106
P
P
Y
Y
Y
Y
Y
P 0168 Y
P 0120 Y
P 0223
P 0059
Y
Y
P 0138 Y
P 0105 Y
P 0108 Y
P 0227 Y
P 0166 Y
P 0060 Y
P 0232 Y
E-102
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ATTACHMENT 7
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ANALYTICAL METHODS 162»C AND 1625C
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18 December 1986
Method 1624, Revision C
Volatile Organic Compounds by Isotope Dilution GCMS
1 Scope and application
1.1 This method is designed to determine the volatile toxic organic
pollutants associated with the 1976 Consent Decree; the Resource
Conservation and Recovery Act; the Comprehensive Environmental
Response, Compensation and Liabilities Act; and other compounds
amenable to purge and trap gas chromatography-mass spectrometry
(GCMS) .
1.2 The chemical compounds listed in tables 1 and 2 may be determined
in waters, soils, and municipal sludges by this method. The method
is designed to meet the survey requirements of the Environmental
Protection Agency.
1.3 The detection limit of this method is usually dependent on the
level of interferences rather than instrumental limitations. The
levels in table 3 typify the minimum quantity that can be detected
with no interferences present.
1.4 The GCMS portions of this method are for use only by analysts
experienced with GCMS or under the close supervision of such quali-
fied persons. Laboratories unfamiliar with analyses of environmen-
tal samples by GCMS should run the performance tests in reference 1
before beginning.
2 Summary of method
2.1 The.percent solids content of the sample is determined. If the
E-105
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solids content is known or determined to be less than one percent,
stable isotopically labeled analogs of the compounds of interest
are added to a 5 mL sample and the sample is purged with an inert
gas at 20 - 25 °C in a chamber designed for soil or water samples.
If the solids content is greater than one percent, five mL of
reagent water and the labeled compounds are added to a 5 gram
aliquot of sample and the mixture is purged at 40 °C. Compounds
that will not purge at 20 - 25 °C or at 40 °C are purged at 75 - 85
°C.
In the purging process, the volatile compounds are transferred from
the aqueous phase into the gaseous phase where they are passed into
a sorbent column and trapped. After purging is completed, the trap
is backflushed and heated rapidly to desorb the compounds into a
gas chromatograph (GC). The compounds are separated by the GC and
detected by a mass spectrometer (MS) (references 2 and 3). The
labeled compounds serve to correct the variability of the analyti-
cal technique.
2.2 Identification of a pollutant (qualitative analysis) is performed
in one of three ways: (1) For compounds listed in table 1 and
other compounds for which authentic standards are available, the
GCMS system is calibrated and the mass spectrum and retention time
for each standard are stored in a user created library. A compound
is identified when its retention time and mass spectrum agree with
the library retention time and spectrum. (2) For compounds listed
in table 2 and other compounds for which standards are not avail-
able, a compound is identified when the retention time and mass
spectrum agree with those specified in this method. (3) For
chromatographic peaks which are not identified by (1) and (2)
above, the background corrected spectrum at the peak maximum is
1624C E-106
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compared with spectra in the EPA/NIH Mass Spectral File (reference
4). Tentative identification is established when the spectrum
agrees.
2.3 Quantitative analysis is performed in one of four ways by GCMS
using extracted ion current profile (EICP) areas: (1) For com-
pounds listed in table 1 and other compounds for which standards
and labeled analogs are available, the GCMS system is calibrated
and the compound concentration is determined using an isotope
dilution technique. (2) For compounds listed in table 1 and for
other compounds for which authentic standards but no labeled
compounds are available, the GCMS system is calibrated and the
compound concentration is determined using an internal standard
technique. (3) For compounds listed in table 2 and other compounds
for which standards are not available, compound concentrations are
determined using known response factors. (4) For compounds for
which neither standards nor known response factors are available,
compound concentration is determined using the sum of the EICP
areas relative to the sum of the EICP areas of the nearest eluted
internal standard.
2.4 Quality is assured through reproducible calibration and testing of
the purge and trap and GCMS systems.
3 Contamination and interferences
3.1 Impurities in the purge gas, organic compounds out-gassing from
the plumbing upstream of the trap, and solvent vapors in the
laboratory account for the majority of contamination problems. The
analytical system is demonstrated to be free from interferences
under conditions of the analysis by analyzing reagent water blanks
initially and with each sample batch (samples analyzed on the same
1624C £-107
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8 hr shift), as described in section 8.5.
3.2 Samples can be contaminated by diffusion of volatile organic
compounds (particularly methylene chloride) through the bottle seal
during shipment and storage. A field blank prepared from reagent
water and carried through the sampling and handling protocol serves
as a check on such contamination.
3.3 Contamination by carry-over can occur when high level and low
level samples are analyzed sequentially. To reduce carry-over, the
purging device (figure 1 for samples containing less than one
percent solids; figure 2 for samples containing one percent solids
or greater) is cleaned or replaced with a clean purging device
after each sample is analyzed. When an unusually concentrated
sample is encountered, it is followed by analysis of a reagent
water blank to check for carry-over. Purging devices are cleaned
by washing with soap solution, rinsing with tap and distilled
water, and drying in an oven at 100-125 °C. The trap and other
parts of the system are also subject to contamination; therefore,
frequent bakeout and purging of the entire system may be required.
3.4 Interferences resulting from samples will vary considerably from
source to source, depending on the diversity of the site being
sampled.
4 Safety
4.1 The toxicity or carcinogenicity of each compound or reagent used
in this method has not been precisely determined; however, each
chemical compound should be treated as a potential health hazard.
Exposure to these compounds should be reduced to the lowest
possible level. The laboratory is responsible for maintaining a
current awareness file of OSHA regulations regarding the safe
1624C E-108
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handling of the chemicals specified in this method. A reference
file of data handling sheets should also be made available to all
personnel involved in these analyses. Additional information on
laboratory safety can be found in references 5-7.
4.2 The following compounds covered by this method have been tenta-
tively classified as known or suspected human or mammalian carci-
nogens: benzene, carbon tetrachloride, chloroform, and vinyl
chloride. Primary standards of these toxic compounds should be
prepared in a hood, and a NIOSH/MESA approved toxic gas respirator
should be worn when high concentrations are handled.
5 Apparatus and materials
5.1 Sample bottles for discrete sampling
5.1.1 Bottle25 to 40 mL with screw cap (Pierce 13075, or equiva-
lent) . Detergent wash, rinse with tap and distilled water, and dry
at >105 °C for one hr minimum before use.
5.1.2 SeptumTeflon-faced silicone (Pierce 12722, or equivalent),
cleaned as above and baked at 100 - 200 °C for one hour minimum.
5.2 Purge and trap deviceconsists of purging device, trap, and
desorber.
5.2.1 Purging devices for water and soil samples
5.2.1.1 Purging device for water samplesdesigned to accept 5 mL
samples with water column at least 3 cm deep. The volume of the
gaseous head space between the water and trap shall be less than 15
mL. The purge gas shall be introduced less than 5 mm from the base
of the water column and shall pass through the water as bubbles
with a diameter less than 3 mm. The purging device shown in figure
1 meets these criteria.
5.2.1.2 Purging device for solid samplesdesigned to accept 5 grams of
1624C E-109
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solids plus 5 mL of water. The volume of the gaseous head space
between the water and trap shall be less than 25 mL. The purge gas
shall be introduced less than 5 mm from the base of the sample and
shall pass through the water as bubbles with a diameter less than 3
mm. The purging device shall be capable of operating at ambient
temperature (20 - 25 °C) and of being controlled at temperatures of
40 +/- 2 °C and 80 +/- 5 °C while the sample is being purged. The
purging device shown in figure 2 meets these criteria.
5.2.2 Trap25 to 30 cm x 2.5 mm i.d. minimum, containing the follow-
ing:
5.2.2.1 Methyl silicone packingone +/~ 0.2 cm, 3 percent OV-1 on
60/80 mesh Chromosorb W, or equivalent.
5.2.2.2 Porous polymer15 +/~ 1-0 cn>> Tenax GC (2,6-diphenylene oxide
polymer), 60/80 mesh, chromatographic grade, or equivalent.
5.2.2.3 Silica gel8 +/- 1.0 cm, Davison Chemical, 35/60 mesh, grade
15, or equivalent. The trap shown in figure 3 meets these specifi-
cations .
5.2.4 Desorbershall heat the trap to 175 +/~ 5 °c in 45 seconds or
less. The polymer section of the trap shall not exceed a tempera-
ture of 180 °C and the remaining sections shall not exceed 220 °C
during desorb, and no portion of the trap shall exceed 225 °C
during bakeout. The desorber shown in figure 4 meets these
specifications.
5.2.5 The purge and trap device may be a separate unit or coupled to a
GC as shown in figures 4 and 5.
5.3 Gas chromatographshall be linearly temperature programmable with
initial and final holds, shall contain a glass jet separator as the
MS interface, and shall produce results which meet the calibration
(section 7), quality assurance (section 8), and performance tests
1624C E-110
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(section 11) of this method.
5.3.1 Column2.8 +/~ 0.4 m x 2 +/~ 0.5 mm i.d. glass, packed with one
percent SP-1000 on Carbopak B, 60/80 mesh, or equivalent.
5.4 Mass spectrometer70 eV electron impact ionization; shall
repetitively scan from 20 to 250 amu every 2-3 seconds, and produce
a unit resolution (valleys between m/z 174-176 less than 10 percent
of the height of the m/z 175 peak), background corrected mass
spectrum from 50 ng 4-bromofluorobenzene (BFB) injected into the
GC. The BFB spectrum shall meet the mass-intensity criteria in
table 4. All portions of the GC column, transfer lines, and
separator which connect the GC column to the ion source shall
remain at or above the column temperature during analysis to
preclude condensation of less volatile compounds.
5.5 Data systemshall collect and record MS data, store mass-
intensity data in spectral libraries, process GCMS data and
generate reports, and shall calculate and record response factors.
5.5.1 Data acquisitionmass spectra shall be collected continuously
throughout the analysis and stored on a mass storage device.
5.5.2 Mass spectral librariesuser created libraries containing mass
spectra obtained from analysis of authentic standards shall be
employed to reverse search GCMS runs for the compounds of interest
(section 7.2).
5.5.3 Data processingthe data system shall be used to search,
locate, identify, and quantify the compounds of interest in each
GCMS analysis. Software routines shall be employed to compute
retention times and EICP areas. Displays of spectra, mass chroma-
tograms, and library comparisons are required to verify results.
5.5.4 Response factors and multipoint calibrationsthe data system
shall be used to record and maintain lists of response factors
1624C E-lll
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(response ratios for isotope dilution) and generate multi-point
calibration curves (section 7). Computations of relative standard
deviation (coefficient of variation) are useful for testing
calibration linearity. Statistics on initial and on-going perfor-
mance shall be maintained (sections 8 and 11).
5.6 Syringes5 mL glass hypodermic, with Luer-lok tips.
5.7 Micro syringes10, 25, and 100 uL.
5.8 Syringe valves2-way, with Luer ends (Teflon or Kel-F).
5.9 Syringe5 mL, gas-tight, with shut-off valve.
5.10 Bottles15 mL, screw-cap with Teflon liner.
5.11 Balances
5.11.1 Analytical, capable of weighing 0.1 mg.
5.11.2 Top loading, capable of weighing 10 mg.
5.12 Equipment for determining percent moisture
5.12.1 Oven, capable of being temperature controlled at 110 +/- 5 °C.
5.12.2 Dessicator
5.12.3 Beakers50 - 100 mL
6 Reagents and standards
6.1 Reagent waterwater in which the compounds of interest and
interfering compounds are not detected by this method (section
11.7). It may be generated by any of the following methods:
6.1.1 Activated carbonpass tap water through a carbon bed (Calgon
Filtrasorb-300, or equivalent).
6.1.2 Water purifierpass tap water through a purifier (Millipore
Super Q, or equivalent).
6.1.3 Boil and purgeheat tap water to 90-100 °C and bubble contami-
nant free inert gas through it for approx one hour. While still
hot, transfer the water to screw-cap bottles and seal with a
1624C E-112
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Teflon-lined cap.
6.2 Sodium thiosulfateACS granular.
6.3 Methanolpesticide quality or equivalent.
6.4 Standard solutionspurchased as solutions or mixtures with
certification to their purity, concentration, and authenticity, or
prepared from materials of known purity and composition. If
compound purity is 96 percent or greater, the weight may be used
without correction to calculate the concentration of the standard.
6.5 Preparation of stock solutionsprepare in methanol using liquid
or gaseous standards per the steps below. Observe the safety
precautions given in section 4.
6.5.1 Place approx 9.8 mL of methanol in a 10 mL ground glass stop-
pered volumetric flask. Allow the flask to stand unstoppered for
approx 10 minutes or until all methanol wetted surfaces have dried.
In each case, weigh the flask, immediately add the compound, then
immediately reweigh to prevent evaporation losses from affecting
the measurement.
6.5.1.1 Liquidsusing a 100 uL syringe, permit 2 drops of liquid to
fall into the methanol without contacting the neck of the flask.
Alternatively, inject a known volume of the compound into the
methanol in the flask using a micro-syringe.
6.5.1.2 Gases (chloromethane, bromomethane, chloroethane, vinyl
chloride)fill a valved 5 mL gas-tight syringe with the compound.
Lower the needle to approx 5 mm above the methanol meniscus. Slowly
introduce the compound above the surface of the meniscus. The gas
will dissolve rapidly in the methanol.
6.5.2 Fill the flask to volume, stopper, then mix by inverting several
times. Calculate the concentration in mg/mL (ug/uL) from the
weight gain (or density if a known volume was injected).
1624C E-113
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6.5.3 Transfer the stock solution to a Teflon sealed screw-cap bottle.
Store, with minimal headspace, in the dark at -10 to -20 °C.
6.5.4 Prepare fresh standards weekly for the gases and 2-chloroethyl-
vinyl ether. All other standards are replaced after one month, or
sooner if comparison with check standards indicate a change in
concentration. Quality control check standards that can be used to
determine the accuracy of calibration standards are available from
the US Environmental Protection Agency, Environmental Monitoring
and Support Laboratory, Cincinnati, Ohio.
6.6 Labeled compound spiking solutionfrom stock standard solutions
prepared as above, or from mixtures, prepare the spiking solution
to contain a concentration such that a 5-10 uL spike into each 5 mL
sample, blank, or aqueous standard analyzed will result in a
concentration of 20 ug/L of each labeled compound. For the gases
and for the water soluble compounds (acrolein, acrylonitrile,
acetone, diethyl ether, and MEK), a concentration of 100 ug/L may
be used. Include the internal standards (section 7.5) in this
solution so that a concentration of 20 ug/L in each sample, blank,
or aqueous standard will be produced.
6.7 Secondary standardsusing stock solutions, prepare a secondary
standard in methanol to contain each pollutant at a concentration
of 500 ug/mL. For the gases and water soluble compounds (section
6.6), a concentration of 2.5 mg/mL may be used.
6.7.1 Aqueous calibration standardsusing a 25 uL syringe, add 20 uL
of the secondary standard (section 6.7) to 50, 100, 200, 500, and
1000 mL of reagent water to produce concentrations of 200, 100, 50,
20, and 10 ug/L, respectively. If the higher concentration
standard for the gases and water soluble compounds was chosen
(section 6.6), these compounds will be at concentrations of 1000,
1624C E-114
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500, 250, 100, and 50 ug/L in the aqueous calibration standards.
6.7.2 Aqueous performance standardan aqueous standard containing all
pollutants, internal standards, labeled compounds, and BFB is
prepared daily, and analyzed each shift to demonstrate performance
(section 11). This standard shall contain either 20 or 100 ug/L of
the labeled and pollutant gases and water soluble compounds, 10
ug/L BFB, and 20 ug/L of all other pollutants, labeled compounds,
and internal standards. It may be the nominal 20 ug/L aqueous
calibration standard (section 6.7.1).
6.7.3 A methanolic standard containing all pollutants and internal
standards is prepared to demonstrate recovery of these compounds
when syringe injection and purge and trap analyses are compared.
This standard shall contain either 100 ug/mL or 500 ug/mL of the
gases and water soluble compounds, and 100 ug/mL of the remaining
pollutants and internal standards (consistent with the amounts in
the aqueous performance standard in 6.7.2).
6.7.4 Other standards which may be needed are those for test of BFB
performance (section 7.1) and for collection of mass spectra for
storage in spectral libraries (section 7.2).
7 Calibration
Calibration of the GCMS system is performed by purging the com-
pounds of interest and their labeled analogs from reagent water at
the temperature to be used for analysis of samples.
7.1 Assemble the gas chromatographic apparatus and establish operating
conditions given in table 3. By injecting standards into the GC,
demonstrate that the analytical system meets the minimum levels in
table 3 for the compounds for which calibration is to be performed,
and the mass-intensity criteria in table 4 for 50 ng BFB.
1624C E-115
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7.2 Mass spectral librariesdetection and identification of the
compounds of interest are dependent upon the spectra stored in user
created libraries.
7.2.1 For the compounds in table 1 and other compounds for which the
GCMS is to be calibrated, obtain a mass spectrum of each pollutant
and labeled compound and each internal standard by analyzing an
authentic standard either singly or as part of a mixture in which
there is no interference between closely eluted components. That
only a single compound is present is determined by examination of
the spectrum. Fragments not attributable to the compound under
study indicate the presence of an interfering compound. Adjust the
analytical conditions and scan rate (for this test only) to produce
an undistorted spectrum at the GC peak maximum. An undistorted
spectrum will usually be obtained if five complete spectra are
collected across the upper half of the GC peak. Software algo-
rithms designed to "enhance" the spectrum may eliminate distortion,
but may also eliminate authentic m/z's or introduce other distor-
tion.
7.2.3 The authentic reference spectrum is obtained under BFB tuning
conditions (section 7.1 and table 4) to normalize it to spectra
from other instruments.
7.2.4 The spectrum is edited by saving the 5 most intense mass
spectral peaks and all other mass spectral peaks greater than 10
percent of the base peak. The spectrum may be further edited to
remove common interfering masses. If 5 mass spectral peaks cannot
be obtained under the scan conditions given in section 5.4, the
mass spectrometer may be scanned to an m/z lower than 20 to gain
additional spectral information. The spectrum obtained is stored
for reverse search and for compound confirmation.
1624C E-U6
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7.2.5 For the compounds in table 2 and other compounds for which the
mass spectra, quantitation m/z's, and retention times are known but
the instrument is not to be calibrated, add the retention time and
reference compound (table 3); the response factor and the quantita-
tion m/z (table 5); and spectrum (Appendix A) to the reverse search
library. Edit the spectrum per section 7.2.4, if necessary.
7.3 Assemble the purge and trap device. Pack the trap as shown in
figure 3 and condition overnight at 170 - 180 °C by backflushing
with an inert gas at a flow rate of 20 - 30 mL/min. Condition
traps daily for a minimum of 10 minutes prior to use.
7.3.1 Analyze the aqueous performance standard (section 6.7.2)
according to the purge and trap procedure in section 10. Compute
the area at the primary m/z (table 5) for each compound. Compare
these areas to those obtained by injecting one uL of the methanolic
standard (section 6.7.3) to determine compound recovery. The
recovery shall be greater than 20 percent for the water soluble
compounds (section 6.6), and 60 - 110 percent for all other
compounds. This recovery is demonstrated initially for each purge
and trap GCMS system. The test is repeated only if the purge and
trap or GCMS systems are modified in any way that might result in a
change in recovery.
7.3.2 Demonstrate that 100 ng toluene (or toluene-d8) produces an area
at m/z 91 (or 99) approx one-tenth that required to exceed the
linear range of the system. The exact value must be determined by
experience for each instrument. It is used to match the calibra-
tion range of the instrument to the analytical range and detection
limits required.
7.4 Calibration by isotope dilutionthe isotope dilution approach is
used for the purgeable organic compounds when appropriate labeled
1624C E
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compounds are available and when interferences do not preclude the
analysis. If labeled compounds are not available, or interferences
are present, the internal standard method (section 7.5) is used. A
calibration curve encompassing the concentration range of interest
is prepared for each compound determined. The relative response
(RR) vs concentration (ug/L) is plotted or computed using a linear
regression. An example of a calibration curve for toluene using
toluene-d8 is given in figure 6. Also shown are the +/- 10 percent
error limits (dotted lines). Relative response is determined
according to the procedures described below. A minimum of five
data points are required for calibration (section 7.4.4).
7.4.1 The relative response (RR) of pollutant to labeled compound is
determined from isotope ratio values calculated from acquired data.
Three isotope ratios are used in this process:
Rx = the isotope ratio measured in the pure pollutant (figure
7A) .
Ry - the isotope ratio of pure labeled compound (figure 7B).
Rm = the isotope ratio measured in the analytical mixture of the
pollutant and labeled compounds (figure 7C)
The correct way to calculate RR is:
RR = (Ry - Rm)(Rx + l)/(Rm - Rx)(Ry + 1)
If Rm is not between 2Ry and 0.5RX, the method does not apply
and the sample is analyzed by the internal standard method (section
7.5) .
7.4.2 In most cases, the retention times of the pollutant and labeled
compound are the same and isotope ratios (R's) can be calculated
from the EICP areas, where:
R = (area at m1/z)/(area at 11*2/2)
If either of the areas is zero, it is assigned a value of one in
1624C E-118
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the calculations; that is, if: area of m]/z = 50721, and area of
m2/z = O/ then R = 50721/1 » 50720. The m/z's are always
selected such that Rx > Ry.
When there is a difference in retention times (RT) between the
pollutant and labeled compounds, special precautions are required
to determine the isotope ratios. Rx, Ry, and Rm are defined
as follows:
Rx =» [area m^/z (at RT^) ]/l
Ry = l/[area ffl2/z (at RT2) ]
Rm = [area m^z (at RT]_)]/[area m2/z (at RT2) ]
7.4.3 An example of the above calculations can be taken from the data
plotted in figure 6 for toluene and toluene-da. For these data, Rx
= 168920/1 » 168900, Ry » 1/60960 - 0.00001640, and Rm =
96868/82508 = 1.174. The RR for the above data is then calculated
using the equation given in section 7.4.1. For the example, RR =
1.174.
Not all labeled compounds elute before their pollutant analogs.
7.4.4 To calibrate the analytical system by isotope dilution, analyze
a 5 mL aliquot of each of the aqueous calibration standards
(section 6.7.1) spiked with an appropriate constant amount of the
labeled compound spiking solution (section 6.6), using the purge
and trap procedure in section 10. Compute the RR at each concen-
tration.
7.4.5 Linearityif the ratio of relative response to concentration
for any compound is constant (less than 20 percent coefficient of
variation) over the 5 point calibration range, an averaged relative
response/concentration ratio may be used for that compound;
otherwise, the complete calibration curve for that compound shall
be used over the 5 point calibration range.
1624C E_119
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7.5 Calibration by internal standardused when criteria for isotope
dilution (section 7.4) cannot be met. The method is applied to
pollutants having no labeled analog and to the labeled compounds.
The internal standards used for volatiles analyses are bromochloro-
methane, 2-bromo-l-chloropropane, and 1,4-dichlorobutane. Concen-
trations of the labeled compounds and pollutants without labeled
analogs are computed relative to the nearest eluted internal
standard, as shown in tables 3 and 5.
7.5.1 Response factorscalibration requires the determination of
response factors (RF) which are defined by the following equation:
RF = (As x Cis)/(Ais x Cs), where
As is the EICP area at the characteristic m/z for the compound in
the daily standard.
A^s is the EICP area at the characteristic m/z for the internal
standard.
Cj^s is the concentration (ug/L) of the internal standard.
Cs is the concentration of the pollutant in the daily standard.
7.5.2 The response factor is determined at 10, 20, 50, 100, and 200
ug/L for the pollutants (optionally at five times these concentra-
tions for gases and water soluble pollutantssee section 6.7), in
a way analogous to that for calibration by isotope dilution
(section 7.4.4). The RF is plotted against concentration for each
compound in the standard (Cs) to produce a calibration curve.
7.5.3 Linearityif the response factor (RF) for any compound is
constant (less than 35 percent coefficient of variation) over the 5
point calibration range, an averaged response factor may be used
for that compound; otherwise, the complete calibration curve for
that compound shall be used over the 5 point range.
7.6 Combined calibrationby adding the isotopically labeled compounds
1624C E-120
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and internal standards (section 6.6) to the aqueous calibration
standards (section 6.7.1), a single set of analyses can be used to
produce calibration curves for the isotope dilution and internal
standard methods. These curves are verified each shift (section
11.5) by purging the aqueous performance standard (section 6.7.2).
Recalibration is required only if calibration and on-going perfor-
mance (section 11.5) criteria cannot be met.
7.7 Elevated purge temperature calibrationsamples containing greater
than one percent solids are analyzed at a temperature of 40 +/~ 2
°C (section 10). For these samples, the analytical system may be
calibrated using a purge temperature of40+/-2°Cin order to
more closely approximate the behavior of the compounds of interest
in high solids samples.
8 Quality assurance/quality control
8.1 Each laboratory that uses this method is required to operate a
formal quality assurance program (reference 8). The minimum
requirements of this program consist of an initial demonstration of
laboratory capability, analysis of samples spiked with labeled
compounds to evaluate and document data quality, and analysis of
standards and blanks as tests of continued performance. Laboratory
performance is compared to established performance criteria to
determine if the results of analyses meet the performance charac-
teristics of the method.
3.1.1 The analyst shall make an initial demonstration of the ability
to generate acceptable accuracy and precision with this method.
This ability is established as described in section 8.2.
8.1.2 The analyst is permitted to modify this method to improve
separations or lower the costs of measurements, provided all
1624C E-121
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performance specifications are met. Each time a modification is
made to the method, the analyst is required to repeat the procedure
in section 8.2 to demonstrate method performance.
8.1.3 Analyses of blanks are required to demonstrate freedom from
contamination and that the compounds of interest and interfering
compounds have not been carried over from a previous analysis
(section 3). The procedures and criteria for analysis of a blank
are described in sections 8.5.
8.1.4 The laboratory shall spike all samples with labeled compounds to
monitor method performance. This test is described in section 8.3.
When results of these spikes indicate atypical method performance
for samples, the samples are diluted to bring method performance
within acceptable limits (section 14.2).
8.1.5 The laboratory shall, on an on-going basis, demonstrate through
the analysis of the aqueous performance standard (section 6.7.2)
that the analysis system is in control. This procedure is
described in sections 11.1 and 11.5.
8.1.6 The laboratory shall maintain records to define the quality of
data that is generated. Development of accuracy statements is
described in sections 8.4 and 11.5.2.
8.2 Initial precision and accuracyto establish the ability to
generate acceptable precision and accuracy, the analyst shall
perform the following operations for compounds to be calibrated:
3.2.1 Analyze two sets of four 5-mL aliquots (8 aliquots total) of the
aqueous performance standard (section 6.7.2) according to the
method beginning in section 10.
3.2.2 Using results of the first set of four analyses in section
8.2.1, compute the average recovery (X) in ug/L and the standard
deviation of the recovery (s) in ug/L for each compound, by isotope
1624C E-122
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dilution for pollutants with a labeled analog, and by internal
standard for labeled compounds and pollutants with no labeled
analog.
8.2.3 For each compound, compare s and X with the corresponding limits
for initial precision and accuracy found in table 6. If s and X
for all compounds meet the acceptance criteria, system performance
is acceptable and analysis of blanks and samples may begin. If,
however, any individual s exceeds the precision limit or any
individual X falls outside the range for accuracy, system perfor-
mance is unacceptable for that compound.
NOTE: The large number of compounds in table 6 present a
substantial probability that one or more will fail one of the
acceptance criteria when all compounds are analyzed. To determine
if the analytical system is out of control, or if the failure can
be attributed to probability, proceed as follows:
8.2.4 Using the results of the second set of four analyses, compute s
and X for only those compounds which failed the test of the first
set of four analyses (section 8.2.3). If these compounds now pass,
system performance is acceptable for all compounds and analysis of
blanks and samples may begin. If, however, any of the same
compounds fail again, the analysis system is not performing
properly for the compound (s) in question. In this event, correct
the problem and repeat the entire test (section 8.2.1).
8.3 The laboratory shall spike all samples with labeled compounds to
assess method performance on the sample matrix.
8.3.1 Spike and analyze each sample according to the method beginning
in section 10.
8.3.2 Compute the percent recovery (P) of the labeled compounds using
the internal standard method (section 7.5).
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8.3.3 Compare the percent recovery for each compound with the corre-
sponding labeled compound recovery limit in table 6. If the
recovery of any compound falls outside its warning limit, method
performance is unacceptable for that compound in that sample.
Therefore, the sample matrix is complex and the sample is to be
diluted and reanalyzed, per section 14.2.
8.4 As part of the QA program for the laboratory, method accuracy for
wastewater samples shall be assessed and records shall be main-
tained. After the analysis of five wastewater samples for which
the labeled compounds pass the tests in section 3.3.3, compute the
average percent recovery (P) and the standard deviation of the
percent recovery (SQ) for the labeled compounds only. Express the
accuracy assessment as a percent recovery interval from P - 2Sp to
P + 2Sp. For example, if P = 90% and sp » 10%, the accuracy
interval is expressed as 70 - 110%. Update the accuracy assessment
for each compound on a regular basis (e.g. after each 5-10 new
accuracy measurements).
3.5 Blanksreagent water blanks are analyzed to demonstrate freedom
from carry-over (section 3) and contamination.
8.5.1 The level at which the purge and trap system will carry greater
than 5 ug/L of a pollutant of interest (tables 1 and 2) into a
succeeding blank shall be determined by analyzing successively
larger concentrations of these compounds. When a sample contains
this concentration or more, a blank shall be analyzed immediately
following this sample to demonstrate no carry-over at the 5 ug/L
level.
8.5.2 With each sample lot (samples analyzed on the same 8 hr shift),
a blank shall be analyzed immediately after analysis of the aqueous
performance standard (section 11.1) to demonstrate freedom from
1624C E-124
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contamination. If any of the compounds of interest (tables 1 and
2) or any potentially interfering compound is found in a blank at
greater than 10 ug/L (assuming a response factor of 1 relative to
the nearest eluted internal standard for compounds not listed in
tables 1 and 2), analysis of samples is halted until the source of
contamination is eliminated and a blank shows no evidence of
contamination at this level.
8.6 The specifications contained in this method can be met if the
apparatus used is calibrated properly, then maintained in a
calibrated state. The standards used for calibration (section 7),
calibration verification (section 11.5) and for initial (section
8.2) and on-going (section 11.5) precision and accuracy should be
identical, so that the most precise results will be obtained. The
GCMS instrument in particular will provide the most reproducible
results if dedicated to the settings and conditions required for
the analyses of volatiles by this method.
8.7 Depending on specific program requirements, field replicates may
be collected to determine the precision of the sampling technique,
and spiked samples may be required to determine the accuracy of the
analysis when the internal method is used.
9 Sample collection, preservation, and handling
9.1 Grab samples are collected in glass containers having a total
volume greater than 20 mL. For aqueous samples which pour freely,
fill sample bottles so that no air bubbles pass through the sample
as the bottle is filled and seal each bottle so that no air bubbles
are entrapped. Maintain the hermetic seal on the sample bottle
until time of analysis.
9.2 Samples are maintained at 0 - 4 °C from the time of collection
1624C E-125
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until analysis. If an aqueous sample contains residual chlorine,
add sodium thiosulfate preservative (10 mg/40 mL) to the empty
sample bottles just prior to shipment to the sample site. EPA
Methods 330.4 and 330.5 may be used for measurement of residual
chlorine (reference 9). If preservative has been added, shake the
bottle vigorously for one minute immediately after filling.
9.3 For aqueous samples, experimental evidence indicates that some
aromatic compounds, notably benzene, toluene, and ethyl benzene are
susceptible to rapid biological degradation under certain environ-
mental conditions. Refrigeration alone may not be adequate to
preserve these compounds in wastewaters for more than seven days.
For this reason, a separate sample should be collected, acidified,
and analyzed when these aromatics are to be determined. Collect
about 500 mL of sample in a clean container. Adjust the pH of the
sample to about 2 by adding HCl (1+1) while stirring. Check pH
with narrow range (1.4 to 2.8) pH paper. Fill a sample container
as described in section 9.1. If residual chlorine is present, add
sodium thiosulfate to a separate sample container and fill as in
section 9.1.
9.4 All samples shall be analyzed within 14 days of collection.
10 Purge, trap, and GCMS analysissamples containing less than one
percent solids are analyzed directly as aqueous samples (section
10.4). Samples containing greater one percent solids or greater
are analyzed as solid samples (section 10.5).
10.1 Determination of percent solids
10.1.1 Weigh 5 - 10 g of sample into a tared beaker.
10.1.2 Dry overnight (12 hours minimum) at 110 +/- 5 °C, and cool in a
dessicator.
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10.1.3 Determine percent solids as follows:
% solids = weight of sample drv x 100
weight of sample wet
10.2 Remove standards and samples from cold storage and bring to 20 -
25 °C.
10.3 Adjust the purge gas flow rate to 40 +/~ 4 mL/min.
10.4 Samples containing less than one percent solids
10.4.1 Mix the sample by shaking vigorously. Remove the plunger from a
5 mL syringe and attach a closed syringe valve. Open the sample
bottle and carefully pour the sample into the syringe barrel until
it overflows. Replace the plunger and compress the sample. Open
the syringe valve and vent any residual air while adjusting the
sample volume to 5.0 +/- 0.1 mL. Because this process of taking an
aliquot destroys the validity of the sample for future analysis,
fill a second syringe at this time to protect against possible loss
of data.
10.4.2 Add an appropriate amount of the labeled compound spiking
solution (section 6.6) through the valve bore, then close the
valve.
10.4.3 Attach the syringe valve assembly to the syringe valve on the
purging device. Open both syringe valves and inject the sample
into the purging chamber. Purge the sample per section 10.6.
10.5 Weighing of samples containing one percent solids or greater.
10.5.1 Mix the sample thoroughly using a clean spatula.
10.5.2 Weigh 5 +/~ 1 grams of sample into a purging vessel (figure 2).
Record the weight to three significant figures.
10.5.3 Add 5.0 +/- 0.1 mL of reagent water to the vessel.
10.5.4 Using a metal spatula, break up any lumps of sample to disperse
the sample in the water.
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10.5.5 Add an appropriate amount of the labeled compound spiking
solution (section 6.6) to the sample in the purge vessel. Place a
cap on the purging vessel and and shake vigorously to further
disperse the sample. Attach the purge vessel to the purging
device.
10.6 Purge the sample for 11.0 +/" °-l minutes at 20 - 25 °C for
samples containing less than one percent solids. Purge samples
containing one percent solids or greater at 40 +/- 2 °C. If the
compounds in table 2 that do not purge at 20 - 40 °C are to be
determined, a purge temperature of 80 +/- 5 °C is used.
10.7 After the 11 minute purge time, attach the trap to the chromato-
graph and set the purge and trap apparatus to the desorb mode
(figure 5). Desorb the trapped compounds into the GC column by
heating the trap to 170 -180 °C while backflushing with carrier gas
at 20 - 60 mL/min for four minutes. Start MS data acquisition upon
start of the desorb cycle, and start the GC column temperature
program 3 minutes later. Table 3 summarizes the recommended
operating conditions for the gas chromatograph. Included in this
table are retention times and minimum levels that can be achieved
under these conditions. An example of the separations achieved by
the column listed is shown in figure 9. Other columns may be used
provided the requirements in section 8 are met. If the priority
pollutant gases produce GC peaks so broad that the precision and
recovery specifications (section 8.2) cannot be met, the column may
be cooled to ambient or sub-ambient temperatures to sharpen these
peaks.
10.8 After desorbing the sample for four minutes, recondition the
trap by purging with purge gas while maintaining the trap tempera-
ture at 170 - 180 °C. After approximately seven minutes, turn off
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the trap heater to stop the gas flow through the trap. When cool,
the trap is ready for the next sample.
10.9 While analysis of the desorbed compounds proceeds, remove and
clean the purge device. Rinse with tap water, clean with detergent
and water, rinse with tap and distilled water, and dry for one hour
minimum in an oven at a temperature greater than 150 °C.
11 System performance
ll.l At the beginning of each 8 hr shift during which analyses are
performed, system calibration and performance shall be verified for
the pollutants and labeled compounds (table 1). For these tests,
analysis of the aqueous performance standard (section 6.7.2) shall
be used to verify all performance criteria. Adjustment and/or
recalibration (per section 7) shall be performed until all perfor-
mance criteria are met. Only after all performance criteria are
met may blanks and samples be analyzed.
11.2 BFB spectrum validitythe criteria in table 4 shall be met.
11.3 Retention timesthe absolute retention times of the internal
standards shall be as follows: bromochloromethane: 653 - 782
seconds; 2-bromo-l-chloropropane: 1270 - 1369 seconds;
1,4-dichlorobutane: 1510 - 1605 seconds. The relative retention
times of all pollutants and labeled compounds shall fall within the
limits given in table 3.
11.4 GC resolutionthe valley height between toluene and toluene-d8
(at m/z 91 and 99 plotted on the same graph) shall be less than 10
percent of the taller of the two peaks.
11.5 Calibration verification and on-going precision and accuracy
compute the concentration of each pollutant (table 1) by isotope
dilution (section 7.4) for those compounds which have labeled
1624C E-129
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analogs. Compute the concentration of each pollutant (table 1)
which has no labeled analog by the internal standard method
(section 7.5). Compute the concentration of the labeled compounds
by the internal standard method. These concentrations are computed
based on the calibration data determined in section 7.
11.5.1 For each pollutant and labeled compound, compare the concentra-
tion with the corresponding limit for on-going accuracy in table 6.
If all compounds meet the acceptance criteria, system performance
is acceptable and analysis of blanks and samples may continue. If
any individual value falls outside the range given, system perfor-
mance is unacceptable for that compound.
NOTE: The large number of compounds in table 6 present a
substantial probability that one or more will fail the acceptance
criteria when all compounds are analyzed. To determine if the
analytical system is out of control, or if the failure may be
attributed to probability, proceed as follows:
11.5.1.1 Analyze a second aliquot of the aqueous performance standard
(section 6.7.2).
11.5.1.2 Compute the concentration for only those compounds which
failed the first test (section 11.5.1). If these compounds now
pass, system performance is acceptable for all compounds and
analyses of blanks and samples may proceed. If, however, any of
the compounds fail again, the measurement system is not performing
properly for these compounds. In this event, locate and correct
the problem or recalibrate the system (section 7), and repeat the
entire test (section 11.1) for all compounds.
11.5.2 Add results which pass the specification in 11.5.1.2 to initial
(section 8.2) and previous on-going data. Update QC charts to form
a graphic representation of laboratory performance (figure 8).
1624C E-130
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Develop a statement of accuracy for each pollutant and labeled
compound by calculating the average percent recovery (R) and the
standard deviation of percent recovery (sr). Express the accuracy
as a recovery interval from R - 2sr to R + 2sr. For example, if R
= 95% and sr = 5%, the accuracy is 85 - 105 percent.
12 Qualitative determinationidentification is accomplished by
comparison of data from analysis of a sample or blank with data
stored in the mass spectral libraries. For compounds for which the
relative retention times and mass spectra are known, identification
is confirmed per sections 12.1 and 12.2. For unidentified GC
peaks, the spectrum is compared to spectra in the EPA/NIH mass
spectral file per section 12.3.
12.1 Labeled compounds and pollutants having no labeled analog (tables
1 and 2) :
12.1.1 The signals for all characteristic m/z's stored in the spectral
library (section 7.2.4) shall be present and shall maximize within
the same two consecutive scans.
12.1.2 Either (1) the background corrected EICP areas, or (2) the
corrected relative intensities of the mass spectral peaks at the GC
peak maximum shall agree within a factor of two (0.5 to 2 times)
for all masses stored in the library.
12.1.3 For the compounds for which the system has been calibrated
(table 1), the relative retention time shall be within the windows
specified in table 3.
12.1.4 For the compounds for which the system has not been calibrated
but the relative retention times and mass spectra are known (table
2), the retention time relative to the internal standard specified
in table 3 shall be within +/- 20 scans or +/- 60 seconds,
1624C E-131
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whichever is greater, based on the nominal relative retention time
specified in table 3.
12.2 Pollutants having a labeled analog (table 1):
12.2.1 The signals for all characteristic m/z's stored in the spectral
library (section 7.2.4) shall be present and shall maximize within
the same two consecutive scans.
12.2.2 Either (1) the background corrected EICP areas, or (2) the
corrected relative intensities of the mass spectral peaks at the GC
peak maximum shall agree within a factor of two for all masses
stored in the spectral library.
13.2.3 The relative retention time between the pollutant and its
labeled analog shall be within the windows specified in table 3.
12.3 Unidentified GC peaks
12.3.1 The signals for m/z's specific to a GC peak shall all maximize
within the same two consecutive scans.
12.3.2 Either (1) the background corrected EICP areas, or (2) the cor-
rected relative intensities of the mass spectral peaks at the GC
peak maximum shall agree within a factor of two with the masses
stored in the EPA/NIH Mass Spectral File.
12.4 M/z's present in the experimental mass spectrum that are not
present in the reference mass spectrum shall be accounted for by
contaminant or background ions. If the experimental mass spectrum
is contaminated, or if identification is ambiguous, an experienced
spectrometrist (section 1.4) is to determine the presence or
absence of the compound.
13 Quantitative determination
13.1 Isotope dilutionby adding a known amount of a labeled compound
to every sample prior to purging, correction for recovery of the
1624C E-132
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pollutant can be made because the pollutant and its labeled analog
exhibit the same effects upon purging, desorption, and gas chroma-
tography. Relative response (RR) values for sample mixtures are
used in conjunction with calibration curves described in section
7.4 to determine concentrations directly, so long as labeled
compound spiking levels are constant. For the toluene example
given in figure 7 (section 7.4.3), RR would be equal to 1.174. For
this RR value, the toluene calibration curve given in figure 6
indicates a concentration of 31.8 ug/L.
13.2 Internal standardcalculate the concentration using the response
factor determined from calibration data (section 7.5) for the
compounds which were calibrated (table 1), or from table 5 for
compounds which were not calibrated (table 2), using the following
equation:
Concentration = (As x Cj_s)/(&is x RF)
where the terms are as defined in section 7.5.1.
13.3 The concentration of the pollutant in the solid phase of the
sample is computed using the concentration of the pollutant
detected in the aqueous solution, as follows:
Concentration in solid (ug/kg) = 0.005 L x aqueous cone (ua/L)
0.01 x % solids (g)
where "% solids" is from section 10.1.3.
13.4 If the EICP area at the quantitation m/z exceeds the calibration
range of the system, the sample is diluted with reagent water by
successive factors of 10 and the dilutions are analyzed until the
area is within the calibration range.
13.5 For GC peaks which are to be identified (per section 12.3), the
sample is diluted by successive factors of 10 when any peak in the
uncorrected mass spectrum at the GC peak maximum is saturated.
13.6 Report results for all pollutants, labeled compounds, and
1624C £-133
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tentatively identified compounds found in all standards, blanks,
and samples, in ug/L for samples containing less than one percent
solids and in ug/kg for samples in which the undilute sample
contains one percent solids or greater, to three significant
figures. Results for samples which have been diluted are reported
at the least dilute level at which the area at the quantitation m/z
is within the calibration range (section 13.4) or at which no m/z
in the spectrum is saturated (section 13.5). For compounds having
a labeled analog, results are reported at the least dilute level at
which the area at the quantitation m/z is within the calibration
range (section 13.4) and the labeled compound recovery is within
the normal range for the method (section 14.2).
y
14 Analysis of complex samples
14.1 Some samples may contain high levels (>1000 ug/kg) of the com-
pounds of interest and of interfering compounds. Some samples will
foam excessively when purged; others will overload the trap/or GC
column.
14.2 Dilute 0.5 mL of samples containing less than one percent solids
or 0.5 gram of samples containing one percent solids or greater
with 4.5 mL of reagent water and analyze this diluted sample when
the recovery of any labeled compound is outside the range given in
table 6. If the recovery remains outside of the range for this
diluted sample, the aqueous performance standard shall be analyzed
(section 11) and calibration verified (section 11.5). If the
recovery for the labeled compound in the aqueous performance
standard is outside the range given in table 6, the analytical
system is out of control. In this case, the instrument shall be
repaired, the performance specifications in section 11 shall be
1624C E-134
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met, and the analysis of the undiluted sample shall be repeated.
If the recovery for the aqueous performance standard is within the
range given in table 6, the method does not work on the sample
being analyzed and the result may not be reported for regulatory
compliance purposes.
14.3 Reverse search computer programs can misinterpret the spectrum of
chromatographically unresolved pollutant and labeled compound pairs
with overlapping spectra when a high level of the pollutant is
present. Examine each chromatogram for peaks greater than the
height of the internal standard peaks. These peaks can obscure the
compounds of interest.
15 Method performance
15.1 The specifications for this method were taken from the interlabo-
ratory validation of EPA Method 624 (reference 10). Method 1624 has
been shown to yield slightly better performance on treated efflu-
ents than method 624. Results of initial tests of this method at a
purge temperature of 80 °C can be found in reference 11 and results
of initial tests of this method on municipal sludge can be found in
reference 12.
1624C E-135
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References
1. "Performance Tests for the Evaluation of Computerized Gas Chroma-
tography/Mass Spectrometry Equipment and Laboratories," USEPA, EMSL
Cincinnati, OH 45268, EPA-600/4-80-025 (April 1980).
2. Bellar, T. A. and Lichtenberg, J. J., "Journal American Water Works
Association," 66/ 739 (1974).
3. Bellar, T. A. and Lichtenberg, J. J., "Semi-automated Headspace
Analysis of Drinking Waters and Industrial Waters for Purgeable
Volatile Organic Compounds," in Measurement of Organic Pollutants
in Water and Wastewater. C. E. VanHall, ed., American Society for
Testing Materials, Philadelphia, PA, Special Technical Publication
686, (1978) .
4. National Standard Reference Data System, "Mass Spectral Tape
Format", US National Bureau of Standards (1979 and later attach-
ments) .
5. "Working with Carcinogens," DHEW, PHS, NIOSH, Publication 77-206
(1977).
6. "OSHA Safety and Health Standards, General Industry," 29 CFR 1910,
OSHA 2206, (1976).
7. "Safety in Academic Chemistry Laboratories," American Chemical
Society Publication, Committee on Chemical Safety (1979).
3. "Handbook of Analytical Quality Control in Water and Wastewater
Laboratories," USEPA, EMSL Cincinnati, OH 45268, EPA-4-79-019
(March 1979).
9. "Methods 330.4 and 330.5 for Total Residual Chlorine," USEPA, EMSL
Cincinnati, OH 45268, EPA-4-79-020 (March 1979).
10. "Method 624Purgeables", 40 CFR Part 136 (49 FR 43234), 26 October
1984.
11. "Narrative for SAS 106: Development of an Isotope Dilution GC/MS
Method for Hot Purge and Trap Volatiles Analysis", S-CUBED Division
of Maxwell Laboratories, Inc., Prepared for W. A. Telliard,
Industrial Technology Division (WH-552), USEPA, 401 M St SW,
Washington DC 20460 (July 1986).
12. Colby, Bruce N. and Ryan, Philip W., "Initial Evaluation of
Methods 1634 and 1635 for the analysis of Municipal Wastewater
Treatment Sludges by Isotope Dilution GCMS", Pacific Analytical
Inc., Prepared for W. A. Telliard, Industrial Technology Division
(WH-552), USEPA, 401 M St SW, Washington DC 20460 (July 1986).
1624C E-136
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Table 1
Volatile Organic Compounds Determined by Calibrated GCMS using Isotope
Dilution and Internal Standard Techniques
Pollutant
Labeled Compound
Comoound
acetone
acrolein
acrytonitrile
benzene
bromod i ch I oromethane
bromoform
bronoflie thane
carbon tetrachloride
chlorobenzene
chloroethane
2-chloroethylvinyl ether
chloroform
chloromethane
di bromoch I oromethane
1 , 1 -dichloroethan*
1 ,2-dichloroethane
1 , 1 dichloroethen*
trans- 1 ,2-dichtorethene
1 , 2 - d i ch I oropropane
t r ans 1 , 3 d i eh I oropropene
diethyl ether
p-dioxane
ethyl benzene
methylene chloride
methyl ethyl ketone
1 , 1 ,2,2- tetrachloroethane
tetrsehlorethene
toluene
1,1,1- trichloroethane
1 , 1 ,2- trichloroethane
trichloroethene
vinyl chloride
Storet
31552
34210
34215
34030
32101
32104
34413
32102
34301
34311
34576
32106
34418
32105
34496
32103
34501
34546
34541
34699
81576
81582
34371
34423
81595
34516
34475
34010
34506
34511
39180
39175
CAS Registry
67-64-1
107-02-8
107-13-1
71-43-2
75-27-4
75-25-2
74-83-9
56-23-5
108-90-7
75-00-3
110-75-8
67-66-3
74-87-3
124-48-1
75-34-3
107-06-2
75-35-4
156-60-5
78-87-5
10061-02-6
60-29-7
123-91-1
100-41-4
75-09-2
78-93-3
79-34-5
127-18-4
108-88-3
71-55-6
79-00-5
79-01-6
75-01-4
EPA -EGO
516 V
002 V
003 V
004 V
048 V
047 V
046 V
006 V
007 V
016 V
019 V
023 V
045 V
051 V
013 V
010 V
029 V
030 V
032 V
033 V
515 V
527 V
038 V
044 V
514 V
015 V
085 V
086 V
011 V
014 V
087 V
088 V
NPOE5
001 V
002 V
003 V
012 V
005 V
020 V
006 V
007 V
009 V
010 V
011 V
021 V
008 V
014 V
015 V
016 V
026 V
017 V
019 V
022 V
023 V
024 V
025 V
027 V
028 V
029 V
031 V
Ana I og
66
d4
d3
d6
13C
13C
d3
13C
dS
d5
13C
d3
13C
d3
d4
d2
d3
d6
d4
d10
d8
d10
d2
d3
d2
13C2
d8
d3
13C2
13C2
d3
CAS Registry
666-52-4
33984-05-3
53807-26-4
1076-43-3
93952-10-4
72802-81-4
1111-88-2
32488-50-9
3114-55-4
19199-91-8
31717-44-9
1111-89-3
93951-99-6
56912-77-7
17070-07-0
22280-73-5
42366-47-2
93952-08-0
93951-86-1
2679-89-2
17647-74-4
25837-05-2
1665-00-5
53389-26-7
33685-54-0
32488-49-6
2037-26-5
2747-58-2
93952-09-1
93952-00-2
6745-35-3
EPA -EGO
616 V
202 V
203 V
204 V
248 V
247 V
246 V
206 V
207 V
216 V
223 V
245 V
251 V
213 V
210 V
229 V
230 V
232 V
233 V
615 V
627 V
238 V
244 V
614 V
215 V
285 V
286 V
211 V
214 V
287 V
288 V
1624C
E-137
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Table 2
Volatile Organic Compounds to be Determined by Reverse Search and Quantita-
tion using Known Retention Times, Response Factors, Reference Compounds,
and Mass Spectra
EGD CAS
No. Compound Registry
532 allyl alcohol* 107-18-6
533 carbon disulfide 75-15-0
534 2-chloro-l,3-butadiene (chloroprene) 126-99-8
535 chloroacetonitrile* 107-14-2
536 3-chloropropene 107-05-1
537 crotonaldehyde* 123-73-9
538 1,2-dibromoethane (EDB) 106-93-4
539 dibromomethane 74-95-3
540 trans-l,4-dichloro-2-butene 110-47-6
541 1,3-dichloropropane 142-28-9
542 cis-l,3-dichloropropene 10061-01-5
543 ethyl cyanide* 107-12-0
544 ethyl methacrylate 97-63-2
545 2-hexanone 591-78-6
546 iodomethane 74-88-4
547 isobutyl alcohol* 78-83-1
548 methacrylonitrile 126-98-7
549 methyl methacrylate 78-83-1
550 4-methyl-2-pentanone 108-10-1
551 1,1,1,2-tetrachloroethane 630-20-6
552 trichlorofluoromethane 75-69-4
553 1,2,3-trichloropropane 96-18-4
554 vinyl acetate . 108-05-4
*determined at a purge temperature of 75 - 85 °C
1624C E-138
-------
Table 3
Gas Chromatography of Purgeable Organic Compounds
Mini-
mum
EGO
No.
ill
245
345
246
346
288
388
216
316
244
344
546
616
716
202
302
203
303
533
552
543
229
329
536
532
181
213
313
615
715
230
330
614
714
223
323
535
210
310
539
548
547
211
311
627
727
206
306
554
248
Retention time
Compound
chloromethane-cS
chlorome thane
bromomethane-d3
bromomethane
vinyl chloride-d3
vinyl chloride
chloroethane-dS
crUoroe thane
methylene chloride-d2
methylene chloride
iodomethane
acetone-d6
acetone
acrolein-d4
acrolein
acrylonitri Ie-d3
acrylonitrile
carbon disulfide
trichlorof luoromethane
ethyl cyanide
1,1-diehloroethene-d2
1 , 1-dichloroethene
3-chloropropene
allyl alcohol
bromochloromethane (I.S.)
1,1-dichlopoethane-d3
1 ,1-dichloroethane
diethyl ether-d10
diethyl ether
trans- 1 ,2-dichloroethene-d2
trans- 1 ,2-dichloroethene
methyl ethyl ketone-d3
methyl ethyl ketone
chloroform- 13C1
chloroform
chloroacetonitrile
1 ,2-dichloroethane-d4
1 ,2-dichloroethane
dibromocnethane
methacrylonitri le
isobutyl alcohol
1,1,1- trichloroethane- 13C2
1,1,1- trichloroethane
p-dioxane-dS
p-dioxane
carbon tetrachloride- 13C1
carbon tetrachloride
vinyl acetate
bromodichloromethane- 13C1
Mean
(see)
147
148
243
246
301
304
378
386
512
517
498
554
565
564
566
606
612
631
663
672
696
696
696
703
730
778
786
S04
820
821
321
840
348
361
361
384
901
910
910
921
962
989
999
982
1001
1018
1018
1031
1045
EGO
Ref
181
245
181
246
181
288
181
216
181
244
181
181
616
181
202
181
203
181
181
181
181
229
181
181
181
181
213
181
615
181
230
181
614
181
223
181
181
210
181
181
181
181
211
181
627
182
206
182
182
level
(3)
Relative
0
0
0
0
0
0
0
0
0
0
0
0
0
0
.141
.922
.233
.898
.286
.946
.373
.999
.582
.999
0
.628
.984
.641
.984
0.735
0
0
0
1
1
0
1
1
1
0
0
0
1
0
1
0
1
0
1
1
0
0
0
.985
0
0
0
.903
.999
0
0
.000
.031
.999
.067
.010
.056
.996
.646
.992
.092
.961
1
.187
.973
1
1
1
.293
.989
.262
.008
.754
.938
0
.766
0
1
- 0
- 1
- 0
1
- 0
- 1
- 0
1
.68
0
1
0
1
0
- 1
.86
.91
.92
- 0
- 1
.95
.96
- 1
1
1
1
- 1
1
1
- 1
- 1
- 1
1
.21
- 1
- 1
.25
.26
.32
- 1
1
- 1
1
0
- 1
.79
- 0
(2} (ug/Ll
.270
.210
.423
.195
.501
.023
.620
.060
.813
.017
.389
.019
.903(5)
.018(5)
.926
.030
.976
.011
.000
.119
.014
.254
.048
.223
.011
.202
.055
.322
.009
.416
.032
.598
.044
.448(5)
.040(5)
.805
.005
.325
50
50
50
50
50
10
50
50
10
10
50
50
50
50
50
50
10
10
10
10
10
50
50
10
10
50
50
10
10
10
10
10
10
10
10
10
10
10
Method Detection
Limit (4)
Low
solids
(no/kg)
207*
148*
190*
789*
566*
3561*
377*
360*
31
16
63
41
241*
21
23
16
-
87
High
solids
(uq/kq)
13
11
11
24
280*
322*
18
9
5
1
12
3
80*
2
3
4
140*
9
1624C
E-139
-------
348 bromodichloromethane 1045 248 0.978 - 1.013 10 28 3
534 2-chloro-1,3-butadiene 1084 182 0.83
537 crotonaldehyde 1098 182 0.84
232 1,2-dichloropropane-d6 1123 182 0.830 0.880 10
332 1,2-dichloropropane 1134 232 0.984 - 1.018 10 29 5
542 cis-1,3-dichloropropene 1138 182 0.37
287 trtchloroethene-13C2 1172 182 0.897 - 0.917 10
387 trichtoroethene 1187 287 0.991 1.037 10 41 2
541 1,3-dichloropcopane 1196 182 0.92
204 benzene-d6 1200 182 0.888 0.952 10
304 benzene 1212 204 1.002 1.026 10 23 3
251 chlorodibronwmethane-13C1 1222 182 0.915 - 0.949 10
351 chlorodibromomethane 1222 251 0.989 - 1.030 10 15 2
214 1,1,2-trichloroethane-13C2 1224 182 0.922 - 0.953 10
314 1,1,2-trichloroethan* 1224 214 0.975 1.027 10 26 1
233 trans-1,3-dichloropropene-d4 1226 182 0.922 - 0.959 10
333 trans-1,3-dtchloropropen« 1226 233 0.993 1.016 10 (6)» (6)"
019 2-cfHoroethylvinyl ether 1278 182 0.983 1.026 10 122 21
538 1,2-dibromoethane 1279 182 0.98
182 2-bromo-l-chloropropane (I.S.) 1306 182 1.000 - 1.000 10
549 methyl methacrylate 1379 182 1.06
247 bromoform-13C1 1386 182 1.048 1.087 10
347 bromoforro 1386 247 0.992 - 1.003 10 91 7
551 1,1,1,2-tetrachtoroethane 1408 182 1.08
550 4-methyl-2-pentanone 1435 183 0.92
553 1,2,3-trichloropropane 1520 183 0.98
215 1,1,2,2-tetrachloroethane-d2 1525 183 0.969 0.996 10
315 1,1,2,2-tetrachloroethane 1525 215 0.890 1.016 10 20 6
545 2-hexanone 1525 183 0.98
285 tetrachloroethene-13C2 1528 183 0.966 - 0.996 10
385 tetrachloroethene 1528 285 0.997 - 1.003 10 106 10
540 trans-1,4-diehloro-2-butene 1551 183 1.00
183 1,4-dichlorobutane (int std) 1555 183 1.000 1.000 10
544 ethyl methacrylate 1594 183 1.03
286 toluene-d8 1603 183 1.016 - 1.054 10
386 toluene 1619 286 1.001 - 1.019 10 27 4
207 chlorobenzene-d5 1679 183 1.066 - 1.135 10
307 chlorobenzene 1679 207 0.914 1.019 10 21 58*
238 ethylbenzene-d10 1802 183 1.144 t.293 10
338 ethylbenzene 1820 238 0.981 1.018 10 28 4
185 bromofluorobenzene 1985 183 1.255-1.290 10
(1) Reference numbers beginning with 0, 1 or 5 indicate a pollutant quan-
tified by the internal standard method; reference numbers beginning with 2
or 6 indicate a labeled compound quantified by the internal standard
method; reference numbers beginning with 3 or 7 indicate a pollutant quan-
tified by isotope dilution.
(2) Based on data from a single wastewater laboratory.
(3) This is a minimum level at which the analytical system shall give rec-
ognizable mass spectra (background corrected) and acceptable calibration
points when calibrated using reagent water. The concentration in the
aqueous or solid phase is determined using the equations in section 13.
(4) Method detection limits determined in digested sludge (low solids) and
in filter cake or compost (high solids).
(5) Specification derived from related compound.
(6) An unknown interference in the particular sludge studied precluded
measurement of the Method Detection Limit (MDL) for this compound.
*Background levels of these compounds were present in the sludge resulting
1624C E-140
-------
in higher than expected MDL's. The MDL for these compounds is expected to
be approximately 20 ug/kg (100 - 200 for the gases and water soluble com-
pounds) for the low solids method and 5-10 ug/kg (25 - 50 for the gases
and water soluble compounds) for the high solids method, with no interfer-
ences present.
Column: 2.4 m (8 ft) x 2 mm i.d. glass, packed with one percent SP-1000
coated on 60/80 Carbopak B.
Carrier gas: helium at 40 mL/min.
Temperature program: 3 min at 45 °C, 8 °C per min to 240 °c, hold at 240 °C
for 15 minutes.
Note: The retention time specifications in this table were developed from
data collected from four wastewater laboratories.
1624C £-141
-------
Table 4
BFB Mass-intensity Specifications
M/z Intensity required
50 15 to 40 percent of m/z 95
75 30 to 60 percent of m/z 95
95 base peak, 100 percent
96 5 to 9 percent of m/z 95
173 less than 2 percent of m/z 174
174 greater than 50 percent of m/z 95
175 5 to 9 percent of m/z
176 95 to 100 percent of m/z 174
177 5 to 9 percent of m/z 176
1624C E-142
-------
Table 5
Volatile Organic Compound Characteristic M/z's
Response fac-
Compound
acetone
acrolein
acrylonitrile
allyl alcohol
benzene
2-bromo-l-chloropropane (3)
bromochloromethane (3)
bromodichloromethane
bromoform
bromomethane
carbon disulfide
carbon tetrachloride
2-chloro-l , 3 -butadiene
chloroacetonitrile
chlorobenzene
chloroethane
2-chloroethylvinyl ether
chloroform
chloromethane
3-chloropropene
crotonaldehyde
dibromochloromethane
1 , 2-dibromoethane
dibromomethane
1 , 4 -dichlorobutane ( 3 )
trans-1, 4-dichloro-2-butene
1, 1-dichloroethane
1 , 2-dichloroethane
1 , 1-dichloroethene
trans-1 , 2-dichlorethene
1 , 2-dichloropropane
1 , 3 -dichloropropane
cis-1, 3-dichloropropene
trans-1, 3-dichloropropene
diethyl ether
p-dioxane
ethyl cyanide
ethyl methacrylate
ethylbenzene
2-hexanone
iodomethane
isobutyl alcohol
methylene chloride
methyl ethyl ketorte
methyl methacrylate
4 -methyl -2 -pentanone
methacrylonitrile
1,1,1,2 -tetrachloroethane
1,1,2, 2 -tetrachloroethane
tetrachlorethene
Labeled
analog
d6
d4
d3
d6
13C
13c
d3
13C
d5
d5
d7
13C
d3
13C
d3
d4
d2
d2
d6
d4
dlO
d3
dlO
d2
d3
d2
13C2
1624C
Primary
m/z 's
58/64
56/60
53/56
57
78/84
77
128
83/86
173/176
96/99
76
47/48
53
75
112/117
64/71
106/113
85/86
50/52
76
70
129/130
107
93
55
75
63/66
62/67
61/65
61/65
63/67
76
75
75/79
74/84
88/96
54
69
106/116
58
142
74
84/88
72/75
69
58
67
131
83/84
166/172
E-14T
Reference
compound
m
181
181
182
181
181
182
182
181
183
182
182
181
183
183
181
181
182
183
181
182
tor at purge
temn.
10_°-C
(2)
1.93
0.29
(2)
0.43
(2)
0.86
1.35
0.093
0.89
0.29
(2)
0.69
0.076
4.55
(2)
0.23
0.15
0.25
0.20
of
80 °-C
0.20
2.02
0.50
1.12
0.63
0.090
0.68
1.91
0.14
0.88
0.41
1.26
0.52
0.33
2.55
0.22
0.79
0.29
0.79
0.25
-------
toluene
1,1,l-trichloroethane
1,1,2-trichloroethane
trichloroethene
trichlorofluoromethane
1,2,3-trichloropropane
vinyl acetate
vinyl chloride
(1)
d8
d3
"C2
13C2
d3
92/99
97/102
83/84
95/136
101
75
86
62/65
181 = bromochloromethane
182 = 2-bromo-l-chloropropane
183 = 1,4-dichlorobutane
(2) not detected at a purge temperature of 25 °C
(3) internal standard
181
183
182
2.31
0.89
0.054
2.19
0.72
0.19
1624C
E-144
-------
Table 6
Acceptance Criteria for Performance Tests
Acceptance criteria at 20 ua/L or as noted
Compound
Initial precision
and accuracy
Section 8.2.3
s fua/L}
51.
72.
16.
9.
8.
7.
25.
6.
8.
15.
36.
7.
26.
7.
6.
7.
12.
7.
19.
22.
15.
44.
7.
9.
9.
57.
9.
6.
6.
5.
7.
8.
228
0
2
0
9
2
9
9
7
7
4
2
6
7
6
6
3
9
1
9
X fua/L}
77
32
70
13
7
7
d
16
14
d
d
12
d
11
11
12
d
11
d
d
d
75
13
16
d
66
11
15
15
11
12
17
d
- 153
- 168
- 132
- 28
- 32
- 35
- 54
- 25
- 30
- 47
- 70
- 26
- 56
- 29
- 31
- 30
- 50
- 32
- 47
- 51
- 40
- 146
- 27
- 29
- 50
- 159
- 30
- 29
- 29
- 33
- 30
- 30
- 59
labeled
compound
recovery
Sec 8.3
and 14.2
p m
35
37
ns
ns
ns
ns
ns
42
ns
ns
ns
18
ns
16
23
12
ns
15
ns
ns
ns
44
ns
ns
ns
36
5
31
4
12
21
35
ns
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
165
163
204
196
99
214
414
165
205
308
554
172
410
185
191
192
315
195
343
381
284
156
239
203
316
164
199
181
193
200
184
196
452
On-going
accuracy
Sec 11.5
R fua/L)
55 -
7 -
58 -
4 -
4 -
6 -
d -
12 -
4 -
d -
d -
8 -
d -
8 -
9 -
8 -
d -
8 -
d -
d -
d -
55 -
11 -
5 -
d -
42 -
7 -
11 -
6 -
8 -
9 -
12 -
d -
145
190
144
33
34
36
61
30
35
51
79
30
64
32
33
33
52
34
51
56
44
145
29
35
50
158
34
32
33
35
32
34
65
acetone*
acrolein*
acrylonitrile*
benzene
bromodichloromethane
bromoform
bromomethane
carbon tetrachloride
chlorobenzene
chloroethane
2-chloroethylvinyl ether
chloroform
chloromethane
dibromochloromethane
1,1-dichloroethane
1,2-dichloroethane
1,1-dichloroethene
trans-1,2-dichiorethene
1,2-dichloropropane
cis-1,3-dichloropropene
trans-1,3-dichloropropene
diethyl ether*
p-dioxane
ethylbenzene
methylene chloride
methyl ethyl Jcetone*
1,1,2,2-tetrachloroethane
tetrachlorethene
toluene
1,1,1-trichloroethane
1,1,2-trichloroethane
trichloroethene
vinyl chloride
* Acceptance criteria at 100 ug/L
d = detected; result must be greater than zero.
ns = no specification; limit would be below detection limit.
1624C E-145
-------
\
SAMMJ ounxr nrriNa
J- i « MM O.H 01>SS TTJBwa
4M.VW.
Figure 1 Purging Device for Waters Figure 2 Purging Device for Soils or
Waters
4~
=!"-
Figure 3 Trap Construction and Pack-
ings
Figure 4 Schematic of Purge and Trap
DevicePurge Mode
1624C E-146
-------
10-
1.0'
^
$
9.1-
2 10 M M 100 MO
CONCENTRATION (u»U
Figure 5 Schematic of Purge and Trap
DeviceDesorb Mode
Figure 6 Relative Response Calibra-
tion Curve for Toluene. The Dotted
Lines Enclose a +/- 10 Percent Error
Window.
(A)
(8)
AMEA>«0960 vft
M/Z 93
1C)
MIZ92 9M6«
M/Z W
r
van
TOUIENE-0.
1 9 *
-3*
1234S«7«»10
ANALYSIS NUMMfl
I 0 1.10
i>
! =
! 2 1.00
i =
£2 a*°
TOLUCNC
-3*
M sn us
OATE ANALYZED
vs
Figure 7 Extracted Ion Current Pro-
files for (A) Toluene, (B) Toluene-d8,
and (C) a Mixture of Toluene and
Toluene-dS.
Figure 8 Quality Control Charts Show-
ing Area (top graph) and Relative
Response of Toluene to Toluene-d8
(lower graph) Plotted as a Function of
Time or Analysis Number
1624C
E-147
-------
Figure 9 Chromatogram of Aqueous Performance Standard
HAS5 OfiOHAI
23i«3«M
OATAs UOAI01343 *1
CAUl UOAI01349 *1
SONS 1 TO 1298
COMS.1
MHGEi C 1.12BS LflflEU M «. 4.4
A I. !. J BASEi U a, 3
46.314
258.375
12M SOW
41:68 Tire
1624C
E-148
-------
Appendix A: Mass Spectra in the Form of Mass/intensity Lists
532 allyl alcohol
m/z int.
42 30
56 55
m/2 int.
43 39
57 1000
m/z int.
45 12
61 15
m/z int.
53 13
533 carbon disulfide
m/2 int. m/2 int. m/2 int. m/2 int. m/2 int.
44 282 46 10 64 14 76 1000 77 27
534 2-chloro-l,3-butadiene (chloroprene)
m/2 int. m/2 int. m/2 int. m/z int.
48 21 49 91 50 223 51 246
54 41 61 30 62 54 63 11
87 12 88 452 89 22 90 137
535 chloroacetonitrile
m/2 int. m/2 int.
,47 135 48 1000
74 43 75 884
536 3-chloropropene
m/2 int. m/2 int.
35 39 36 40
49 176 51 64
76 1000 77 74
537 crotonaldehyde
m/2 int. m/2 int.
35 26 40 28
50 40 51 20
69 511 70 1000
m/2 int.
49 88
76 39
m/2 int.
50 294
77 278
m/z
52
64
m/2
51
int.
241
16
int.
12
m/2 int.
55 59
m/z int.
78 82
m/z int.
53 1000
73 21
m/2 int.
73 22
m/2
40
52
78
int.
44
31
324
m/z
42
61
int.
206
29
m/2
47
73
int.
40
22
m/2
58
75
int.
35
138
m/2
42
52
71
int.
339
21
43
m/2
43
53
int.
43
31
m/z
44
55
int.
335
55
m/2
49
68
int.
27
24
m/z
45
93
174
int.
30
1000
719
m/z
79
94
175
int.
184
64
12
m/z
80
95
176
int.
35
875
342
m/z
81
160
int.
175
18
538 1,2-dibromoethane (EDB)
m/2 int. m/z int. m/z int. m/z int. m/z int.
79 50 80 13 31 51 82 15 93 54
105 32 106 29 107 1000 108 38 109 922
186 13 188 27 190 13
539 dibromomethane
m/2 int. m/z int.
43 99 44 101
91 142 92 61
172 375 173 14
540 trans-1,4-dichloro-2-butane
m/2 int. m/z int. m/2 int. m/z int. m/z int.
49 166 50 171 51 289 52 85 53 878
62 286 64 91 75 1000 77 323 88 246
90 93 91 129 124 138 126 86 128 12
541 1,3-dichloropropane
m/z, int. m/z int. m/z int. m/2 int. m/z int.
40 15 42 44 47 19 48 20 49 193
61 18 62 22 63 131 65 38 75 47
77 46 78 310 79 12
m/z int.
95 42
110 19
m/2 int.
54 273
89 415
m/2 int.
51 55
76 1000
1624C
E-149
-------
542 cis-l,3-dichloropropene
37 262 38 269 39 998
77 328 110 254 112 161
543 ethyl cyanide
m/z int. m/z int. m/z int.
44 115 50 34 51 166
55 193
544 ethyl methacrylate
m/z int. m/z int. m/z int.
42 127 43 48 45 155
69 1000 70 83 71 25
96 17 99 93 113 11
545 2-hexanone (methyl butyl ketone)
m/z int. m/z int. m/z- int.
42 61 43 1000 44 24
59 21 71 36 85 37
49
596
51
189
546 iodomethane
m/z int. m/z int.
44 57 127 328
142 1000 143 12
547 isobutyl alcohol
m/z int. m/z int.
34 21 35 13
43 1000 44 42
m/z int.
128 17
m/z int.
36 13
45 21
59
25
73
12
74
63
548 methacrylonitrile
m/z int. m/z int.
38 24 39 21
51 214 52 446
65 55 66 400
549 methyl methacrylate
m/z int. m/z int.
42 127 43 52
59 124 68 28
98 20 99 89
m/z int.
41 26
53 19
67 1000
m/z int.
45 48
69 1000
100 442
m/z int.
52 190
m/z int.
55 32
85 14
114 119
m/z int.
55 12
100 56
m/z int.
139 39
m/z int.
37 11
55 40
m/z int.
42 100
62 24
68 51
m/z int.
53 30
70 51
101 22
m/z int.
53 127
m/z int.
58 39
86 169
m/z int.
57 130
m/z int.
140 34
m/z int.
39 10
56 37
m/z int.
49 19
63 59
m/z int.
55 100
82 26
550 4-methyl-2-pentanone (methyl isobutyl ketone; MIBK)
m/z int. m/z int. m/z int. m/z int. m/z int.
42 69 43 1000 44 54 53 11 55 15
57 205 58 346 59 20 67 12 69 10
100 94
551 1,1,1,2-tetrachloroethane
m/z int. m/z int. m/z int. m/z int. m/z int.
47 144 49 163 60 303 61 330 62 98
84 31 95 416 96 152 97 270 98 84
121 236 131 1000 133 955 135 301
75 1000
m/z int.
54 1000
m/z int.
68 60
87 21
m/z int.
58 382
m/z int.
42 575
57 21
m/z int.
50 60
64 136
m/z int.
56 49
85 45
m/z int.
56 13
85 96
1624C E-150
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552 trichlorofluoromethane
m/z int. m/z int. m/z int. m/z int. m/z int. m/z int.
44 95 47 153 49 43 51 21 52 14 66 162
68 53 82 40 84 28 101 1000 102 10 103 671
105 102 117 16 119 14
553 1,2,3-trichloropropane
m/z int. ro/z int. m/z int. m/z int. m/z int. m/z int.
49 285 51 87 61 300 62 107 63 98 75 1000
76 38 77 302 83 23 96 29 97 166 98 20
99 103 110 265 111 28 112 164 114 25
554 vinyl acetate
36 5 42 103 43 1000 44 70 45 8 86 57
1624C E-151
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31 October 1986 Draft
Method 1625, Revision C
Semivolatile Organic Compounds by Isotope Dilution GCMS
1 Scope and application
1.1 This method is designed to determine the semivolatile toxic
organic pollutants associated with the 1976 Consent Decree; the
Resource Conservation and Recovery Act; the Comprehensive Environ-
mental Response, Compensation and Liability Act; and other com-
pounds amenable to extraction and analysis by capillary column gas
chromatography-mass spectrometry (GCMS).
1.2 The chemical compounds listed in tables 1 through 4 may be deter-
mined in waters, soils, and municipal sludges by this method. The
method is designed to meet the survey requirements of the Environ-
mental Protection Agency (EPA).
1.3 The detection limit of this method is usually dependent on the
level of interferences rather than instrumental limitations. The
limits in tables 5 and 6 typify the minimum quantity that can be
detected with no interferences present.
1.4 The GCMS portions of this method are for use only by analysts
experienced with GCMS or under the close supervision of such quali-
fied persons. Laboratories unfamiliar with analyses of environmen-
tal samples by GCMS should run the performance tests in reference 1
before beginning.
2 Summary of method
2.1 The percent solids content of a sample is determined.
E-152
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Stable isotopically labeled analogs of the compounds of interest
are added to the sample.
If the solids content is less than one percent, a one liter sample
is extracted at pH 12 - 13, then at pH <2 with methylene chloride
using continuous extraction techniques. If the solids content is
30 percent percent or less, the sample is diluted to one percent
solids with reagent water, homogenized ultrasonically, and
extracted at pH 12-13, then at pH <2 with methylene chloride using
continuous extraction techniques. If the solids content is greater
than 30 percent, the sample is extracted using ultrasonic tech-
niques.
Each extract is dried over sodium sulfate, concentrated to a volume
of five mL, cleaned up using gel permeation chromatography (GPC),
if necessary, and concentrated to one mL. An internal standard is
added to the extract, and a one uL aliquot of the extract is
injected into the gas chromatograph (GC). The compounds are separ-
ated by GC and detected by a mass spectrometer (MS). The labeled
compounds serve to correct the variability of the analytical tech-
nique.
2.2 Identification of a pollutant (qualitative analysis) is performed
in one of three ways: (1) For compounds listed in tables 1 and 2,
and for other compounds for which authentic standards are avail-
able, the GCMS system is calibrated and the mass spectrum and
retention time for each standard are stored in a user created
library. A compound is identified when its retention time and mass
spectrum agree with the library retention time and spectrum. (2)
For compounds listed in tables 3 and 4, and for other compounds for
which standards are not available, a compound is identified when
the retention time and mass spectrum spectrum agree with those spe-
1625C E-153
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cified in this method. (3) For chromatographic peaks which are not
identified by (1) and (2) above, the background corrected spectrum
at the peak maximum is compared with spectra in the EPA/NIH Mass
Spectral File (reference 2). Tentative identification is estab-
lished when the spectrum agrees.
2.3 Quantitative analysis is performed in one of four ways by GCMS
using extracted ion current profile (EICP) areas: (1) For com-
pounds listed in tables 1 and 2, and for other compounds for which
standards and labeled analogs are available, the GCMS system is
calibrated and the compound concentration is determined using an
isotope dilution technique. (2) For compounds listed in tables 1
and 2, and for other compounds for which authentic standards but no
labeled compounds are available, the GCMS system is calibrated and
the compound concentration is determined using an internal standard
technique. (3) For compounds listed in tables 3 and 4, and for
other compounds for which standards are not available, compound
concentrations are determined using known response factors. (4)
For compounds for which neither standards nor known response fac-
tors are available, compound concentration is determined using the
sum of the EICP areas relative to the sum of the EICP areas of the
internal standard.
2.4 Quality is assured through reproducible calibration and testing of
the extraction and GCMS systems.
3 Contamination and interferences
3.1 Solvents, reagents, glassware, and other sample processing hard-
ware may yield artifacts and/or elevated baselines causing misin-
terpretation of chromatograms and spectra. All materials used in
the analysis shall be demonstrated to be free from interferences
1625C E-154
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under the conditions of analysis by running method blanks initially
and with each sample lot (samples started through the extraction
process on a given 8 hr shift, to a maximum of 20). Specific
selection of reagents and purification of solvents by distillation
in all-glass systems may be required. Glassware and, where pos-
sible, reagents are cleaned by solvent rinse and baking at 450 °C
for one hour minimum.
3.2 Interferences coextracted from samples will vary considerably from
source to source, depending on the diversity of the site being
sampled.
4 Safety
4.1 The toxicity or carcinogenicity of each compound or reagent used
in this method has not been precisely determined; however, each
chemical compound should be treated as a potential health hazard.
Exposure to these compounds should be reduced to the lowest pos-
sible level. The laboratory is responsible for maintaining a cur-
rent awareness file of OSHA regulations regarding the safe handling
of the chemicals specified in this method. A reference file of
data handling sheets should also be made available to all personnel
involved in these analyses. Additional information on laboratory
safety can be found in references 3 - 5.
4.2 The following compounds covered by this method have been tenta-
tively classified as know or suspected human or mammalian carcinog-
ens: benzo(a)anthracene, 3,3'-dichlorobenzidine, benzo(a)pyrene,
dibenzo(a,h)anthracene, N-nitrosodimethylamine, and beta-naphthyla-
mine. Primary standards of these compounds shall be prepared in a
hood, and a NIOSH/MESA approved toxic gas respirator should be worn
when high concentrations are handled.
1625C E-155
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5 Apparatus and materials
5.1 Sampling equipment for discrete or composite sampling.
5.1.1 Sample Bottles and Caps
5.1.1.1 Liquid Samples (waters, sludges and similar materials that
contain less than five percent solids)Sample bottle, amber glass,
1.1 liters minimum, with screw cap.
5.1.1.2 Solid samples (soils, sediments, sludges, filter cake, com-
post, and similar materials that contain more than five percent
solids)Sample bottle, wide mouth, amber glass, 500 mL minimum.
5.1.1.3 If amber bottles are not available, samples shall be protected
from light.
5.1.1.4 Bottle capsthreaded to fit sample bottles. Caps shall be
lined with Teflon.
5.1.1.5 Cleaning
5.1.1.5.1 Bottles are detergent water washed, then solvent rinsed or
baked at 450 °C for one hour minimum before use.
5.1.1.5.2 Liners are detergent water washed, then reagent water (sec-
tion 6.5.1) and solvent rinsed, and baked at approx 200 °C for one
hour minimum prior to use.
5.1.2 Compositing equipmentautomatic or manual compositing system
incorporating glass containers cleaned per bottle cleaning proce-
dure above. Sample containers are kept at 0 - 4 °C during samp-
ling. Glass or Teflon tubing only shall be used. If the sampler
uses a peristaltic pump, a minimum length of compressible silicone
rubber tubing may be used in the pump only. Before use, the tubing
shall be thoroughly rinsed with methanol, followed by repeated
rinsings with reagent water (section 6.5.1) to minimize sample con-
tamination. An integrating flow meter is used to collect propor-
1625C E-156
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tional composite samples.
5.2 Equipment for determining percent moisture
5.2.1 Oven, capable of being temperature controlled at 110 +/- 5 °C.
5.2.2 Dessicator
5.3 Sonic disrupter375 watt with pulsing capability and 3/4 in.
disruptor horn (Ultrasonics, Inc, Model 375C, or equivalent).
5.4 Extraction apparatus
5.4.1 Continuous liquid-liquid extractorTeflon or glass connecting
joints and stopcocks without lubrication, 1.5-2 liter capacity
(Hershberg-Wolf Extractor, Ace Glass 6841-10, or equivalent).
5.4.2 Beakers
5.4.2.1 1.5 - 2 liter, calibrated to one liter
5.4.2.2 400 - 500 mL
5.4.2.3 Spatulasstainless steel
5.4.3 Filtration apparatus
5.4.3.1 Glass funnel125 - 250 mL
5.4.3.2 Filter paper for above (Whatman 41, or equivalent)
5.5 Drying column15 to 20 mm i.d. Pyrex chromatographic column
equipped with coarse glass frit or glass wool plug.
5.6 Kuderna-Danish (K-D) apparatus
5.6.1 Concentrator tubelOmL, graduated (Kontes K-570050-1025, or
equivalent) with calibration verified. Ground glass stopper (size
19/22 joint) is used to prevent evaporation of extracts.
5.6.2 Evaporation flask500 mL (Kontes K-570001-0500, or equivalent),
attached to concentrator tube with springs (Kontes K-662750-0012).
5.6.3 Snyder columnthree ball macro (Kontes K-503000-0232, or equi-
valent) .
5.6.4 Snyder columntwo ball micro (Kontes K-469002-0219, or equiva-
lent) .
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5.6.5 Boiling chipsapprox 10/40 mesh, extracted with methylene chlo-
ride and baked at 450 °C for one hr minimum.
5.7 Water bathheated, with concentric ring cover, capable of temper-
ature control (+/- 2 °C), installed in a fume hood.
5.8 Sample vialsamber glass, 2 - 5 mL with Teflon-lined screw cap.
5.9 Balances
5.9.1 Analyticalcapable of weighing 0.1 mg.
5.9.2 Top loadingcapable of weighing 10 mg.
5.10 Automated gel permeation chromatograph (Analytical Biochemical
Labs, Inc, Model GPC Autoprep 1002, or equivalent)
5.10.1 Column600 - 700 mm x 25 mm i.d., packed with 70 g of SX-3
Bio-beads
5.11 Gas chromatographshall have splitless or on-column injection
port for capillary column, temperature program with 30 °C hold, and
shall meet all of the performance specifications in section 12.
5.11.1 Column30 +/~5 m x 0.25 +/- 0-02 mm i.d. 5% phenyl, 94%
methyl, 1% vinyl silicone bonded phase fused silica capillary col-
umn (J & W DB-5, or equivalent).
5.12 Mass spectrometer70 eV electron impact ionization, shall repeti-
tively scan from 35 to 450 amu in 0.95 - 1.00 second, and shall
produce a unit resolution (valleys between m/z 441-442 less than 10
percent of the height of the 441 peak), background corrected mass
spectrum from 50 ng decafluorotriphenylphosphine (DFTPP) introduced
through the GC inlet. The spectrum shall meet the mass-intensity
criteria in table 7 (reference 6). The mass spectrometer shall be
interfaced to the GC such that thef end of the capillary column ter-
minates within one centimeter of the ion source but does not inter-
cept the electron or ion beams. All portions of the column which
connect the GC to the ion source shall remain at or above the col-
1625C E-158
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umn temperature during analysis to preclude condensation of less
volatile compounds.
5.13 Data systemshall collect and record MS data, store ntass-
intensity data in spectral libraries, process GCMS data, generate
reports, and shall compute and record response factors.
5.13.1 Data acquisitionmass spectra shall be collected continuously
throughout the analysis and stored on a mass storage device.
5.13.2 Mass spectral librariesuser created libraries containing mass
spectra obtained from analysis of authentic standards shall be
employed to reverse search GCMS runs for the compounds of interest
(section 7.2).
5.13.3 Data processingthe data system shall be used to search,
locate, identify, and quantify the compounds of interest in each
GCMS analysis. Software routines shall be employed to compute
retention times and peak areas. Displays of spectra, mass chroma-
tograms, and library comparisons are required to verify results.
5.13.4 Response factors and multipoint calibrationsthe data system
shall be used to record and maintain lists of response factors
(response ratios for isotope dilution) and multi-point calibration
curves (section 7). Computations of relative standard deviation
(coefficient of variation) are used for testing calibration
linearity. Statistics on initial (section 8.2) and on-going (sec-
tion 12.7) performance shall be computed and maintained.
6 Reagents and standards
6.1 Reagents for adjusting sample pH
6.1.1 Sodium hydroxidereagent grade, 6N in reagent water.
6.1.2 Sulfuric acidreagent grade, 6N in reagent water.
6.2 Sodium sulfatereagent grade, granular anhydrous, rinsed with
1625C E-159
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methylene chloride (20 mL/g), baked at 450 °C for one hour minimum,
cooled in a dessicator, and stored in a pre-cleaned glass bottle
with screw cap which prevents moisture from entering.
6.3 Methylene chloridedistilled in glass (Burdick and Jackson, or
equivalent).
6.4 GPC calibration solutions
6.4.1 Corn oil200 mg/mL in methylene chloride
6.4.2 Bis(2-ethylhexyl)phthalate) and pentachlorophenol4.0 mg/mL
each in methylene chloride
6.5 Reference matrices
6.5.1 Reagent waterwater in which the compounds of interest and
interfering compounds are not detected by this method.
6.5.2 High solids reference matrixplayground sand or similar mate-
rial in which the compounds of interest and interfering compounds
are not detected by this method.
6.6 Standard solutionspurchased as solutions or mixtures with certi-
fication to their purity, concentration, and authenticity, or pre-
pared from materials of known purity and composition. If compound
purity is 96 percent or greater, the weight may be used without
correction to compute the concentration of the standard. When not
being used, standards are stored in the dark at -20 to -10 °C in
screw-capped vials with Teflon-lined lids. A mark is placed on the
vial at the level of the solution so that solvent evaporation loss
can be detected. The vials are brought to room temperature prior
to use. Any precipitate is redissolved and solvent is added if
solvent loss has occurred.
6.7 Preparation of stock solutionsprepare in methylene chloride,
benzene, p-dioxane, or a mixture of these solvents per the steps
below. Observe the safety precautions in section 4. The large
1625C E-160
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number of labeled and unlabeled acid and base/neutral compounds
used for combined calibration (section 7) and calibration verifica-
tion (12.5) require high concentrations (approx 40 mg/mL) when
individual stock solutions are prepared, so that dilutions of mix-
tures will permit calibration with all compounds in a single set of
solutions. The working range for most compounds is 10-200 ug/mL.
Compounds with a reduced MS response may be prepared at higher con-
centrations.
6.7.1 Dissolve an appropriate amount of assayed reference material in
a suitable solvent. For example, weigh 400 mg naphthalene in a 10
mL ground glass stoppered volumetric flask and fill to the mark
with benzene. After the naphthalene is completely dissolved,
transfer the solution to a 15 mL vial with Teflon-lined cap.
6.7.2 Stock standard solutions should be checked for signs of degrada-
tion prior to the preparation of calibration or performance test
standards. Qaulity control check samples that can be used to
determine the accuracy of calibration standards are available from
the US Environmental Protection Agency, Environmental Monitoring
and Support Laboratory, Cincinnati, Ohio 45268.
6.7.3 Stock standard solutions shall be replaced after six months, or
sooner if comparison with quality control check standards indicates
a change in concentration.
6.8 Labeled compound spiking solutionfrom stock standard solutions
prepared as above, or from mixtures, prepare the spiking solution
at a concentration of 200 ug/mL, or at a concentration appropriate
to the MS response of each compound.
6.9 Secondary standardusing stock solutions (section 6.7), prepare a
secondary standard containing all of the compounds in tables 1 and
2 at a concentration of 400 ug/mL, or higher concentration appro-
1625C E-161
-------
priate to the MS response of the compound.
6.10 Internal standard solutionprepare 2,2'-difluorobiphenyl (DFB)
at a concentration of 10 mg/mL in benzene.
6.11 DFTPP solutionprepare at 50 ug/mL in acetone.
6.12 Solutions for obtaining authentic mass spectra (section
7.2)prepare mixtures of compounds at concentrations which will
assure authentic spectra are obtained for storage in libraries.
6.13 Calibration solutionscombine 0.5 mL of the solution in section
6.8 with 25, 50, 125, 250, and 500 uL of the solution in section
6.9 and bring to 1.00 mL total volume each. This will produce cal-
ibration solutions of nominal 10, 20, 50, 100 and 200 ug/mL of the
pollutants and a constant nominal 100 ug/mL of the labeled com-
pounds. Spike each solution with 10 uL of the internal standard
solution (section 6.10). These solutions permit the relative
response (labeled to unlabeled) to be measured as a function of
concentration (section 7.4).
6.14 Precision and recovery standardused for determination of ini-
tial (section 8.2) and on-going (section 12.7) precision and recov-
ery. This solution shall contain the pollutants and labeled com-
pounds at a nominal concentration of 100 ug/mL.
6.15 Stability of solutionsall standard solutions (sections 6.8 -
6.14) shall be analyzed within 48 hours of preparation and on a
monthly basis thereafter for signs of degradation. Standards will
remain acceptable if the peak area at the quantitation mass rela-
tive to the DFB internal standard remains within +/- 15 percent of
the area obtained in the initial analysis of the standard.
7 Calibration
7.1 Assemble the GCMS and establish the operating conditions in table
1625C E-162
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5. Analyze standards per the procedure in section 11 to demon-
strate that the analytical system meets the minimum levels in
tables 5 and 6, and the mass-intensity criteria in table 7 for 50
ng DFTPP.
7.2 Mass spectral librariesdetection and identification of compounds
of interest are dependent upon spectra stored in user created
libraries.
7.2.1 Obtain a mass spectrum of each pollutant, labeled compound, and
the internal standard by analyzing an authentic standard either
singly or as part of a mixture in which there is no interference
between closely eluted components. That only a single compound is
present is determined by examination of the spectrum. Fragments
not attributable to the compound under study indicate the presence
of an interfering compound.
7.2.2 Adjust the analytical conditions and scan rate (for this test
only) to produce an undistorted spectrum at the GC peak maximum.
An undistorted spectrum will usually be obtained if five complete
spectra are collected across the upper half of the GC peak. Soft-
ware algorithms designed to "enhance" the spectrum may eliminate
distortion, but may also eliminate authentic masses or introduce
other distortion.
7.2.3 The authentic reference spectrum is obtained under DFTPP tuning
conditions (section 7.1 and table 7) to normalize it to spectra
from other instruments.
7.2.4 The spectrum is edited by saving the 5 most intense mass spec-
tral peaks and all other mass spectral peaks greater than 10 per-
cent of the base peak. The spectrum may be further edited to
remove common interfering masses. If 5 mass spectral peaks cannot
be obtained under the scan conditions given in section 5.12, the
1625C E-163
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mass spectrometer may be scanned to an m/z lower than 35 to gain
additional spectral information. The spectrum obtained is stored
for reverse search and for compound confirmation.
7.2.5 For the compounds in tables 3 and 4 and for other compounds for
which the mass spectra, quantitation m/z's, and retention times are
known but the instrument is not to be calibrated, add the retention
time and reference compound (tables 5 and 6); the responsefactor
and the quantitation m/z (tables 8 and 9); and spectrum (Appendix
A) to the reverse search library. Edit the spectrum per section
7.2.4, if necessary.
7.3 Analytical rangedemonstrate that 20 ng anthracene or phenan-
threne produces an area at m/z 178 approx one-tenth that required
to exceed the linear range of the system. The exact value must be
determined by experience for each instrument. It is used to match
the calibration range of the instrument to the analytical range and
detection limits required, and to diagnose instrument sensitivity
problems (section 15.3). The 20 ug/mL calibration standard (sec-
tion 6.13) can be used to demonstrate this performance.
7.3.1 Polar compound detectiondemonstrate that unlabeled pentachlo-
rophenol and benzidine are detectable at the 50 ug/mL level (per
all criteria in section 13). The 50 ug/mL calibration standard
(section 6.13) can be used to demonstrate this performance.
7.4 Calibration with isotope dilutionisotope dilution is used when
1) labeled compounds are available, 2) interferences do not pre-
clude its use, and 3) the quantitation m/z (tables 8 and 9)
extracted ion current profile (EICP) area for the compound is in
the calibration range. Alternate labeled compounds and quantita-
tion m/z's may be used based on availability. If any of the above
conditions preclude isotope dilution, the internal standard method
1625C E-164
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(section 7.5) is used.
7.4.1 A calibration curve encompassing the concentration range is pre-
pared for each compound to be determined. The relative response
(pollutant to labeled) vs concentration in standard solutions is
plotted or computed using a linear regression. The example in Fig-
ure 1 shows a calibration curve for phenol using phenol-d5 as the
isotopic diluent. Also shown are the +/- 10 percent error limits
(dotted lines). Relative Response (RR) is determined according to
the procedures described below. A minimum of five data points are
employed for calibration.
7.4.2 The relative response of a pollutant to its labeled analog is
determined from isotope ratio values computed from acquired data.
Three isotope ratios are used in this process:
Rx =« the isotope ratio measured for the pure pollutant.
Ry = the isotope ratio measured for the labeled compound.
Rm - the isotope ratio of an analytical mixture of pollutant and
labeled compounds.
The m/z's are selected such that Rx > Ry. If Rm is not
between 2Ry and 0.5RX, the method does not apply and the sample
is analyzed by the internal standard method.
7.4.3 Capillary columns usually separate the pollutant-labeled pair,
with the labeled compound eluted first (figure 2). For this case,
Rx * [area n^/z]/!, at the retention time of the pollutant
(RT2).
Ry = I/[area m2/z], at the retention time of the labeled
compound RT^J
Rm = [area at mj/z (at RT2)]/[area at m2/z (at RTX)], as
measured in the mixture of the pollutant and labeled compounds
(figure 2), and RR = Rm.
1625C E-165
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7.4.4 Special precautions are taken when the pollutant-labeled pair is
not separated, or when another labeled compound with interfering
spectral masses overlaps the pollutant (a case which can occur with
isomeric compounds). In this case, it is necessary to determine
the respective contributions of the pollutant and labeled compounds
to the respective EICP areas. If the peaks are separated well
enough to permit the data system or operator to remove the contri-
butions of the compounds to each other, the equations in section
7.4.3 apply. This usually occurs when the height of the valley
between the two GC peaks at the same m/z is less than 10 percent of
the height of the shorter of the two peaks. If significant GC and
spectral overlap occur, RR is computed using the following equa-
tion:
RR = (Ry - Rm) (Rx + D/(Rm - Rx) (Ry + D where Rx is
measured as shown in figure 3A, Ry is measured as shown in figure
3B, and Rm is measured as shown in figure 3C. For the example,
Rx - 46100/4780 - 9.644, Ry » 2650/43600 - 0.0608, Rm =
49200/48300 - 1.019, and RR - 1.114.
7.4.5 To calibrate the analytical system by isotope dilution, analyze
a 1.0 uL aliquot of each of the calibration standards (section
6.13) using the procedure in section 11. Compute the RR at each
concentration.
7.4.6 Linearityif the ratio of relative response to concentration
for any compound is constant (less than 20 percent coefficient of
variation) over the 5 point calibration range, an averaged relative
response/concentration ratio may be used for that compound; other-
wise, the complete calibration curve for that compound shall be
used over the 5 point calibration range.
7.5 Calibration by internal standardused when criteria for isotope
1625C E-166
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dilution (section 7.4) cannot be met. The internal standard to be
used for both acid and base/neutral analyses is 2,2'-difluorobi-
phenyl. The internal standard method is also applied to determina-
tion of compounds having no labeled analog, and to measurement of
labeled compounds for intra-laboratory statistics (sections 8.4 and
12.7.4) .
7.5.1 Response factorscalibration requires the determination of
response factors (RF) which are defined by the following equation:
RF * (As x Cig)/(Aig x Cs) , where
As is the area of the characteristic mass for the compound in the
daily standard
Aj_s is the area of the characteristic mass for the internal
standard
Cj_s is the concentration of the internal standard (ug/mL)
Cs is the concentration of the compound in the daily standard
(ug/mL)
7.5.1.1 The response factor is determined for at least five concentra-
tions appropriate to the response of each compound (section 6.13) ;
nominally, 10, 20, 50, 100, and 200 ug/mL. The amount of internal
standard added to each extract is the same (100 ug/mL) so that C±s
remains constant. The RF is plotted vs concentration for each com-
pound in the standard (Cs) to produce a calibration curve.
7.5.1.2 Linearityif the response factor (RF) for any compound is
constant (less than 35 percent coefficient of variation) over the 5
point calibration range, an averaged response factor may be used
for that compound? otherwise, the complete calibration curve for
that compound shall be used over the 5 point range.
7.6 Combined calibrationby using calibration solutions (section
6.13) containing the pollutants, labeled compounds, and the inter-
1625C E-167
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nal standard, a single set of analyses can be used to produce cali-
bration curves for the isotope dilution and internal standard meth-
ods. These curves are verified each shift (section 12.5) by ana-
lyzing the 100 ug/mL calibration standard (section 6.13). Recali-
bration is required only if calibration verification (section 12.5)
criteria cannot be met.
8 Quality assurance/quality control
8.1 Each laboratory that uses this method is required to operate a
formal quality assurance program (reference 7). The minimum
requirements of this program consist of an initial demonstration of
laboratory capability, analysis of samples spiked with labeled com-
pounds to evaluate and document data quality, and analysis of stan-
dards and blanks as tests of continued performance. Laboratory
performance is compared to established performance criteria to
determine if the results of analyses meet the performance charac-
teristics of the method.
If the method is to be applied routinely to samples containing high
solids with very little moisture (e.g., soils, filter cake, com-
post) , the high solids reference matrix (section 6.5.2) is substi-
tuted for the reagent water (6.5.1) in all performance tests, and
the high solids method (section 10) is used for these tests.
8.1.1 The analyst shall make an initial demonstration of the ability
to generate acceptable accuracy and precision with this method.
This ability is established as described in section 8.2.
8.1.2 The analyst is permitted to modify this method to improve sepa-
rations or lower the costs of measurements, provided all perfor-
mance specifications are met. Each time a modification is made to
the method, the analyst is required to repeat the procedure in sec-
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tion 8.2 to demonstrate method performance.
8.1.3 Analyses of blanks are required to demonstrate freedom from con-
tamination. The procedures and criteria for analysis of a blank
are described in section 8.5.
8.1.4 The laboratory shall spike all samples with labeled compounds to
monitor method performance. This test is described in section 8.3.
When results of these spikes indicate atypical method performance
for samples, the samples are diluted to bring method performance
within acceptable limits (section 15).
8.1.5 The laboratory shall, on an on-going basis, demonstrate through
calibration verification and the analysis of the precision and
recovery standard (section 6.14) that the analysis system is in
control. These procedures are described in sections 12.1, 12.5,
and 12.7.
8.1.6 The laboratory shall maintain records to define the quality of
data that is generated. Development of accuracy statements is
described in section 8.4.
8.2 Initial precision and accuracyto establish the ability to gener-
ate acceptable precision and accuracy, the analyst shall perform
the following operations:
8.2.1 For low solids (aqueous samples), extract, concentrate, and ana-
lyze two sets of four one-liter aliquots (8 aliquots total) of the
precision and recovery standard (section 6.14) according to the
procedure in section 10. For high solids samples, two sets of four
30 gram aliquots of the high solids reference matrix are used.
8.2.2 Using results of the first set of four analyses, compute the
average recovery (X) in ug/mL and the standard deviation of the
recovery (s) in ug/mL for each compound, by isotope dilution for
pollutants with a labeled "analog, and by internal standard for
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labeled compounds and pollutants with no labeled analog.
8.2.3 For each compound, compare s and X with the corresponding limits
for initial precision and accuracy in table 10. If s and X for all
compounds meet the acceptance criteria, system performance is
acceptable and analysis of blanks and samples may begin. If, how-
ever, any individual s exceeds the precision limit or any individ-
ual X falls outside the range for accuracy, system performance is
unacceptable for that compound.
NOTE: The large number of compounds in table 10 present a substan-
tial probability that one or more will fail the acceptance criteria
when all compounds are analyzed. To determine if the analytical
system is out of control, or if the failure can be attributed to
probability, proceed as follows:
8.2.4 Using the results of the second set of four analyses, compute s
and X for only those compounds which failed the test of the first
set of four analyses (section 8.2.3). If these compounds now pass,
system performance is acceptable for all compounds and analysis of
blanks and samples may begin. If, however, any of the same com-
pounds fail again, the analysis system is not performing properly
for these compounds. In this event, correct the problem and repeat
the entire test (section 8.2.1).
8.3 The laboratory shall spike all samples with labeled compounds to
assess method performance on the sample matrix.
8.3.1 Analyze each sample according to the method beginning in section
10.
8.3.2 Compute the percent recovery (P) of the labeled compounds using
the internal standard method (section 7.5).
8.3.3 Compare the labeled compound recovery for each compound with the
corresponding limits in table 10. If the recovery of any compound
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falls outside its warning limit, method performance is unacceptable
for that compound in that sample. Therefore, the sample is com-
plex. Water samples are diluted, and smaller amounts of soils,
sludges, and sediments are reanalyzed per section 15.
8.4 As part of the QA program for the laboratory, method accuracy for
samples shall be assessed and records shall be maintained. After
the analysis of five samples or a given matrix type (water, soil,
sludge, sediment) for which the labeled compounds pass the tests in
section 8.3, compute the average percent recovery (P) and the stan-
dard deviation of the percent recovery (sp) for the labeled com-
pounds only. Express the accuracy assessment as a percent recovery
interval from P -2Sp to P + 2Sp for each matrix. For example, if
P » 90% and sp » 10% for five analyses of compost, the accuracy
interval is expressed as 70 - 110%. Update the accuracy assessment
for each compound in each matrix on a regular basis (e.g. after
each 5-10 new accuracy measurements).
8.5 Blanksreagent water and high solids reference matrix blanks are
analyzed to demonstrate freedom from contamination.
8.5.1 Extract and concentrate a one liter reagent water blank or a
high solids reference matrix blank with each sample lot (samples
started through the extraction process on the same 8 hr shift, to a
maximum of 20 samples). Analyze the blank immediately after analy-
sis of the precision and recovery standard (section 6.14) to demon-
strate freedom from contamination.
8.5.2 If any of the compounds of interest (tables 1 thru 4) or any
potentially interfering compound is found in an aqueous blank at
greater than 10 ug/L, or in a high solids reference matrix blank at
greater than 100 ug/kg (assuming a response factor of 1 relative to
the internal standard for compounds not listed in tables 1 thru 4),
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analysis of samples is halted until the source of contamination is
eliminated and a blank shows no evidence of contamination at this
level.
8.6 The specifications contained in this method can be met if the
apparatus used is calibrated properly, then maintained in a cali-
brated state. The standards used for calibration (section 7), cal-
ibration verification (section 12.5), and for initial (section 8.2)
and on-going (section 12.7) precision and recovery should be iden-
tical, so that the most precise results will be obtained. The GCMS
instrument in particular will provide the most reproducible results
if dedicated to the settings and conditions required for the ana-
lyses of semi-volatiles by this method.
8.7 Depending on specific program requirements, field replicates may
be collected to determine the precision of the sampling technique,
and spiked samples may be required to determine the accuracy of the
analysis when the internal standard method is used.
9 Sample collection, preservation, and handling
9.1 Collect samples in glass containers following conventional samp-
ling practices (reference 8). Aqueous samples which flow freely
are collected in refrigerated bottles using automatic sampling
equipment. Solid samples are collected as grab samples using wide
mouth jars.
9.2 Maintain samples at 0 - 4 °C from the time of collection until
extraction. If residual chlorine is present in aqueous samples,
add 80 mg sodium thiosulfate per liter of water. EPA methods 330.4
and 330.5 may be used to measure residual chlorine (reference 9).
9.3 Begin sample extraction within seven days of collection, and ana-
lyze all extracts within 40 days of extraction.
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10 Sample extraction, concentration, and cleanupsamples containing
one percent solids or less are extracted directly using continuous
liquid/liquid extraction techniques (section 10.2.1 and figure 4).
Samples containing one to 30 percent solids are diluted to the one
percent level with reagent water (section 10.2.2) and extracted
using continuous liquid/liquid extraction techniques. Samples con-
taining greater than 30 percent solids are extracted using ultra-
sonic techniques (section 10.2.5)
10.1 Determination of percent solids
10.1.1 Weigh 5 - 10 g of sample into a tared beaker.
10.1.2 Dry overnight (12 hours minimum) at 110 +/- 5 °C, and cool in a
dessicator.
10.1.3 Determine percent solids as follows:
% solids = weight of dry sample x 100
weight of wet sample
10.2 Preparation of samples for extraction
10.2.1 Samples containing one percent solids or lessextract sample
directly using continuous liquid/liquid extraction techniques.
10.2.1.1 Measure 1.00 +/~ 0.01 liter of sample into a clean 1.5 - 2.0
liter beaker.
10.2.1.2 Dilute aliquotfor samples which are expected to be diffi-
cult to extract, concentrate, or clean-up, measure an additional
100.0 +/- 1.0 mL into a clean 1.5 - 2.0 liter beaker and dilute to
a final volume of 1.00 +/~ °-l liter with reagent water.
10.2.1.3 Spike 0.5 mL of the labeled compound spiking solution (sec-
tion 6.8) into the sample aliquots. Proceed to preparation of the
QC aliquots for low solids samples (section 10.2.3).
10.2.2 Samples containing one to 30 percent solids
10.2.2.1 Mix sample thoroughly.
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10.2.2.2 Using the percent solids found in 10.1.3, determine the
weight of sample required to produce one liter of solution contain-
ing one percent solids as follows:
sample weight » 1000 grams
% solids
10.2.2.3 Place the weight determined in 10.2.2.2 in a clean 1.5 - 2.0
liter beaker. Discard all sticks, rocks, leaves and other foreign
material prior to weighing.
10.2.2.4 Dilute aliquotfor samples which are expected to be diffi-
cult to extract, concentrate, or clean-up, weigh an amount of
sample equal to one-tenth the amount determined in 10.2.2.2 into a
second clean 1.5 - 2.0 liter beaker. When diluted to 1.0 liter,
this dilute aliquot will contain 0.1 percent solids.
10.2.2.5 Bring the sample aliquot(s) above to 100 - 200 mL volume with
reagent water.
10.2.2.6 Spike 0.5 mL of the labeled compound spiking solution (section
6.8) into each sample aliquot.
10.2.2.7 Using a clean metal spatula, break any solid portions of the
sample into small pieces.
10.2.2.8 Place the 3/4 in. horn on the ultrasonic probe approx 1/2 in.
below the surface of each sample aliquot and pulse at 50 percent
for three minutes at full power. If necessary, remove the probe
from the solution and break any large pieces using the metal spat-
ula or a stirring rod and repeat the sonication. Clean the probe
with methylene chloride:acetone (1:1) between samples to preclude
cross-contamination.
10.2.2.9 Bring the sample volume to 1.0 +/- 0.1 liter with reagent
water.
10.2.3 Preparation of QC aliquots for samples containing low solids
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(<30 percent).
10.2.3.1 For each sample or sample lot (to a maximum of 20) to be
extracted at the same time, place three 1.0 +/- 0.01 liter aliquots
of reagent water in clean 1.5 - 2.0 liter beakers.
10.2.3.2 Spike 0.5 mL of the labeled compound spiking solution (sec-
tion 6.8) into one reagent water aliquot. This aliquot will serve
as the blank.
10.2.3.3 Spike 1.0 mL of the precision and recovery standard (section
6.14) into the two remaining reagent water aliquots.
10.2.4 Stir and equilibrate all sample and QC solutions for 1-2
hours. Extract the samples and QC aliquots per section 10.3.
10.2.5 Samples containing 30 percent solids or greater
10.2.5.1 Mix the sample thoroughly
10.2.5.2 Weigh 30 +/- 0.3 grams into a clean 400 - 500 mL beaker.
Discard all sticks, rocks, leaves and other foreign material prior
to weighing.
10.2.5.3 Dilute aliquotfor samples which are expected to be diffi-
cult to extract, concentrate, or clean-up, weigh 3 +/- 0.03
grams into a clean 400 - 500 mL beaker.
10.2.5.4 Spike 0.5 mL of the labeled compound spiking solution (sec-
tion 6.8) into each sample aliquot.
10.2.5.5 QC aliquotsfor each sample or sample lot (to a maximum of
20) to be extracted at the same time, place three 30 +/- 0.3 gram
aliquots of the high solids reference matrix in clean 400 - 500 mL
beakers.
10.2.5.6 Spike 0.5 mL of the labeled compound spiking solution (sec-
tion 6.8) into one high solids reference matrix aliquot. This ali-
quot will serve as the blank.
10.2.5.7 Spike 1.0 mL of the precision and recovery standard (section
1625C E-175
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6.14) into the two remaining high solids reference matrix aliquots.
Extract, concentrate, and clean up the high solids samples per sec-
tions 10.4 through 10.8.
10.3 Continuous extraction of low solids (aqueous) samplesplace
100 - 150 mL methylene chloride in each continuous extractor and
200 - 300 mL in each distilling flask.
10.3.1 Pour the sample(s), blank, and standard aliquots into the
extractors. Rinse the glass containers with 50 - 100 mL methylene
chloride and add to the respective extractors. Include all solids
in the extraction process.
10.3.2 Base/neutral extractionadjust the pH of the waters in the
extractors to 12 - 13 with 6N NaOH while monitoring with a pH
meter. Begin the extraction by heating the flask until the methy-
lene chloride is boiling. When properly adjusted, 1-2 drops of
methylene chloride per second will fall from the condenser tip into
the water. Test and adjust the pH of the waters during the first
1 - 2 hr and during the fifth to tenth hr of extraction. Extract
for 24-48 hours.
10.3.3 Remove the distilling flask, estimate and record the volume of
extract (to the nearest 100 mL), and pour the contents through a
drying column containing 7 to 10 cm anhydrous sodium sulfate.
Rinse the distilling flask with 30 - 50 mL of methylene chloride
and pour through the drying column. Collect the solution in a 500
mL K-D evaporator flask equipped with a 10 mL concentrator tube.
Seal, label as the base/neutral fraction, and concentrate per sec-
tions 10.5 to 10.6.
10.3.4 Acid extractionadjust the pH of the waters in the extractors
to 2 or less using 6N sulfuric acid. Charge clean distilling
flasks with 300 - 400 mL of methylene chloride. Test and adjust
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the pH of the waters during the first 1 - 2 hr and during the fifth
to tenth hr of extraction. Extract for 24 - 48 hours. Repeat sec-
tion 10.3.3, except label as the acid fraction.
10.4 Ultrasonic extraction of high solids samples
10.4.1 Add 60 grams of anhydrous sodium sulfate the sample and QC ali-
quot (s) (section 10.2.5) and mix thoroughly.
10.4.2 Add 100 +/~ 10 mL of acetone:methylene chloride (1:1) to the
sample and mix thoroughly.
10.4.3 Place the 3/4 in. horn on the ultrasonic probe approx 1/2 in.
below the surface of the solvent but above the solids layer and
pulse at 50 percent for three minutes at full power. If necessary,
remove the probe from the solution and break any large pieces using
the metal spatula or a stirring rod and repeat the sonication.
10.4.4 Decant the extracts through Whatman 41 filter paper using
glass funnels and collect in 500 - 1000 mL graduated cylinders.
10.4.5 Repeat the extraction steps (10.4.2 - 10.4.4) twice more for
each sample and QC aliquot. On the final extraction, swirl the
sample or QC aliquot, pour into its respective glass funnel, and
rinse with acetone:methylene chloride. Record the total extract
volume.
10.4.6 Pour each extract through a drying column containing 7 to 10 cm
of anhydrous sodium sulfate. Rinse the graduated cylinder with
30 - 50 mL of methylene chloride and pour through the drying col-
umn. Collect each extract in a 500 mL K-D evaporator flask
equipped with a 10 mL concentrator tube. Seal and label as the
high solids semi-volatile fraction. Concentrate and clean up the
samples and QC aliquots per sections 10.5 through 10.8.
10.5 Macro concentrationconcentrate the extracts in separate 500 mL
K-D flasks equipped with 10 mL concentrator tubes.
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10.5.1 Add 1 to 2 clean boiling chips to the flask and attach a three-
ball macro Snyder column. Prewet the column by adding approx one
mL of methylene chloride through the top. Place the K-D apparatus
in a hot water bath so that the entire lower rounded surface of the
flask is bathed with steam. Adjust the vertical position of the
apparatus and the water temperature as required to complete the
concentration in 15 to 20 minutes. At the proper rate of distilla-
tion, the balls of the column will actively chatter but the cham-
bers will not flood. When the liquid has reached an apparent vol-
ume of 1 mL, remove the K-D apparatus from the bath and allow the
solvent to drain and cool for at least 10 minutes. Remove the
Snyder column and rinse the flask and its lowers joint into the
concentrator tube with 1 - 2 mL of methylene chloride. A 5 mL
syringe is recommended for this operation.
10.5.2 For performance standards (sections 8.2 and 12.7) and for
blanks (section 8.5), combine the acid and base/neutral extracts
for each at this point. Do not combine the acid and base/neutral
extracts for aqueous samples.
10.6 Micro-concentrationAdd a clean boiling chip and attach a two
ball micro Snyder column to the concentrator tube. Prewet the col-
umn by adding approx 0.5 mL methylene chloride through the top.
Place the apparatus in the hot water bath. Adjust the vertical
position and the water temperature as required to complete the con-
centration in 5 - 10 minutes. At the proper rate of distillation,
the balls of the column will actively chatter but the chambers will
not flood. When the liquid reaches an apparent volume of approx
0.5 mL, remove the apparatus from the water bath and allow to drain
and cool for at least 10 minutes. Remove the micro Snyder column
and rinse its lower joint into the concentrator tube with approx
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0.2 mL of methylene chloride. Adjust the final volume to 5.0 mL if
the extract is to be cleaned up by GPC, or to 1.0 mL if it has been
cleaned up or does not require clean-up.
10.7 Transfer the concentrated extract to a clean screw-cap vial. Seal
the vial with a Teflon-lined lid, and mark the level on the vial.
Label with the sample number and fraction, and store in the dark at
-20 to -10 °C until ready for analysis.
10.8 GPC setup and calibration
10.8.1 Column packing
10.8.1.1 Place 75 +/~ 5 g of SX-3 Bio-beads in a 400 - 500 mL beaker.
10.8.1.2 Cover the beads and allow to swell overnight (12 hours mini-
mum) .
10.8.1.3 Transfer the swelled beads to the column and pump solvent
through the column, from bottom to top, at 4.5 - 5.5 mL/min.
10.8.1.4 After purging the column with solvent for 1-2 hours, adjust
the column head pressure to 7 - 10 psig, and purge for 4-5 hours
to remove air from the column. Maintain a head pressure of 7 - 10
psig.
10.8.2 Column calibration
10.8.2.1 Load 5 mL of the corn oil solution into sample loop number
one, and 5 mL of the phthalate/phenol solution into sample loop
number two.
10.8.2.2 Inject the corn oil and collect approx 10 mL fractions at two
minute intervals for 36 minutes.
10.8.2.3 Inject the phthalate/phenol mixture and collect 15 mL frac-
tions for 60 minutes.
10.8.2.4 Determine the corn oil elution pattern gravimetrically (by
evaporation of each fraction and weighing the residue), or by UV,
IR, or other technique which will detect the corn oil.
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10.8.2.5 Determine the phthalate/phenol elution pattern by GC, GCMS,
UV, IR, or other technique which will detect these compounds.
10.8.2.6 Plot a normalized chromatogram of the corn oil and phthal-
ate/phenol mixture.
10.8.2.7 Choose the "dump time" to allow >85 percent removal of the
corn oil and >85 percent recovery of the phthalate.
10.8.2.8 Choose the "collect time" to extend at least 10 minutes past
the elution of the phenol.
10.8.2.9 Verify the calibration with pentachlorophenol after every 20
extracts. Calibration is verified if the recovery of the pentach-
lorophenol is greater than 85 percent. If calibration is not veri-
fied, the system shall be recalibrated using the corn oil and
phthalate/phenol mixture.
10.9 Extract cleanup
10.9.1 Filter the extract or load through the filter holder to remove
particulates. Load the 5.0 mL extract onto the column. The maxi-
mum capacity of the column is 0.5 -l.o gram. If necessary, split
the extract into multiple aliquots to prevent column overload.
10.9.2 Elute the extract using the calibration data determined in
10.8.2. Collect the eluate in a clean 400 - 500 mL beaker.
10.9.3 Concentrate the cleaned up extract per section 10.5.
10.9.4 Rinse the sample loading tube thoroughly with methylene chlo-
ride between extracts to prepare for the next sample.
10.9.5 If a particularly dirty extract is encountered, a 5.0 mL
methylene chloride blank shall be run through the system to check
for carry-over.
10.9.6 Reconcentrate the extract to one mL and transfer to a screw-cap
vial per sections 10.6 and 10.7.
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11 GCMS analysis
11.1 Establish the operating conditions given in tables 5 or 6 for
analysis of the base/neutral or acid extracts, respectively. For
analysis of combined extracts (section 10.5.2 and 10.9.6), use the
operating conditions in table 5.
11.2 Bring the concentrated extract (section 10.7) or standard (sec-
tions 6.13 - 6.14) to room temperature and verify that any precipi-
\
x ,,
tate has redissolved. Verify the level on the extract (sections
6.6 and 10.7) and bring to the mark with solvent if required.
11.3 Add the internal standard solution (section 6.10) to the extract
(use 1.0 uL of solution per 0.1 mL of extract) immediately prior to
injection to minimize the possibility of loss by evaporation,
adsorption, or reaction. Mix thoroughly.
11.4 Inject a volume of the standard solution or extract such that 100
ng of the internal standard will be injected, using on-column or
splitless injection. For 1 mL extracts, this volume will be 1.0
uL. Start the GC column initial isothermal hold upon injection.
Start MS data collection after the solvent peak elutes. Stop data
collection after the benzo(ghi)perylene or pentachlorophenol peak
elutes for the base/neutral (or semi-volatile) or acid"fraction,
respectively. Return the column to the initial temperature for
analysis of the next sample.
12 System and laboratory performance
12.1 At the beginning of each 8 hr shift during which analyses are
performed, GCMS system performance and calibration are verified for
all pollutants and labeled compounds. For these tests, analysis of
the 100 ug/mL calibration standard (section 6.13) shall be used to
verify all performance criteria. Adjustment and/or recalibration
1625C E-181
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(per section 7) shall be performed until all performance criteria
are met. Only after all performance criteria are met may samples,
blanks, and precision and recovery standards be analyzed.
12.2 DFTPP spectrum validityinject 1 uL of the DFTPP solution (sec-
tion 6.11) either separately or within a few seconds of injection
of the standard (section 12.1) analyzed at the beginning of each
shift. The criteria in table 7 shall be met.
12.3 Retention timesthe absolute retention time of 2,2'-difluoro-
biphenyl shall be within the range of 1078 to 1248 seconds and the
relative retention times of all pollutants and labeled compounds
shall fall within the limits given in tables 5 and 6.
12.4 GC resolutionthe valley height between anthracene and phenan-
threne at m/z 178 (or the analogs at m/z 188) shall not exceed 10
percent of the taller of the two peaks.
12.5 Calibration verificationcompute the concentration of each pol-
lutant (tables 1 and 2) by isotope dilution (section 7.4) for those
compounds which have labeled analogs. Compute the concentration of
each pollutant which has no labeled analog by the internal standard
method (section 7.5). Compute the concentration of the labeled
compounds by the internal standard method. These concentrations
are computed based on the calibration data determined in section 7.
12.5.1 For each pollutant and labeled compound being tested, compare
the concentration with the calibration verification limit in table
10. If all compounds meet the acceptance criteria, calibration has
been verified and analysis of blanks, samples, and precision and
recovery standards may proceed. If, however, any compound fails,
the measurement system is not performing properly for that com-
pound. In this event, prepare a fresh calibration standard or cor-
rect the problem causing the failure and repeat the test (section
1625C E-182
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12.1), or recalibrate (section 7).
12.6 Multiple peakseach compound injected shall give a single, dis-
tinct GC peak.
12.7 On-going precision and accuracy.
12.7.1 Analyze the extract of one of the pair of precision and recov-
ery standards (section 10) prior to analysis of samples from the
same lot.
12.7.2 Compute the concentration of each pollutant (tables 1 and 2) by
isotope dilution (section 7.4) for those compounds which have
labeled analogs. Compute the concentration of each pollutant which
has no labeled analog by the internal standard method (section
7.5). Compute the concentration of the labeled compounds by the
internal standard method.
12.7.3 For each pollutant and labeled compound, compare the concentra-
tion with the limits for on-going accuracy in table 10. If all com-
pounds meet the acceptance criteria, system performance is accept-
able and analysis of blanks and samples may proceed. If, however,
any individual concentration falls outside of the range given, sys-
tem performance is unacceptable for that compound.
NOTE: The large number of compounds in table 10 present a
substantial probability that one or more will fail when all com-
pounds are analyzed. To determine if the extraction/concentration
system is out of control or if the failure is caused by probabil-
ity, proceed as follows:
12.7.3.1 Analyze the second aliquot of the pair of precision and
recovery standards (section 10).
12.7.3.2 Compute the concentration of only those pollutants or labeled
compounds that failed the previous test (section 12.7.3). If these
compounds now pass, the extraction/concentration processes are in
1625C E-183
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control and analysis of blanks and samples may proceed. If, how-
ever, any of the same compounds fail again, the extraction/concen-
tration processes are not being performed properly for these com-
pounds. In this event, correct the problem, re-extract the sample
lot (section 10) and repeat the on-going precision and recovery
test (section 12.7).
12.7.4 Add results which pass the specifications in section 12.7.3 to
initial and previous on-going data for each compound in each mat-
rix. Update QC charts to form a graphic representation of conti-
nued laboratory performance (Figure 5). Develop a statement of
laboratory accuracy for each pollutant and labeled compound in each
matrix type by calculating the average percent recovery (R) and the
standard deviation of percent recovery (sr). Express the accuracy
as a recovery interval from R - 2sr to R + 2sr. For example, if R =
95% and sr - 5%, the accuracy is 85 - 105%.
13 Qualitative determination--identification is accomplished by
comparison of data from analysis of a sample or blank with data
stored in the mass spectral libraries. For compounds for which the
relative retention times and mass spectra are known, identification
is confirmed per sections 13.1 and 13.2. For unidentified GC
peaks, the spectrum is compared to spectra in the EPA/NIH mass
spectral file per section 13.3.
13.1 Labeled compounds and pollutants having no labeled analog (tables
1 thru 4):
13.1.1 The signals for all characteristic m/z's stored in the spectral
library (section 7.2.4) shall be present and shall maximize within
the same two consecutive scans.
13.1.2 Either (1) the background corrected EICP areas, or (2) the
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corrected relative intensities of the mass spectral peaks at the GC
peak maximum shall agree within a factor of two (0.5 to 2 times)
for all masses stored in the library.
13.1.3 For the compounds for which the system has been calibrated
(tables 1 and 2), the retention time shall be within the windows
specified in tables 5 and 6, or within +/- 15 scans or +/- 15 sec-
onds (whichever is greater) for compounds for which no window is
specified.
13.1.4 For the compounds for which the system has not been calibrated
but the relative retention times and mass spectra are known (tables
3 and 4), the retention time relative to the 2,2'-difluorobiphenyl
internal standard shall be within +/---3Q scans or +/- 30 seconds
(whichever is greater) based on the nominal retention time speci-
fied in tables 5 and 6.
13.2 Pollutants having a labeled analog (tables 1 and 2):
13.2.1 The signals for all characteristic m/z's stored in the spectral
library (section 7.2.4) shall be present and shall maximize within
the same two consecutive scans.
13.2.2 Either (1) the background corrected EICP areas, or (2) the
corrected relative intensities of the mass spectral peaks at the GC
peak maximum shall agree within a factor of two for all masses
stored in the spectral library.
13.2.3 The relative retention time between the pollutant and its
labeled analog shall be within the windows specified in tables 5
and 6.
13.3 Unidentified GC peaks
13.3.1 The signals for masses specific to a GC peak shall all maximize
within +/- 1 scan.
13.3.2 Either (1) the background corrected EICP areas, or (2) the cor-
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rected relative intensities of the mass spectral peaks at the GC
peak maximum shall agree within a factor of two with the masses
stored in the EPA/NIH Mass Spectral File.
13.4 M/z's present in the experimental mass spectrum that are not pre-
sent in the reference mass spectrum shall be accounted for by con-
taminant or background ions. If the experimental mass spectrum is
contaminated, or if identification is ambiguous, an experienced
spectrometrist (section 1.4) is to determine the presence or
absence of the compound.
14 Quantitative determination
14.1 Isotope dilutionby adding a known amount of a labeled compound
to every sample prior to extraction, correction for recovery of the
pollutant can be made because the pollutant and its labeled analog
exhibit the same effects upon extraction, concentration, and gas
chromatography. Relative response (RR) values for sample mixtures
are used in conjunction with calibration curves described in sec-
tion 7.4 to determine concentrations directly, so long as labeled
compound spiking levels are constant. For the phenol example given
in figure 1 (section 7.4.1), RR would be egual to 1.114. For this
RR value, the phenol calibration curve given in figure 1 indicates
a concentration of 27 ug/mL in the sample extract (Cex).
14.2 Internal standardcompute the concentration in the extract using
the response factor determined from calibration data (section 7.5)
and the following equation:
Cex (ug/mL) - (As x Cis)/(Ais x RF)
where Cex is the concentration of the compound in the extract,
and the other terms are as defined in section 7.5.1.
14.3 The concentration of the pollutant in the solid phase of the
1625C E-186
-------
sample is computed using the concentration of the pollutant in the
extract and the weight of the solids (section 10), as follows:
Concentration in solid (ug/kg) = (Cex x Vex)/Ws
where Cex is the extract volume in mL and Ws is the sample weight
in kg.
14.4 If the EICP area at the quantitation m/z for any compound exceeds
the calibration range of the system, the extract of the dilute ali-
quot (section 10) is analyzed by isotope dilution; otherwise, the
extract is diluted by a factor of 10, 9 uL of internal standard
solution (section 6.10) are added to a 1.0 mL aliquot, and this
diluted extract is analyzed by the internal standard method (sec-
tion 14.2) .
14.5 For GC peaks which are to be identified (per section 13.3), the
sample is diluted by successive factors of 10 when any peak in the
uncorrected mass spectrum at the GC peak maximum is saturated.
14.6 Results are reported for all pollutants, labeled compounds, and
tentatively identified compounds found in all standards, blanks,
and samples, in units of ug/L for aqueous samples or in ug/kg dry
weight of solids for high solids samples (soils, sediments, filter
cake, compost), to three significant figures. Results for samples
which have been diluted are reported at the least dilute level at
which the area at the quantitation m/z is within the calibration
range (section 14.4) or at which no m/z in the spectrum is satu-
rated (section 14.5). For compounds having a labeled analog,
results are reported at the least dilute level at which the area at
the quantitation m/z is within the calibration range (section 14.4)
and the labeled compound recovery is within the normal range for
the method (section 15.4).
1625C E-187
-------
15 Analysis of complex samples
15.1 Some samples may contain high levels (>1000 ug/L) of the com-
pounds of interest, interfering compounds, and/or polymeric materi-
als. Some samples will not concentrate to one mL (section 10.6);
others will overload the GC column and/or mass spectrometer.
15.2 Analyze the dilute aliquot (section 10) when the sample will not
concentrate to 1.0 mL. If a dilute aliquot was not extracted, and
the sample holding time (section 9.3) has not been exceeded, dilute
an aliquot of an aqueous sample with reagent water, or weigh a
dilute aliquot of a high solids sample and re-extract (section 10);
otherwise, dilute the extract (section 14.4) and analyze by the
internal standard method (section 14.2).
15.3 Recovery of internal standardthe EICP area of the internal
standard should be within a factor of two of the area in the shift
standard (section 12.1). If the absolute areas of the labeled com-
pounds are within a factor of two of the respective areas in the
shift standard, and the internal standard area is less than one-
half of its respective area, then internal standard loss in the
extract has occurred. In this case, use one of the labeled com-
pounds (preferably a polynuclear aromatic hydrocarbon) to compute
the concentration of a pollutant with no labeled analog.
15.4 Recovery of labeled compoundsin most samples, labeled compound
recoveries will be similar to those from reagent water or from the
high solids reference matrix (section 12.7). If the labeled com-
pound recovery is outside the limits given in table 10, the extract
from the dilute aliquot (section 10) is analyzed as in section
14.4. If the recoveries of all labeled compounds and the internal
standard are low (per the criteria above), then a loss in instru-
ment sensitivity is the most likely cause. In this case, the 100
1625C E-188
-------
ug/mL calibration standard (section 12.1) shall be analyzed and
calibration verified (section 12.5). If a loss in sensitivity has
occurred, the instrument shall be repaired, the performance speci-
fications in section 12 shall be met, and the extract reanalyzed.
If a loss in instrument sensitivity has not occurred, the method
does not work on the sample being analyzed and the result may not
be reported for regulatory compliance purposes.
16 Method performance
16.1 Interlaboratory performance for this method is detailed in refer-
ence 10. Reference mass spectra, retention times, and response
factors are from references 11 and 12. Results of initial tests of
this method on municipal sludge can be found in reference 13.
16.2 A chromatogram of the 100 ug/mL acid/base/neutral calibration
standard (section 6.13) is shown in figure 6.
1625C E-189
-------
References
1. "Performance Tests for the Evaluation of Computerized Gas Chroma-
tography/Mass Spectrometry Equipment and Laboratories" USEPA, EMSL
Cincinnati, Ohio 45268, EPA-600/4-80-025 (April 1980).
2. National Standard Reference Data System, "Mass Spectral Tape
Format", US National Bureau of Standards (1979 and later attach-
ments) .
3. "Working with Carcinogens," DHEW, PHS, CDC, NIOSH, Publication
77-206, (Aug 1977).
4. "OSHA Safety and Health Standards, General Industry" OSHA 2206, 29
CFR 1910 (Jan 1976).
5. "Safety in Academic Chemistry Laboratories," ACS Committee on Chem-
ical Safety (1979).
6. "Interlaboratory Validation of U. S. Environmental Protection
Agency Method 1625A, Addendum Report", SRI International, Prepared
for Analysis and Evaluation Division (WH-557), USEPA, 401 M St SW,
Washington DC 20460 (January 1985).
7. "Handbook of Analytical Quality Control in Water and Wastewater
Laboratories," USEPA, EMSL, Cincinnati, OH 45268, EPA-600/4-79-019
(March 1979).
8. "Standard Practice for Sampling Water," ASTM Annual Book of Stan-
dards, ASTM, Philadelphia, PA, 76 (1980).
9. "Methods 330.4 and 330.5 for Total Residual Chlorine," USEPA, EMSL,
Cincinnati, OH 45268, EPA 600/4-70-020 (March 1979).
10. "Inter-laboratory Validation of US Environmental Protection Agency
Method 1625," USEPA, Effluent Guidelines Division, Washington, DC
20460 (June 15, 1984).
11. "Narrative for Episode 1036: Paragraph 4(c) Mass Spectra, Reten-
tion Times, and Response Factors", U S Testing Co, Inc, Prepared
for W. A. Telliard, Industrial Technology Division (WH-552), USEPA,
401 M St SW, Washington DC 20460 (October 1985).
12. "Narrative for SAS 109: Analysis of Extractable Organic Pollutant
Standards by Isotope Dilution GC/MS", S-CUBED Division of Maxwell
Laboratories, Inc., Prepared for W. A. Telliard, Industrial Tech-
nology Division (WH-552), USEPA, 401 M St SW, Washington DC 20460
(July 1986).
13. Colby, Bruce N. and Ryan, Philip W., "Initial Evaluation of
Methods 1634 and 1635 for the analysis of Municipal Wastewater
Treatment Sludges by Isotope Dilution GCMS", Pacific Analytical
Inc., Prepared for W. A. Telliard, Industrial Technology Division
(WH-552), USEPA, 401 M St SW, Washington DC 20460 (July 1986).
1625C E-190
-------
Table 1
Base/Neutral Extractable Compounds Determined by Calibrated GCMS Using
Isotope Dilution and Internal Standard Techniques
Pollutant
Labeled Compound
Compound
acenaphthene
acenaphthylene
anthracene
benzidine
benzo( a ) anthracene
benzo(b)fluoranthene
b«nzo( k ) f I uoranthene
benzo(a)pyren«
benzo(ghi )perylene
bfphenyt (Appendix C}
bts(2-chloroethyl) ether
bis(2-chloroethoxy)methane
bis(2-chloroisopropyt) ether
bis(2-ethylhexyl) phthalate
4-bromophenyl phenyl ether
butyl benzyl phthalate
n-C10 (Appendix C)
n-C12 (Appendix C)
n-C14 (Appendix C)
n-C16 (Appendix C)
n-C18 (Appendix C)
n-C20 (Appendix C)
n-C22 (Appendix C)
n-C24 (Appendix C)
n-C26 (Appendix C)
n-C28 (Appendix C)
n-C30 (Appendix C)
earbazole (4c)
2-chloronaphthalene
4-chlorophenyl phenyl ether
ehrysene
p-cymene (Appendix C)
dibenzo(a,h)anthracene
dibenzofuran (Appendix C & 4c>
dibenzothiophene (Synfuel)
di-n- butyl phthalate
1 ,2-dichlorobenzene
1 ,3-dichlorobenzene
1 , 4 - d i ch I orobenzene
3,3l-dichlorobenzidine
diethyl phthalate
2,4-dimethylphenol
dimethyl phthalate
2,4-dinitrotoluene
2,6-dinitrotoluene
di-n-octyl phthalate
diphenylamine (Appendix C)
diphenyl ether (Appendix C)
1.2-diphenylhydrazine
fluoranthene
fluorene
Storet
34205
34200
34220
39120
34526
34230
34242
34247
34521
31513
34273
34278
34283
39100
34636
34292
77427
77588
77691
77757
77804
77830
77859
77886
77901
78116
78117
77571
34581
34641
34320
77356
34556
81302
77639
39110
34536
34566
34571
34631
34336
34606
34341
34611
34626
34596
77579
77587
34346
34376
34381
CAS Registry EPA-EGD NPDES Analog
83-32-9
208-96-8
120-12-7
92-87-5
56-55-3
205-99-2
207-08-9
50-32-3
191-24-2
92-52-4
111-44-4
111-91-1
108-60-1
117-81-7
101-55-3
35-63-7
124-18-5
112-40-3
629-59-4
544-76-3
593-45-3
112-95-8
629-97-0
646-31-1
630-01-3
630-02-4
638-68-6
86-74-8
91-58-7
7005-72-3
218-01-9
99-87-6
53-70-3
132-64-9
132-65-0
84-74-2
95-50-1
541-73-1
106-46-7
91-94-1
84-66-2
105-67-9
131-11-3
121-14-2
606-20-2
117-84-0
122-39-4
101-84-8
122-66-7
206-44-0
86-73-7
001
077
078
005
072
074
075
073
079
512
018
043
042
066
041
067
517
506
513
519
520
521
522
523
524
525
526
528
020
040
076
513
082
505
504
068
025
026
027
023
070
034
071
035
036
069
507
508
037
039
080
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
8
B
B
B
B
B
B
B
B
B
B
B
B
B
3
B
B
B
B
B
8
B
B
A
B
B
B
B
B
3
B
B
B
001
002
003
004
005
007
009
006
008
011
010
012
013
014
015
016
017
018
019
026
020
021
022
023
024
003
025
027
028
029
030
031
032
B
B
B
B
B
3
8
B
B
B
B
B
8
3
8
3
B
B
B
a
8
3
3
8
B
A
B
3
B
B
3
B
8
d10
d8
d10
d8
d12
d12
d12
d12
d12
d10
d8
dS
d12
d4
d5
d4
d22
d26
d34
d42
dSO
d62
oB
d7
d5
d12
d14
d14
d8
d8
d4
d4
d4
d4
d6
d4
d3
d4
cS
d3
d4
d10
d10
d10
d10
d10
CAS Registry
15067-20-2
93951-97-4
1719-06-8
92890-63-6
1718-53-2
93951-98-5
93952-01-3
63466-71-7
93951-66-7
1486-01-7
93952-02-4
93966-78-0
93951-67-8
93951-87-2
93951-83-8
93951-88-3
16416-29-3
16416-30-1
15716-08-2
62369-67-9
16416-32-3
93952-07-9
38537-24-5
93951-84-9
93951-85-0
1719-03-5
93952-03-5
13250-98-1
93952-04-6
33262-29-2
93952-11-5
2199-69-1
2199-70-4
3855-82-1
93951-91-8
93952-12-6
93951-75-8
93951-89-4
93951-68-9
93951-90-7
93952-13-7
37055-51-9
93952-05-7
93951-92-9
93951-69-0
81103-79-9
EPA -EGO
201
277
278
205
272
274
275
273
279
612
218
243
242
266
241
267
617
606
618
619
620
621
622
623
624
625
626
628
220
240
276
613
282
605
604
268
225
226
227
228
270
234
271
235
236
269
607
608
237
231
080
B
3
B
B
8
B
B
B
3
B
8
B
3
B
B
B
B
B
3
B
B
B
B
3
3
3
B
B
B
B
B
B
8
3
B
B
B
B
B
3
3
A
3
3
B
B
B
B
B
8
3
1625C
E-191
-------
hexachIorobenzene
hexachIorobutadi ene
hexachIoroethane
hexachlorocyclopentadiene
ideno<1>2,3-cd)pyrene
isophorone
naphthalene
beta-naphthylamine (Appendix C)
ni trobenzene
N-nitrosodimethylanint
N-nitrosodi-n-proplyamin*
M-nitrosodiphenylamine
phenanthrene
phenol
alpha-picoline (Synfuel)
pyrene
styrene (Appendix C)
alpha-terpineol (Appendix C)
1,2,3-tricMorobenzene (4c)
1,2,4-trichlorobenzen*
39700
34391
34396
34386
34403
34408
34696
82553
34447
34438
34428
34433
34461
34694
77088
34469
77128
77493
77613
34551
118-74-1
87-68-3
67-72-1
77-47-4
193-39-5
78-59-1
91-20-3
91-59-8
98-95-3
62-75-9
621-64-7
86-30-6
85-01-8
108-95-2
109-06-8
129-00-0
100-42-5
98-55-5
87-61-6
120-82-1
009
052
012
053
083
054
055
502
056
061
063
062
081
065
503
084
510
509
529
008
B
S
3
B
8
B
B
B
B
B
B
B
a
A
B
B
3
3
B
B
033
034
036
035
037
038
039
040
041
042
043
044
010
045
046
3
B
B
3
8
B
3
3
B
B
B
B
A
a
B
13C6
13C4
13C
13C4
d8
dfl
d7
dS
d6
d14
d6
d10
d5
d7
d10
dS
d3
d3
d3
93952-14-8
93951-70-3
93952-15-9
93951-71-4
93952-16-0
1146-65-2
93951-94-1
4165-60-0
17829-05-9
93951-96-3
93951-95-2
1517-22-2
4165-62-2
93951-93-0
1718-52-1
5161-29-5
93952-06-8
3907-98-0
93952-16-0
209
252
212
253
254
255
602
256
261
263
262
281
265
503
284
610
609
629
208
3
3
3
8
B
3
B
B
3
B
B
B
A
3
B
8
B
3
B
1625C E-192
-------
Table 2
Acid Extractable Compounds Determined by Calibrated GCMS Using Isotope
Dilution and Internal Standard Techniques
Pollutant
Labeled Compound
Comoound
4-chloro-3-methylphenol
2-chlorophenol
2,4-dichlorophenol
2,4-dinitrophenol
2-methyl-4,6-dinitrophenol
2-nitrophenol
4-nitrophenol
pcntachlorophenol
2,3,6-trichlorophenot (4c)
2,4,5-trichlorophenol (4c)
2,4,6-trichlorophenol
Storet
34452
34586
34601
34616
34657
34591
34646
39032
77688
34621
CAS Registry
59-50-7
95-57-8
120-83-2
51-28-5
534-52-1
88-75-5
100-02-7
87-86-5
933-75-5
95-95-4
88-06-2
EPA-EGD
022 A
024 A
031 A
059 A
060 A
057 A
058 A
064 A
530 A
531 A
021 A
NPOES
008 A
001 A
002 A
005 A
004 A
006 A
007 A
009 A
011 A
Analog
d2
d4
d3
d3
d2
d4
d4
13C6
d2
d2
d2
CAS Registry
93951-72-5
93951-73-6
93951-74-7
93951-77-0
93951-76-9
93951-75-1
93951-79-2
85380-74-1
93951-81-6
93951-82-7
93951-80-5
EPA -EGO
222 A
224 A
231 A
259 A
260 A
257 A
258 A
264 A
630 A
631 A
221 A
1625C
E-193
-------
Table 3
Base/neutral Extractable Compounds to be Determined by Reverse Search and
Quantisation using Known Retention Times, Response Factors, Reference Com-
pound, and Mass Spectra
EGD
No.
555
556
557
558
559
560
561
562
563
564
565
566
567
568
569
570
571
572
573
574
575
576
577
578
579
580
581
582
583
584
585
586
587
588
589
590
591
592
593
594
595
596
597
598
599
900
901
902
903
904
Comnound
acetophenone
4-aminobiphenyl
aniline
o-anisidine
aramite
benzanthrone
1,3-benzenediol (resorcinol)
benzenethiol
2 , 3-benzof luorene
benzyl alcohol
2-bromochlorobenzene
3-bromochlorobenzene
4 -chloro-2-nitroanil ine
5-chloro-o-toluidine
4-chloroaniline
3 -chloronitrobenzene
o-cresol
crotoxyphos
2 , 6-di-tert-butyl-p-benzoquinone
2 , 4-diaminotoluene
1 , 2-dibromo-3-chloropropane
2 , 6-dichloro-4-nitroaniline
1 , 3-dichloro-2-propanol
2 , 3-dichloroaniline
2 , 3-dichloronitrobenzene
1,2:3, 4-diepoxybutane
3,3' -dimethoxybenzidine
dimethyl sulfone
p-dimethy 1 aminoa z obenz ene
7 , 12-dimethylbenz (a) anthracene
N, N-dimethylf ormamide
3 , 6-dimethylphenanthrene
1, 3-dinitrobenzene
diphenyldisulfide
ethyl methanesulfonate
ethylenethiourea
ethynylestradiol 3 -methyl ether
hexachloropropene
2-isopropylnaphthalene
isosafrole
longifolene
malachite green
methapyrilene
methyl methanesulfonate
2-methylbenzothioazole
3 -methy 1 chol anthr ene
4, 4 '-methylenebis(2-chloroaniline)
4 , 5-methylenephenanthrene
1-methy If luorene
2-methylnaphthalene
CAS
Reaistrv
98-86-2
92-67-1
62-53-3
90-04-0
140-57-9
82-05-3
108-46-3
108-98-5
243-17-4
100-51-6
694-80-4
108-37-2
89-63-4
95-79-4
106-47-8
121-73-3
95-48-7
7700-17-6
719-22-2
95-80-7
96-12-8
99-30-9
96-23-1
608-27-5
3209-22-1
1464-53-5
119-90-4
67-71-0
60-11-7
57-97-6
68-12-2
1576-67-6
100-25-4
882-33-7
62-50-0
96-45-7
72-33-3
1888-71-7
2027-17-0
120-58-1
475-20-7
569-64-2
91-80-5
66-27-3
120-75-2
56-49-5
101-14-4
203-64-5
1730-37-6
91-57-6
1625C
E-194
-------
905 l-methylphenanthrene 832-69-9
906 2-(methylthio)benzothiazole 120-75-2
907 1,5-naphthalenediamine 2243-62-1
908 1,4-naphthoquinone 130-15-4
909 alpha-naphthylamine 134-32-7
910 5-nitro-o-toluidine 99-55-8
911 2-nitroaniline 88-77-4
912 3-nitroaniline 99-09-2
913 4-nitroaniline 100-01-6
914 4-nitrobiphenyl 92-93-3
915 N-nitrosodi-n-butylamine 924-16-3
916 N-nitrosodiethylamine 55-18-5
917 N-nitrosomethylethylamine 10595-95-6
918 N-nitrosomethylphenylamine 614-00-6
919 N-nitrosomorpholine 59-89-2
920 N-nitrosopiperidine 100-75-4
921 pentachlorobenzene 608-93-5
922 pentachloroethane 76-01-7
923 pentamethylbenzene 700-12-9
924 perylene 198-55-0
925 phenacetin 62-44-2
926 phenothiazine 92-84-2
927 1-phenylnaphthalene 605-02-7
928 2-phenylnaphthalene 612-94-2
929 pronamide 23950-58-5
930 pyridine 110-86-1
931 safrole 94-59-7
932 squalene 7683-64-9
933 1,2,4,5-tetrachlorobenzene 95-94-3
934 thianaphthene (2,3-benzothiophene) 95-15-8
935 thioacetamide 62-55-5
936 thioxanthone 49 2-22-8
937 o-toluidine 95-53-4
938 1,2,3-trimethoxybenzene 634-36-6
939 2,4,5-trimethylaniline 137-17-7
940 triphenylene 217-59-4
941 tripropyleneglycol methyl ether 20324-33-8
942 1,3,5-trithiane 291-21-4
1625C E-195
-------
Table 4
Acid Extractable Compounds to be Determined by Reverse Search and Quanti-
tation using Known Retention Times, Response Factors, Reference Compound,
and Mass Spectra
EGD CAS
No. Compound Registry
943 benzoic acid 65-85-0
944 p-cresol 106-44-5
945 3,5-dibromo-4-hydroxybenzonitrile 1689-84-5
946 2,6-dichlorophenol 87-65-0
947 hexanoic acid 142-62-1
948 2,3,4,6-tetrachlorophenol 58-90-2
. 1625C E-196
-------
Table 5
Gas Chromatography of Base/neutral Extractable Compounds
Mini- Method Detection
mum Limit (4)
EGO
No.
ill
164
930
261
361
585
530
603
703
917
598
610
710
916
577
589
582
562
922.
557
613
713
265
365
218
318
617
717
226
326
227
327
225
325
935
564
242
342
571
263
363
555
212
312
937
919
575
256
356
566
Retention time
Mean
Comoound (see)
2,2'-difluorobiphenyl (int std)
pyridine
N-nitrosodimethylamine-d6 (5)
N-nitrosodiiMthylaroine (5)
M,N-dimethylformamide
1,2:3,4-diepoxybutane
alpha picoline-d7
alpha picoline
N-nitrosomethylethylamine
methyl methanesulfonate
styrene-d5
styrene
N -nitrosodi ethyl ami n«
1,3-dichloro-2-propano'l
ethyl methanesulfonate
dimethyl sulfone
benzenethiol
pentach I oroethane
aniline
p-cymene-d14
p-cymene
phenol -d5
phenol
bis(2-chloroethyl) ether-d8
bis(2-chloroethyl) ether
n-decane-d22
n-decane
1,3-dichlorobenzene-d4
1 ,3-dichlorobenzene
1 ,4-dichlorobenzene-d4
1 ,4-dichlorobenzene
1,2-dichlorobenzene-d4
1 , 2-dich locobenzenc
thioacet amide
benzyl alcohol
bis(2-chloroisopropyl) ether-d12
bis(2-chloroisopropyl) ether
o-cresol
M-nitPosodi-n-propylamine-d14 (5)
N-nitrosodi-n-propylamine (5)
acetophenone
hexach 1 oroethane- 13C
hexachloroethane
o-toluidine
N-ni trosomorphol ine
1 ,2-dibromo-3-chloropropane
nitrobenzene- d5
nitrobenzene
3 - bromoch I orobenzene
1163
378
378
385
407
409
417
426
451
511
546
549
570
589
637
649
667
680
694
742
755
696
TOO
696
704
698
720
722
724
737
740
758
760
768
785
788
799
814
817
830
818
819
823
830
834
839
845
849
854
EGD
Stf
164
164
164
261
164
164
164
603
164
164
164
610
164
164
164
164
164
164
164
164
613
164
265
164
218
164
617
164
226
164
227
164
225
164
164
164
242
164
164
263
164
164
212
164
164
164
164
256
164
Relative (2)
1
0
1
0
1
0
1
0
1
0
0
0
1
0
1
0
0
0
0
0
0
0
1
0
1
0
0
0
1
.000
0.
.286
.006
0.
0.
.326
.006
0.
0.
.450
.002
0.
0.
0.
0.
0.
0.
0.
.624
.008
.584
.995
.584
.007
.585
.022
.605
.998
.601
.997
.632
.995
0.
0.
.664
.010
0.
.689
.008
0.
.690
.999
0.
0.
0.
.706
.002
0.
1.
325
0.
1.
350
352
0.
1.
338
439
- 0.
1.
490
506
548
558
574
585
597
0.
1.
0.
- 1.
0.
1.
0.
1.
0.
- 1.
0.
- 1.
0.
1.
660
675
0.
- 1.
700
0.
1.
703
0.
1.
714
717
721
0.
1.
734
000
364
028
393
028
488
009
652
023
613
010
607
016
615
038
636
008
666
009
667
008
691
016
716
023
717
001
727
007
Lev-
el (3)
low high
solids solids
(ug/mL) (ug/kg) (ug/ltg)
10
50
50
50
50
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
20
20
10
10
10
10
16 27
25 87
149* 17
426* 912*
2501* 757*
32 22
299* 1188*
46 26
35 20
63 16
24 39
46 47
58 55
39 28
1625C E-197
-------
565 2-bromoehlorob«nzene 880 164 0.757
941 tripropylene glycol methyl ether 381 164 0.758
254 isophoron«-dB 881 164 0.747 - 0.767 10
354 isophorone 889 254 0.999 1.017 10 8 5
942 1,3,5-trithiane 889 164 0.764
920 N-nitrosopiperidine 895 164 0.770
234 2,4-dimethylphenol-d3 921 164 0.781 0.803 10
334 2.4-dimethylphenol 924 234 0.999 1.003 10 26 13
243 bis<2-chloroethoxy) irwthane-d6 (5) 933 164 0.792 0.807 10
343 bis(2-chlopoethoxy) methane (5) 939 243 1.000 1.013 10 26 23
208 1.2,4-trichlorobenzene-d3 955 164 0.813 0.830 10
308 1,2,4-trichlorobenzene 958 208 1.000 - 1.005 10 49 24
558 o-anisidine 962 164 0.827
255 naphthalene-dS 963 164 0.819 0.836 10
355 naphthalene 967 255 1.001 1.006 10 62 42
934 thianapthene 971 164 0.835
609 alpha-terpineol-d3 973 164 0.829 0.844 '10
709 alpha-terpineol 975 609 0.998 1.008 10 nd nd
606 n-dodecane-d26 953 164 0.730 0.908 10
706 n-dodecane 981 606 0.986 1.051 10 860* 3885*
629 1,2,3-trichlorobenzene-d3 (5) 1000 164 0.852 0.868 10
729 1,2,3-trichlorobenzene (5) 1003 629 1.000 1.005 10 260* 164*
252 hexachlorobutadiene-13C4 1005 164 0.856 0.871 10
352 hexachlorobutadiene 1006 252 0.999 1.002 10 46 22
918 N-nitrosomethylphenylanine 1006 164 0.865
592 hexachIoropropene 1013 164 0.871
569 4-ehloroaniline 1016 164 0.874
570 3-chloronitrobenzene 1018 164 0.875
915 N-nitrosodi-n-butylamine 1063 164 0.914
923 pentanwthylbenzene 1083 164 0.931
561 1,3-benzenediol 1088 164 0.936
931 safrole 1090 164 0.937
939 2,4,5-trimthylaniline 1091 164 0.938
904 2-fMthytnaphthalene 1098 164 0.944
599 2-nethylbenzothtazole 1099 164 0.945
568 5-chloPO-o-toluidine 1101 164 0.947
938 1,2.3-trimethoxybenzene 1128 164 0.970
933 1,2,4,5-tetrachlorobenzene 1141 164 0.981
253 hexachlorocyctopentadierw13C4 1147 164 0.976 0.986 10
353 hexachIorocycIopentadiene 1142 253 0.999 1.001 10 nd nd
594 isosafrole Ccis or trans) 1147 164 0.986
594 isosafrole (cis or trans) 1190 164 1.023
578 2,3-dichloroaniline 1160 164 0.997
574 2,4-diaminotoluene 1187 164 1.021
220 2-chloronaphthalene-d7 1185 164 1.014 - 1.024 10
320 2-chloronaphthalene 1200 220 0.997 1.007 10 80 59
518 n-tetradecane 1203 164 1.034 10 256 3533
612 biphenyl-d10 1195 164 1.016 - 1.027 10
712 biphenyl 1205 612 1.001 1.006 10 67 55
608 diphenyl ether-did 1211 164 1.036 1.047 10
708 diphenyl ether 1216 608 0.997 1.009 10 44 12
579 2.3-dichloronitrobenzene 1214 164 1.044
911 2-mtroaniline 1218 164 1.047
908 1,4-naphthoquinone 1224 164 1.052
595 longifolene 1225 164 1.053
277 acenaphthylene-d8 1265 164 1.080 1.095 10
377 acenaphthylene 1247 277 1.000 1.004 10 57 18
593 2-isopropylnaphthalene 1254 164 1.078
1625C E-198
-------
587 1,3-dinitrobenzene 1255 164 1.079
576 2,6-dichloro-4-nitroamline 1259 164 1.083
271 dimethyl phthatate-d4 1269 164 1.083 1.102 10
371 dimethyl phthalate 1273 271 0.998 - 1.005 10 62 21
573 2,6-di-t-butyl-p-benzoquinone 1273 164 1.095
236 2.6-dinitrotoluene-d3 1283 164 1.090 - 1.112 10
336 2.6-dinitPotoluene 1300 236 1.001 1.005 10 55 47
912 3-nitroaniline 1297 164 1.115
201 acenaphthene-d10 1298 164 1.107 1.125 10
301 acenaphthene 1304 201 0.999 1.009 10 64 55
605 dibenzofuran-dS 1331 164 1.134 1.155 10
705 dibenzofuran 1335 605 0.998 1.007 10 77 210*
921 pentachlorobenzene 1340 164 1.152
909 alpha-naphthytamine 1358 164 1.168
235 2,4-dinitrotoluene-d3 1359 164 1.152 1.181 10
335 2,4-dinitrotoluen« 1364 235 1.000 - 1.002 10 65 209*
602 beta-naphthylamine-d7 1368 164 1.163 1.189 50
702 beta-naphthylaoiine 1371 602 0.996 - 1.007 50 49 37
590 cthylenethiourea 1381 164 1.187
280 fluorene-d10 1395 164 1.185 1.214 10
380 fluorene 1401 281 0.999 1.008 10 69 61
240 4-chlorophenyl ph«nyl ether-d5 1406 164 1.194 1.223 10
340 4-chlorophenyl phenyt ether 1409 240 0.990 1.015 10 73 59
270 diethyl phthalate-d4 1409 164 1.197 1.229 10
370 diethyl phthalate 1414 270 0.996 1.006 10 52 16
906 2- 1439 237 0.999-1.009 20 48 27
607 diphenylamine-d10 1437 164 1.213 1.249 20
707 diphenylamine 1439 607 1.000 1.007 20 58 54
262 N-nitrosodiphenylamine-d6 1447 164 1.225 1.252 20
362 N-nitrosodiphenylamine (7) 1464 262 1.000 1.002 20 55 36
241 4-bromophenyl phenyl ether-dS (5) 1495 164 1.271 1.307 10
341 4-bromophenyl phenyl ether (5) 1498 241 0.990 1.015 10 55 17
925 phenacetin 1512 164 1.300
903 1-methylfluorene 1514 164 1.302
209 hexachIorobenzene-13C6 1521 164 1.288 - 1.327 10
309 hexachIorobenzene 1522 209 0.999 - 1.001 10 51 48
556 4-aminobiphenyl 1551 164 1.334
929 pronamide 1578 164 1.357
281 phenanthrene-dIO 1578 164 1.334 - 1.380 10
520 n-octadecane 1580 164 1.359 10 134* 344*
381 phenanthrene 1583 281 1.000-1.005 10 42 22
273 anthracene-d10 1588 164 1.342 - 1.388 10
378 anthracene 1592 278 0.998 1.006 10 52 21
604 dibenzothiophene-d8 1559 164 1.314 1.361 10
704 dibenzothiophene 1564 604 1.000 - 1.006 10 72 71
588 diphenyldisulfide 1623 164 1.396
914 4-nitrobiphenyl 1639 164 1.409
927 1-phenylnaphthalene 1643 164 1.413
628 carbazole-d8 (5) 1645 164 1.388 1.439 20
728 carbazole (5) 1650 628 1.000 - 1.006 20 47 24
621 n-eicosane-d42 1655 164 1.184 1.662 10
1625C E-199
-------
721 n-«icosane
907 1,5-naphthalenediamine
902 4,5-methylenephenanthrene
905 1-methylphenanthrene
268 di-n-butyl phthalate-d4
363 di-n-butyl phthalate
928 2-phenylnaphthalene
586 3,6-dimethylphenanthrene
597 nwthapyrilene
926 phenothiazine
239 fluoranthene-d10
339 fluoranthene
572 crotoxyphos
936 thioxanthone
284 pyrene-d10
384 pyrcne
205 benzidine-d8
305 benzidine
522 n-docosana
559 araraite
559 arantte
583 p-dimethylaminoazobenzene
563 2.3-benzofluorene
623 n*tetracosane-dSO
723 n-tetracosane
932 squalene
267 butylbenzyl phthalate-d4 (5)
367 butylbenzyl phthalate (5)
276 chryaene-d12
376 chrysene
901 4,4lmethylenebis<2-chloroaniline)
272 benzo
-------
282 dibenzo(a,h)anthracene-d14 <5) 2649 164 2.107 2.445 20
382 dib«nzo(a,h)anthracene (5) 2660 282 1.000 - 1.007 20 49 125
279 benzo(ghi)p*pylene-d12 2741 164 2.187 - 2.524 20
379 b*nzo
-------
Table 6
Gas Chromatography of Acid Extractable
Compounds
Mini- Method Detection
nun Limit (4)
EGO
No.
ill
164
224
324
947
944
257
357
231
331
943
946
222
322
221
321
631
731
530
259
359
258
358
948
260
360
945
264
364
Retention time
Mean
Comoound (sec)
2,2'-difluorobiphenyl
-------
Gas velocity: 30 +/- 5 cm/sec at 30 °C
1625C E-203
-------
Table 7
DFTPP Mass-intensity Specifications*
Mass Intensity required
51 8-82 percent of m/z 198
68 less than 2 percent of m/z 69
69 11 - 91 percent of m/z 198
70 less than 2 percent of m/z 69
127 32 - 59 percent of m/z 198
197 less than 1 percent of m/z 198
198 base peak, 100 percent abundance
199 4-9 percent of m/z 198
275 11 - 30 percent of m/z 198
441 44 - 110 percent of m/z 442
442 30 - 86 percent of m/z 198
443 14 - 24 percent of m/z 442
^Reference 6
1625C E-204
-------
Table 8
Base/neutral Extractable Compound Characteristic m/z's and Response
Factors
Labeled Primary Response
Compound analog m/z Factor (
acenaphthene dlO 154/164
acenaphthylene d8 152/160
acetophenone 105 0.79
4-aminobiphenyl 169 0.81
aniline 93 1.04
o-anisidine 108 0.43
anthracene dlO 178/188
aramite 185 0.19
benzanthrone 230 0.15
1,3-benzenediol 110 0.78
benzenethiol 110 0.18
benzidine d8 184/192
benzo(a)anthracene d!2 228/240
benzo(b)fluoranthene d!2 252/264
benzo(k)fluoranthene d!2 252/264
benzo(a)pyrene d!2 252/264
benzo(ghi)perylene d!2 276/288
2,3-benzofluorene 216 0.35
benzoic acid 105 0.16
benzyl alcohol 79 0.47
biphenyl dlO 154/164
bis(2-chloroethyl) ether d8 93/101
bis(2-chloroethoxy)methane d8 93/97
bis(2-chloroisopropyl) ether d!2 121/131
bis(2-ethylhexyl) phthalate d4 149/153
2-bromochlorobenzene 111 0.33
3-bromochlorobenz ene 192 0.40
4-bromophenyl phenyl ether d5 248/255
butyl benzyl phthalate d4 149/153
n-CIO d22 55/66
n-C12 d26 55/66
n-C14 55
n-C16 d34 55/66
n-C18 55
n-C20 d42 55/66
n-C22 55
n-C24 d50 55/66
n-C26 55
n-C28 55
n-C30 d62 55/66
carbazole d8 167/175
4-chloro-2-nitroaniline 172 0.20
5-chloro-o-toluidine 106 0.50
4-chloroaniline 127 0.73
2-chloronaphthalene d7 162/169
3-chloronitrobenzene 157 0.18
4-chlorophenyl phenyl ether d5 204/209
3-chloropropionitrile 54 0.42
chrysene d!2 228/240
o-cresol 108 0.59
crotoxyphos 127 0.017
1625C E-205
-------
p-cymene d!4
2,6-di-tert-butyl-p-benzoquinone
di-n-butyl phthalate d4
2,4-diaminotoluene
dibenzo(a,h)anthracene d!4
dibenzofuran d8
dibenzothiophene d8
1,2-dibromo-3-chloropropane
2,6-dichloro-4-nitroaniline
1,3-dichloro-2-propanol
2,3-dichloroaniline
1,2-dichlorobenzene d4
1,3-dichlorobenzene d4
1,4-dichlorobenzene d4
3,3'-dichlorobenz idine d6
2,2'-difluorobiphenyl (int std)
2,3-dichloronitrobenzene
1,2:3,4-diepoxybutane
diethyl phthalate d4
3,3'-dimethoxybenzidine
dimethyl phthalate d4
dimethyl sulfone
p-dimethylaminoazobenzene
7,12-dimethylbenz(a)anthracene
N,N-dimethylformamide
3,6-dimethylphenanthrene
2,4-dimethylphenol d3
1,3-dinitrobenz ene
2,4-dinitrotoluene d3
2,6-dinitrptoluene d3
di-n-octyl phthalate d4
diphenylamine dlO
diphenyl ether dlO
diphenyldisulfide
1,2-diphenylhydrazine (2) dlO
ethyl methanesulfonate
ethylenethiourea
ethynylestradiol 3-methyl ether
fluoranthene dlO
fluorene dlO
hexachlorobenzene 13C6
hexachlorobutadiene 13C4
hexachloroethane ^3C
hexachlorocyclopentadiene 13C4
hexachloropropene
indeno(1,2,3-cd)pyrene
isophorone dS
2-isopropylnaphthalene
isosafrole
longifolene
malachite green
methapyrilene
methyl methanesulfonate
2-methylbenzothiazole
3-methylcholanthrene
4,4'-methylenebis(2-chloroaniline)
4,5-methylenephenanthrene
1-methylfluorene
119/130
220
149/153
122
278/292
168/176
184/192
157
124
79
161
146/152
146/152
146/152
252/258
190
191
55
149/153
244
163/167
79
120
256
73
206
122/125
168
165/168
165/167
149/153
169/179
170/180
218
77/82
109
102
227
202/212
166/176
284/292
225/231
201/204
237/241
213
276
82/88
170
162
161
330
97
80
149
268
231
190
180
0.078
0.059
0.22
0.019
0.68
0.47
0.11
0.27
0.19
0.40
0.23
0.58
0.51
0.72
0.24
0.25
0.28
0.22
0.28
0.23
0.32
0.33
0.14
0.43
0.20
0.59
0.59
0.21
0.44
0.37
1625C E-206
-------
2-methylnaphthalene
1-methylphenanthrene
2-(methylthio)benzothiazole
naphthalene d8
1,5-naphthalenediamine
1,4-naphthoquinone
alpha-naphthylamine
beta-naphthylamine d7
5-nitro-o-toluidine
2-nitroaniline
3-nitroaniline
4-nitroaniline
nitrobenzene d5
4-nitrobiphenyl
N-nitrosodi-n-butylamine
N-nitrosodi-n-propylamine d!4
N-nitrosodiethylamine
N-nitrosodimethylamine d6
N-nitrosodiphenylamine (3) d6
N-nitrosomethylethylamine
N-nitrosomethylphenylamine
N-nitrosomorpholine
N-nitrosopiperidine
pentachlorobenzene
pentachloroethane
pentamethyIbenzene
perylene
phenacetin
phenanthrene d10
phenol d5
phenothiazine
1-phenylnaphthalene
2-phenylnaphthalene
alpha-picoline d7
pronamide
pyrene dlO
pyridine
safrole
sgualene
styrene d5
alpha-terpineol d3
1,2,4,5-tetrachlorobenzene
thianaphthene
thioacetamide
thioxanthone
o-toluidine
1,2,3-trichlorobenzene d3
1,2,4-trichlorobenzene d3
1,2,3-trimethoxybenzene
2,4,5-trimethylaniline
triphenylene
tripropylene glycol methyl ether
1,3,5-trithiane
(1) referenced to 2,2'-difluorobiphenyl
(2) detected as azobenzene
(3) detected as diphenylamine
142
192
181
128/136
158
158
143
143/150
152
138
138
138
128/128
199
84
70/78
102
74/80
169/175
88
106
56
114
248
117
148
252
108
178/188
94/71
199
204
204
93/100
173
202/212
79
162
69
104/109
59/62
216
134
75
212
106
180/183
180/183
168
120
228
59
138
0.99
0.65
0.42
0.085
0.021
0.89
0.31
0.39
0.27
0.11
0.35
0.47
0.45
0.33
0.024
0.49
.41
25
0.20
0.42
0.30
0.38
0,
0,
0.15
0.48
0.73
0.31
0.68
0.45
0.042
0.43
1.52
0.28
0.23
1.04
0.48
0.28
1.32
0.092
0.15
1625C E-207
-------
Table 9
Acid Extractable Compound Characteristic m/z's
Compound
Labeled
analog
d2
d4
benzoic acid
4-chloro-3-methyIpheno1
2-chlorophenol
p-cresol
3,5-dibromo-4-hydroxybenzonitrile
2,4-dichlorophenol d3
2,6-dichlorophenol
2,4-dinitrophenol d3
hexanoic acid
2-methyl-4,6-dinitrophenol d2
2-nitrophenol d4
4-nitrophenol d4
pentachlorophenol 13C6
2,3,4,6-tetrachlorophenol
2,3,6-trichlorophenol d2
2,4,5-trichlorophenol d2
2,4,6-trichlorophenol d2
(1) referenced to 2,2'-difluorobiphenyl
Primary m/z
105
107/109
128/132
108
277
162/167
162
184/187
60
198/200
139/143
139/143
266/272
232
196/200
196/200
196/200
Response
Factor (l)
0.16
0.61
0.12
0.42
0.62
0.17
1625C
E-208
-------
Table 10
Acceptance Criteria for Performance Tests
EGD
No.
(I) Compound
301 acenaphthene
201 acenaphthene-dlO
377 acenaphthylene
277 acenaphthylene-d8
378 anthracene
278 anthracene-dIO
305 benzidine
205 benzidine-d8
372 benzo(a) anthracene
272 benzo(a)anthracene-d!2
374 benzo(b) fluoranthene
274 benzo(b) fluoranthene-d!2
375 benzo(k) fluoranthene
275 benzo(k) fluoranthene-d!2
373 benzo(a)pyrene
273 benzo(a)pyrene-d!2
379 benzo(ghi)perylene
279 benzo(ghi)perylene-d!2
712 biphenyl (Appendix C)
612 biphenyl-dlO
318 bis(2-chloroethyl) ether
218 bis(2-chloroethyl) ether-d8
343 bis (2-chloroethoxy) methane
243 bis(2-chloroethoxy)methane-d8 (3
342 bis(2-chloroisopropyl) ether
242 bis ( 2-chloroisopropy 1 ) ether-d!2
366 bis(2-ethylhexyl) phthalate
266 bis(2-ethylhexyl) phthalate-d4
341 4-bromophenyl phenyl ether
241 4-bromophenylphenyl ether-d5(3)
367 butyl benzyl phthalate
267 butyl benzyl phthalate-d4 (3)
717 n-CIO (Appendix C)
617 n-C10-d22
706 n-C12 (Appendix C)
606 n-C12-d26
518 n-C14 (Appendix C) (3)
719 n-C16 (Appendix C)
619 n-C16-d34
520 n-C18 (Appendix C) (3)
721 n-C20 (Appendix C)
621 n-C20-d42
522 n-C22 (Appendix C) (3)
723 n-C24 (Appendix C)
623 n-C24-d50
524 n-C26 (Appendix C) (3)
525 n-C28 (Appendix C) (3)
Initial
precision
and accuracy
Section 8.2.3
fua/L}
s
21
38
38
31
41
49
119
269
20
41
183
168
26
114
26
24
21
45
41
43
34
33
27
)33
17
27
31
29
44
52
31
29
51
70
74
53
109
33
46
39
59
34
31
11
28
35
35
79
38
69
39
58
31
16
ns
65
25
32
11
59
15
62
35
72
29
75
28
55
29
43
29
81
35
69
32
44
40
19
32
24
ns
35
ns
ns
80
37
42
53
34
45
80
27
35
35
X
-
-
-
-
(2)
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
labeled
compound
recovery
Sec 8.3
and 14.2
p m
134
147
186
146
174
194
518
ns
168
298
545
577
143
514
195
181
160
268
148
165
196
196
153
196
138
149
220
205
140
161
233
205
195
298
369
331
ns
162
162
131
263
172
152
139
211
193
193
20
23
14
ns
12
ns
ns
21
14
ns
15
15
20
18
19
18
ns
ns
18
19
15
- 270
- 239
- 419
ns
- 605
ns
- ns
- 290
- 529
- ns
- 372
- 372
- 260
- 364
- 325
- 364
ns
ns
- 308
- 306
- 376
calibra-
tion
verifi-
cation
Sec 12.5
fua/mL)
80
71
60
66
60
58
34
ns
70
28
61
14
13
13
78
12
69
13
58
52
61
52
44
52
67
44
76
43
52
57
22
43
42
44
60
41
37
72
54
40
54
62
40
65
50
26
26
- 125
- 141
- 166
- 152
- 168
- 171
- 296
ns
- 142
- 357
- 164
- ns
ns
ns
- 129
- ns
- 145
ns
- 171
- 192
- 164
- 194
- 228
- 194
- 148
- 229
- 131
- 232
- 193
- 175
- 450
- 232
- 235
- 227
- 166
- 242
- 268
- 138
- 186
- 249
- 184
- 162
- 249
- 154
- 199
- 392
- 392
On-going
accuracy
Sec 12.7
R fuo/L)
72
30
61
33
50
23
11
ns
62
22
20
ns
53
ns
59
32
58
25
62
17
50
25
39
25
77
30
64
28
35
29
35
28
19
ns
29
ns
ns
71
28
35
46
29
39
78
25
31
31
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
144
180
207
168
199
242
672
ns
176
329
ns
ns
155
685
206
194
168
303
176
267
213
222
166
222
145
169
232
224
172
212
170
224
237
504
424
408
ns
181
202
167
301
198
195
142
229
212
212
1625C
E-209
-------
726 n-C30 (Appendix C) 32 61 - 200 66 - 152 56 - 215
626 n-C30-d62 41 27 - 242 13 - 479 24 - 423 23 - 274
728 carbazole (4C) 38 36 - 165 44 - 227 31 - 188
628 carbazole-d8 (3) 31 48 - 130 29 - 215 69 - 145 40 - 156
320 2-chloronaphthalene 100 46 - 357 58 - 171 35 - 442
220 2-chloronaphthalene-d7 41 30 - 168 15 - 324 72 - 139 24 - 204
322 4-chloro-3-methylphenol 37 76 - 131 85 - 115 62 - 159
222 4-chloro-3-methylphenol-d2 111 30 - 174 ns - 613 68 - 147 14 - 314
324 2-chlorophenol 13 79 - 135 78 - 129 76 - 138
224 2-chlorophenol-d4 24 36 - 162 23 - 255 55 - 180 33 - 176
340 4-chlorophenyl phenyl ether 42 75 - 166 71 - 142 63 - 194
240 4-chlorophenyl phenyl ether-d5 52 40 - 161 19 - 325 57 - 175 29 - 212
376 chrysene 51 59 - 186 70 - 142 48 - 221
276 chrysene-d!2 69 33 - 219 13 - 512 24 - 411 23 - 290
713 p-cymene (Appendix C) 18 76 - 140 79 - 127 72 - 147
613 p-cymene-d!4 67 ns - 359 ns - ns 66 - 152 ns - 463
382 dibenzo(a,h)anthracene 55 23 - 299 13 - 761 19 - 340
282 dibenzo(a,h)anthracene-d!4 (3) 45 29 - 268 14 - 529 13 - ns 25 - 303
70S dibenzofuran (Appendix C) 20 85 - 136 73 - 136 79 - 146
605 dibenzofuran-d8 31 47 - 136 28 - 220 66 - 150 39 - 160
704 dibenzothiophene (Synfuel) 31 79 - 150 72 - 140 70 - 163
604 dibenzothiophene-d8 31 48 - 130 29 - 215 69 - 145 40 - 156
368 di-n-butyl phthalate ' 15 76 - 165 71 - 142 74 - 169
268 di-n-butyl phthalate-d4 23 23 - 195 13 - 346 52 - 192 22 - 209
325 1,2-dichlorobenzene 17 73 - 146 74 - 135 70 - 152
225 l,2-dichlorobenzene-d4 35 14 - 212 ns - 494 61 - 164 11 - 247
326 1,3-dichlorobenzene 43 63 - 201 65 - 154 55 - 225
226 l,3-dichlorobenzene-d4 48 13 - 203 ns - 550 52 - 192 ns - 260
327 1,4-dichlorobenzene 42 61 - 194 62 - 161 53 - 219
227 l,4-dichlorobenzene-d4 48 15 - 193 ns - 474 65 - 153 11 - 245
328 3,3'-dichlorobenzidine 26 68 - 174 77 - 130 64 - 135
228 3,3'-dichlorobenzidine-d6 80 ns - 562 ns - ns 18 - 558 ns - ns
331 2,4-dichlorophenol 12 85 - 131 67 - 149 83 - 135
231 2,4-dichlorophenol-d3 28 38 - 164 24 - 260 64 - 157 34 - 182
370 diethyl phthalate 44 75 - 196 74 - 135 65 - 222
270 diethyl phthalate-d4 78 ns - 260 ns - ns 47-211 ns - ns
334 2,4-dimethylphenol 13 62 - 153 67 - 150 60 - 156
234 2,4-dimethylphenol-d3 22 15 - 228 ns - 449 58 - 172 14 - 242
371 dimethyl phthalate 36 74 - 188 73 - 137 67 - 207
271 dimethyl phthalate-d4 108 ns - 640 ns - ns 50 - 201 ns - ns
359 2,4-dinitrophenol 18 72 - 134 75 - 133 68 - 141
259 2,4-dinitrophenol-d3 66 22 - 308 ns - ns 39 - 256 17 - 373
335 2,4-dinitrotoluene 18 75 - 158 79 - 127 72 - 164
235 2,4-dinitrotoluene-d3 37 22 - 245 10 - 514 53 - 187 19 - 275
336 2,6-dinitrotoluene 30 80 - 141 55 - 183 70 - 159
236 2,6-dinitrotoluene-d3 59 44 - 184 17 - 442 36 - 278 31 - 250
369 di-n-octyl phthalate 16 77 - 161 71 - 140 74 - 166
269 di-n-octyl phthalate-d4 46 12 - 383 ns - ns 21 - 467 10 - 433
707 diphenylamine (Appendix C) 45 58 - 205 57 - 176 51 - 231
607 diphenylamine-dlO 42 27 - 206 11 - 488 59 - 169 21 - 249
708 diphenyl ether (Appendix C) 19 82 - 136 83 - 120 77 - 144
608 diphenyl ether-dlO 37 36 - 155 19 - 281 77 - 129 29 - 186
337 1,2-diphenylhydrazine 73 49 - 308 75 - 134 40 - 360
237 1,2-diphenylhydrazine-dlO 35 31 - 173 17 - 316 58 - 174 26 - 200
339 fluoranthene 33 71 - 177 67 - 149 64 - 194
239 fluoranthene-dlO 35 36 - 161 20 - 278 47 - 215 30 - 187
380 fluorene 29 81 - 132 74 - 135 70 - 151
280 fluorene-dlO 43 51 - 131 27 - 238 61 - 164 38 - 172
1625C £.210
-------
16
81
56
63
227
77
15
60
55
25
23
19
64
20
39
49
33
25
28
15
23
42
138
49
33
45
37
45
37
21
49
13
40
36
161
38
138
19
29
42
49
44
48
69
57
19
57
30
30
47
57
47
90
36
51
ns
21
ns
69
ns
23
76
49
77
36
80
28
10
ns
69
18
78
41
62
14
10
ns
65
54
65
54
76
37
93
45
77
21
59
11
76
32
53
ns
42
22
15
15
82
15
58
58
43
59
43
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
124
228
251
316
ns
400
144
ns
299
156
133
133
247
139
157
ns
ns
161
265
140
145
146
398
ns
ns
142
126
142
126
140
212
119
130
127
210
149
380
152
176
221
281
234
292
229
212
136
212
137
137
183
205
183
13
ns
ns
ns
33
16
14
ns
ns
27
ns
ns
26
26
18
24
ns
ns
18
ns
ns
ns
ns
21
21
- 595
- ns
ns
ns
- 193
- 527
- 305
ns
ns
- 217
ns
ns
- 256
- 256
- 412
- 241
ns
ns
- 303
ns
- 672
- 592
- 592
- 363
- 363
78
38
74
68
71
47
77
47
13
70
52
69
56
73
71
39
44
85
46
77
61
55
35
39
44
68
59
63
59
77
42
75
67
65
48
60
31
76
48
65
44
54
20
60
61
78
61
56
56
69
81
69
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
128
265
135
148
141
212
129
211
761
142
194
145
177
137
141
256
230
115
219
129
163
183
287
256
230
148
170
148
170
130
237
133
149
155
208
165
324
132
210
153
228
186
502
167
163
128
163
180
180
144
123
144
85
23
43
ns
13
ns
67
ns
19
70
44
72
28
75
22
ns
ns
65
15
75
37
51
ns
ns
ns
53
40
53
40
71
29
87
34
62
ns
50
ns
72
28
48
ns
38
18
11
10
77
10
51
51
34
48
34
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
132
321
287
413
ns
563
148
ns
340
168
147
142
307
149
192
ns
ns
169
314
145
158
175
ns
ns
ns
173
166
173
166
150
254
126
168
154
ns
174
608
159
196
244
343
258
339
297
282
144
282
153
153
226
244
226
309 hexachlorobenzene
209 hexachlorobenzene-13C6
352 hexachlorobutadiene
252 hexachlorobutadiene-13C4
312 hexachloroethane
212 hexachloroethane-13Cl
353 hexachlorocyclopentadlene
253 hexachlorocyclopentadiene-13C4
083 ideno(l,2,3-cd)pyrene (3)
354 isophorone
254 isophorone-d8
360 2-methyl-4,6-dinitrophenol
260 2-methyl-4,6-dinitrophenol-d2
355 naphthalene
255 naphthaIene-d8
702 beta-naphthylamine (Appendix C)
602 beta-naphthylamine-d7
356 nitrobenzene
256 nitrobenzene-d5
357 2-nitrophenol
257 2-nitrophenol-d4
358 4-nitrophenol
258 4-nitrophenol-d4
361 N-nitrosodimethylamine
261 N-nitrosodimethylamine-d6 (3)
363 N-nitrosodi-n-propylamine
263 N-nitrosodi-n-propylamine (3)
362 N-nitrosodiphenylamine
262 N-nitrosodiphenylamine-d6
364 pentachlorophenol
264 pentachlorophenol-13C6
381 phenanthrene
281 phenanthrene-dlO
365 phenol
265 phenol-d5
703 alpha-picoline (Synfuel)
603 alpha-picoline-d7
384 pyrene
284 pyrene-dlO
710 styrene (Appendix C)
610 styrene-d5
709 alpha-terpineol (Appendix C)
609 alpha-terpineol-d3
729 1,2,3-trichlorobenzene (4c)
629 1,2,3-trichlorobenzene-d3 (3)
308 1,2,4-trichlorobenzene
208 1,2,4-trichlorobenzene-d3
530 2,3, 6-trichlorophenol (4c) (3)
731 2,4,5-trichlorophenol (4c)
631 2,4,5-trichlorophenol-d2 (3)
321 2,4,6-trichlorophenol
221 2,4, 6-trichlorophenol-d2
(1) Reference numbers beginning with 0, 1 or 5 indicate a pollutant quan-
tified by the internal standard method; reference numbers beginning with 2
or 6 indicate a labeled compound quantified by the internal standard
method; reference numbers beginning with 3 or 7 indicate a pollutant quan-
tified by isotope dilution.
1625C E-211
-------
(2) ns no specification: limit is outside the range that can be measured
reliably.
(3) This compound is to be determined by internal standard; specification
is derived from related compound.
10-
1.0-
0.1-
TI I Ti
2 10 20 SO 100 200
CONCENTRATION (ug/mL)
AREA. 4780
AREA-43000
AREA 40300
FIGURE 1 Relative Response Calibration Curve
for Phenol. The Dotted Lines Enclose a ±10
Percent Error Window.
FIGURE 3 Extracted Ion Current Profiles for (3A)
Unlabeled Compound, (38) Labeled Compound,
and (3C) Equal Mixture of Unlabeled and Labeled
Compounds.
FIGURE 2 Extracted Ion Current Profiles for
Chromatographically Resolved Labeled (m,/z) and
Unlabeled (m,/z) Pairs.
1625C E-212
-------
STANDARD
BLANK
SAMPLE
[10.2.1 &
10.2.3]
[10.2.1.3 &
10.2.3.2]
[10.2.3.3]
[10.2.4]
[10.3 &
10.3.2]
1 L REAGENT
WATER
1 L REAGENT
WATER
1 L ALIQUOT
SPIKE 500 pL
OF 200 pg/mL
ISOTOPES
SPIKE 500 pL
OF 200 pg/mL
ISOTOPES
SPIKE 500 pL
OF 200 pg/mL
ISOTOPES
SPIKE 1.0 mL
OF STANDARDS
STIR AND
EQUILIBRATE
STIR AND
EQUILIBRATE
STIR AND
EQUILIBRATE
STANDARD OR BLANK
EXTRACT BASE/
NEUTRAL
ORGANIC
EXTRACT BASE/
NEUTRAL
AQUEOUS
ORGANIC
AQUEOUS
[10.3.4]
EXTRACT ACID
[10.5]
CONCENTRATE
TO 2-4 mL
CONCENTRATE
TO 2-4 mL
EXTRACT ACID
[10.6]
[11.31
CONCENTRATE
TOLOmL
CONCENTRATE
TO 1.0 mL
CONCENTRATE
TO 1.0 mL
ADO INTERNAL
STANDARD
ADO INTERNAL
STANDARD
ADD INTERNAL
STANDARD
{11.41
INJECT
INJECT
INJECT
FIGURE 4 Flow Chart for Extraction/Concentration of Precision and Recovery Standard, Blank,
and Sample by Method 1625. Numbers in Brackets I I Refer to Section Numbers in the Method.
1625C
E-213
-------
3S(VM
1 1 1 1 L 1 1 J_. 1
ANTHRACENE-D*
*" «
123458789 10
ANALYSIS NUMBER
o
1.lO-
0.90
1 1 1 1
ANTHRACENE
_.
8/1 8/1 8/1 8/1 « 8/2 8/3 8/3 8/4 8/5
DATE ANALYZED
-3s
FIGURE 5 Quality Control Charts Showing Area (top graph) and
Relative Response of Anthracene to Anthracene-d10 (lower graph)
Plotted as a Function of Time or Analysis Number.
tic O*TM
I3-13/44 3i24:«» CM.Il J«N10U« II
SMTlfl M.e.ua.MtM.M.C.HMttt.NM _
COWS.: l(2M.MH.».2Ml.it3I.M-2MM.I9eM.3ICII^S
MMXl 6 l.SM LMCLl N 2. 3.» QUMi » :. 2.» J *
i TO
U 2i. 3
'1C.
t*M
ISlS*
I9M
23145
rant.
47: M T1IC
FIGURE 6 Chromatogram of Combined Acid/base/neutral Standard.
1625C E-214
-------
Appendix A: Mass Spectra in the Form of Mass/Intensity Lists
555 acetophenone
m/z int.
42 21
61 13
75 36
105 1000
556 4-aminobiphenyl
m/z int. m/z int.
51 55 63 65
139 65 141 132
m/z
43
62
76
106
int.
245
26
62
87
m/z
49
63
77
120
int.
19
422
941
479
m/z
50
65
78
121
int.
221
31
11
38
m/z
51
73
89
int^
524
13
12
m/z
52
74
91
int.
75
64
22
m/z int.
72 82
167 163
m/z int.
83 73
168 280
m/z int.
85 163
169 1000
557
m/z
40
51
63
91
aniline
int.
65
47
59
10
m/z
41
52
64
92
int.
66
54
33
136
m/z
42
53
65
93
int.
16
12
226
1000
m/z
46
54
66
94
int.
11
40
461
73
m/z
47
61
74
int.
75
17
11
m/z
50
62
78
int.
40
28
14
558 o-anisidine
m/z
40
53
65
80
108
int.
22
286
142
915
1000
m/z
41
54
66
81
109
int.
43
39
20
41
55
m/z
42
61
76
92
122
int.
10
12
13
47
123
m/z
50
62
77
93
844
int.
60
25
36
14
124
m/z
51
63
68
94
56
int.
106
43
32
18
m/z
52
64
79
105
int^
202
24
25
18
559 aramite
m/z int. m/z int.
41 606 57 758
77 155 91 339
163 143 175 182
319 270 334 137
560 benzanthrone
m/z int. m/z int.
74 69 75 71
101 278 150 58
202 762 203 126
561 1,3-benzenediol
m/z
59
105
185
int.
328
153
1000
m/z
63
107
187
int.
782
239
328
m/z
65
121
191
int.
285
107
346
m/Z
74
123
197
int.
113
120
191
m/z int.
87 97
174 67
230 1000
m/z int.
38 160
199 63
231 177
m/z int.
99 69
200 350
m/z
40
51
62
71
111
int.
64
54
27
16
51
m/z
41
52
63
81
int.
19
29
74
201
m/z
52
53
64
82
int.
42
184
61
251
m/z
43
54
65
95
int.
36
89
13
13
m/z
49
55
68
109
int.
11
97
56
11
m/z
50
61
69
110
int.
43
15
119
1000
562 benzenethiol
m/z int. m/z
45 128 50
77 161 84
m/z int.
51 205
109 316
m/z int.
65 175
110 1000
m/z int.
66 505
111 102
m/z
52
74
91
m/z
115
170
m/z
50
62
78
m/z
52
64
79
105
m/z
74
123
197
m/z
100
201
m/z
50
61
69
110
m/z
69
int.
75
64
22
int.
142
216
int.
40
28
14
int^
202
24
25
18
int.
113
120
191
int.
215
236
int.
43
15
119
1000
int.
114
1625C E-215
-------
563 2,3-benzofluorene
m/z int. m/z int. m/z int. m/z int. m/z int.
74 52 81 69 94 143 95 253 106 60
108 491 187 75 189 90 213 233 214 "60
216 1000 217 166
943 benzoic acid
m/z int. m/z int. m/z int. m/z int. m/z int.
45 29 50 221 51 413 52 45 66 11
75 25 76 81 77 778 78 76 105 1000
564 benzyl alcohol
m/z int.
107 205
215 987
m/z int.
74 53
122 868
m/Z
40
61
75
89
108
int.
17
11
13
65
737
m/z
59
62
76
90
109
int.
16
31
18
64
43
m/z
50
63
77
91
int.
155
70
565
125
m/z
51
64
78
105
int.
319
12
116
38
m/z
52
65
79
106
int.
78
75
1000
18
m/z
53
74
80
107
int.
84
35
73
523
565 2-bromochlorobenzene
m/z int. m/z int. m/z int. m/z int. m/z int. m/z int.
49 237 50 890 51 183 73 158 74 506 75 1000
76 202 111 961 113 287 190 638 192 809 194 193
566 3-bromochlorobenzene
m/z int. m/z int. m/z int. m/z int. m/z int. m/z int.
49 201 50 834 51 174 73 169 74 509 75 914
76 197 111 1000 113 301 190 625 192 802 194 191
567 4-chloro-2-nitroaniline
m/z
49
63
76
126
int.
119
1000
127
766
m/Z
50
64
78
128
int.
174
315
152
234
m/z
51
65
90
142
int.
260
192
724
211
m/z
52
73
91
172
int.
531
290
253
915
m/z int.
61 205
74
101
174 -
105
232
289
m/z
62
75
114
int.
394
156
312
568 5-chloro-o-toluidine
m/z int. m/z int. m/z int. m/z int. m/z int. m/z int.
50 115 51 261 52 257 53 137 77 420 78 134
79 140 89 152 106 1000 140 599 141 964 142 265
143 313
569 4-chloroaniline
m/z int. m/z int. m/z int. m/z int. m/z int. m/z int.
41 60 62 55 63 147 64 135 65 329 73 51
91 63 92 186 99 67 100 115 127 1000 128 81
129 292
570 3-chloronitrobenzene
m/z int. m/z int. m/z int. m/z int. m/z int. m/z int.
50 619 51 189 73 144 74 330 75 1000 76 169
85 101 99 258 111 851 113 266 157 424 159 137
571 o-cresol
m/z int. m/z int. m/z int. m/z int. m/z int.
50 102 51 181 53 144 77 358 79 380
89 114 90 231 107 783 108 1000
1625C E-216
-------
944 p-cresol
m/z int. m/2. int. m/z. int.
50 136 51 224 52 106
80 145 90 122 107 822
572 crotoxyphos
m/z int. m/z int. m/z int.
40 633 44 448 67 42
105 484 109 21 127 1000
573 2,6-di-t-butyl-p-benzoquinone
m/z int. m/z int. m/z int.
51 392 53 586 55 325
77 376 79 308 91 456
135 538 136 240 149 429
220 410
574 2,4-diaminotoluene
m/z int. m/z int.
40 70 42 55
67 50 77 147
105 134 106 67
575 1,2-dibromo-3-chloropropane
m/z int. m/z int. m/z int.
42 38 59 341 51 104
77 331 81 43 93 117
106 17 119 74 121 66
159 204 187 10
945 3,5-dibromo-4-hydroxybenzonitrile
m/z int. m/z int. m/z int.
53 148 61 193 62 222
170 141 275 489 277 1000
*
576 2,6-dichloro-4-nitroaniline
m/z int. m/z int. m/z int.
41 206 52 1000 61 523
65 137 89 218 90 443
133 218 160 401 176 431
577 1,3-dichloro-2-propanol
m/z int. m/z int. m/z int.
40 14 42 55 43 503
49 113 50 15 51 37
78 11 79 1000 80 25
578 2,3-dichloroaniline
m/z int. m/z int. m/z int.
52 138 61 151 62 265
73 130 90 460 99 202
163 626 165 101
m/z int.
53 196
108 1000
m/z int.
77 70
166 180
m/z int.
57 668
95 322
163 292
m/z int.,
77 420
m/z int.
79 41
193 401
m/z int.
65 416
107 248
177 1000
m/z
88
279
m/z
62
97
178
m/z
44
57
81
m/z
63
125
int.
632
451
int.
828
458
134
int.
22
10
310
int.
455
108
m/z int.
117 137
m/z int.
63 588
124 954
206 378
m/z int.
47 12
61 12
m/z int.
64 142
126 149
m/z
79
m/z
104
194
m/z
67
121
205
int.
308
j.nt.
100
20
int.
927
255
203
m/z
51
78
121
int.
76
69
958
m/z
52
93
122
int.
70
63
1000
m/Z
53
94
123
int.
51
224
79
m/z
61
104
int.
91
128
m/z
61
95
155
int.
38
106
635
m/z
75
97
157
int.
1000
12
784
m/z int.
76 75
105
158
67
20
m/z
168
m/z int.
73 470
126 401
m/z int.
58 15
75 14
m/z int.
65 105
161 1000
1625C E-217
-------
579 2,3-dichloronitrobenzene
m/z int. m/z int. m/z int. m/z int.
49 220 50 257 61 150 62 120
74 976 75 743 84 351 85 166
110 204 111 303 133 701 135 435
161 190 163 121 191 411 193 263
946 2,6-dichlorophenol
m/z Int. m/z int. m/z int. m/z int.
49 111 62 160 63 714 73 132
126 260 162 1000 164 613 166 101
580 l,2:3,4-diepoxybutane
m/z int. m/z int. m/z int. m/z int.
40 37 41 29 42 83 43 60
57 155 58 16 85 13
581 3,3'-dimethoxybenzidine
m/z int. m/z int. m/z int. m/z int.
65 44 79 222 85 69 93 84
122 115 158 154 186 144 201 552
245 152
582 dimethyl sulfone
m/z int. m/z int. m/z int. m/z int.
44 10 45 94 46 29 47 18
63 69 64 22 65 19 79 1000
96 23
583 p-dimethylaminoazobenzene
m/z int. m/z int. m/z int. m/z int.
42 483 51 181 77 447 78 120
104 142 105 190 120 1000 148 160
584 7,12-dimethylbenzo(a)anthracene
m/z int. m/z int. m/z int. m/z int.
101 24 112 34 113 112 114 38
125 46 126 81 127 60 128 76
237 23 239 313 240 230 241 433
252 68 253 33 255 84 256 1000
585 N,N-dimethylformamide
m/z int. m/z int. m/z int. m/z int.
40 58 41 79 42 497 43 115
57 17 58 83 72 89 73 994
586 3,6-dimethyIphenanthrene
m/z int. m/z int. m/z int. m/z int.
76 113 89 129 94 179 101 142
190 193 191 430 205 246 206 1000
587 1,3-dinitrobenzene
m/z int. m/z int. m/z int. m/z int.
50 1000 51 131 63 228 64 218
76 664 92 240 122 166 168 399
m/z int.
63 173
86 125
145 580
m/z int.
98 293
m/z int.
55 1000
m/z int.
107 46
229 162
m/z int.
48 69
81 36
m/z int.
79 147
225 676
m/z int.
119 212
215 24
242 61
257 180
m/z int.
44 1000
74 35
m/z int.
102 151
207 159
m/z int.
74 311
m/z
99
m/z
56
m/z
115
244
m/z
62
94
m/z
91
m/z
120
226
250
m/z
45
m/z
189
m/z
75
int.
117
int.
67
int.
110
1000
int.
14
528
int.
109
int.
296
47
32
int.
19
int.
388
int.
623
1625C E-218
-------
588 diphenyldisulfide
m/z int. m/z int. m/z int.
50 153 51 293 65 671
110 132 154 191 185 117
589 ethyl methanesulfonate
m/z int. m/z int. m/z int.
42 16 43 72 45 208
64 22 65 93 79 1000
97 206 109 579 111 18
590 ethylenethiourea
m/z int. m/z int. m/z int.
41 46 42 126 45 97
73 151 102 1000
591 ethynylestradiol 3-methyl ether
m/z int. m/z int. m/z int.
41 155 53 101 91 157
160 115 173 199 174 313
310 516
592 hexachloropropene
m/z int. m/z int. m/z int.
47 131 71 333 106 334
141 206 143 196 211 631
947 hexanoic acid
m/z int. m/z int.
41 627 42 535
56 90 57 102
73 412 74 56
593 2-isopropylnaphthalene
m/z int. m/z int. m/z int.
51 100 63 111 76 157
128 216 152 133 153 184
170 368
m/z int.
59 282
218 418
m/z
77
int.
141
m/z int.
109 1000
ro/z
48
80
123
int.
40
127
15
m/z int.
59 19
81
124
42
33
m/z int.
63 23
96 16
m/z int.
46 42
m/z int.
115 143
227 1000
m/z int.
108 200
213 1000
m/z
59
m/z
147
228
int.
14
int.
226
149
m/z int.
117 329
215 623
m/z int.
72 89
m/z int.
159 132
242 153
m/z int.
119 320
217 186
m/z
43
60
87
int.
214
1000
98
m/z
45
61
int.
186
66
m/z
46
69
int.
19
21
m/z
55
70
int.
128
20
m/z int.
77 129
154 114
m/z int.
115 147
155 1000
m/z int.
127 131
156 139
594 isosafrole
m/z int. m/z int. m/z int. m/z
50 110 51 222 63 127 77
104 441 131 371 132 107 135
595 longifolene
m/z int. m/z int.
53 438 55 719
91 1000 93 611
119 394 133 338
596 malachite green
m/z int. m/z int. m/z int. m/z
118 113 126 313 165 369 208
237 158 253 1000 254 160 329
int.
277
129
m/z
78
161
int.
208
250
m/z
103
162
int.
355
1000
m/z
65
94
161
int.
346
546
568
m/z
67
95
204
int.
453
404
172
m/z
77
105
int.
566
614
m/z
69
107
int.
713
475
int.
135
189
ro/z
209
330
int.
233
775
m/z
210
331
int.
181
170
1625C
E-219
-------
597 methapyriline
m/z int. m/z int. m/z int. m/z int.
42 72 45 47 53 40 58 1000
78 54 79 48 97 516 190 40
598 methyl methanesulfonate
m/z int. m/z int. m/z int. m/z int.
45 178 56 15 48 108 50 26
65 285 78 27 79 821 80 1000
95 137 109 59 110 60
599 2-methylbenzothiozole
m/z int. m/z int. m/z int. m/z int.
45 152 50 133 58 153 62 106
82 204 108 392 109 102 148 279
900 3-methylcholanthrene
m/z int. m/z int. m/z int. m/z int.
113 58 119 55 125 83 126 305
134 160 250 56 252 322 253 271
266 50 267 192 268 1000 269 185
901 4,4'-methylenebis(2-chloroaniline)
m/z int. m/z int. m/z int. m/z int.
77 190 84 107 98 299 104 133
195 352 229 228 231 1000 233 227
267 144 268 358
902 4,5-methylenephenanthrene
m/z int. m/z int. m/z int.
50 50 62 55 63 95
87 60 94 255 95 659
189 900 190 1000
903 1-methylfluorene
m/z int. m/z int.
50 66 51 87
76 196 83 135
139 54 151 73
166 136 176 96
181 99
904 2-methylnaphthalene
m/z int.
74 69
163 80
m/z
63
81
m/z
63
149
m/z
132
263
m/z
115
265
m/z
81
187
int.
35
44
int.
309
1000
int.
99
59
int.
226
171
int.
145
213
m/z int.
72 225
m/z int.
64 48
82 33
m/z
69
150
m/z
133
265
m/z
140
266
m/z
86
188
513
110
int.
122
106
int.
316
631
int.
53
137
m/z
62
87
152
177
int.
57
53
124
52
m/z
63
88
163
178
int.
137
78
57
202
m/z
74
89
164
179
int.
64
203
58
182
m/z
75
90
165
180
int.
85
58
1000
686
m/z
50
65
76
114
141
int.
29
19
14
13
748
m/z
51
69
77
115
142
int.
39
56
15
303
1000
m/z
57
70
86
116
143
int.
28
25
13
25
105
m/2
58
71
87
126
int.
47
126
18
13
m/2
62
74
89
139
int.
26
25
42
98
m/z
63
75
113
140
int.
65
23
19
24
905 1-methylphenanthrene
m/2 int. m/2 int. m/2 int. m/z int. m/z int. m/z int.
51 54 63 86 70 62 74 51 81 52 83 164
96 132 163 55 165 217 189 165 191 532 192 1000
193 152
1625C E-220
-------
906 2-(methylthio)benzothiazole
m/2 int. m/2 int. m/2 int.
45 790 50 212 63 383
136 239 148 938 180 250
907 1,5-naphthalenediamine
m/z int. m/z int. m/z int.
51 48 65 83 77 75
130 262 131 40 141 43
908 1,4-naphthoquinone
m/z int. m/z int.
50 445 51 62
76 590 101 51
158 1000 159 100
909 alpha-naphthylamine
m/z int. m/z int.
50 25 51 31
65 27 71 58
115 401 116 212
910 5-nitro-o-toluidine
m/z int. m/z int.
51 194 52 159
94 168 104 120
911 2-nitroaniline
m/z int. m/z int.
41 64 50 51
63 181 64 155
92 566 108 170
912 3-nitroaniline
m/z int. m/z int.
41 101 52 120
65 1000 66 114
108 87 138 717
913 4-nitroaniline
m/z int. m/z int.
52 228 53 160
66 124 80 266
914 4-nitrobiphenyl
m/z int. m/z int.
51 131 63 104
152 902 153 284
m/z int.
52 52
102 613
m/z int.
57 36
72 104
142 53
m/z int.
53 121
106 691
m/z int.
62 110
92 300
m/z int.
76 179
169 374
915 N-nitroso-di-n-butylamine
m/2 int. m/z int. m/z int.
41 1000 42 536 43 570
57 994 84 985 86 103
158 161
m/z int.
69 578
181 1000
m/z int.
79 111
157 89
m/z int.
66 69
103 52
m/z int.
59 46
89 62
143 1000
m/z int.
77 766
152 1000
m/z int.
103 86
158 1000
m/z int.
74 189
104 550
m/z int.
62 28
113 22
144 101
m/2 int.
78 176
m/2 int.,
108 627
m/z int.
118 52
159 117
m/2 int.
75 205
130 433
m/2 int.
63 59
114 34
m/2 int.
79 619
m/2
51
65
138
int.
89
960
1000
m/2
52
66
139
int.
207
96
63
m/2
53
80
int.
74
212
m/2
62
91
int.
58
86
m/2
53
80
139
int.
59
169
51
m/2
62
91
int.
58
62
ro/2
63
92
int.
143
764
m/2
64
93
int.
121
62
m/z
63
108
m/z
115
199
m/z
44
99
int.
216
636
int.
134
1000
int.
313
197
m/z
64
138
m/2
141
200
m/2
55
115
int.
164
520
int.
277
125
int.
129
158
m/z
151
m/z
56
116
int.
259
int.
167
237
1625C E-221
-------
916 N-nitrosodiethylamine
m/z int. m/z int. m/z int.
41 170 42 079 43 69
56 525 57 492 70 24
102 807 103 35
917 N-nitrosomethylethylamine
m/z int. m/z int. m/z int.
40 117 42 1000 43 667
57 99 59 13 71 60
918 N-nitrosomethylphenylamine
m/z int. m/z int. m/z int.
50 181 51 434 52 104
79 331 104 147 106 673
919 N-nitrosomorpholine
m/z int. m/z int. m/z int.
41 181 42 192 43 52
56 1000 57 49 85 13
920 N-nitrosopiperidine
m/z int. m/z int. m/z int.
41 320 42 1000 43 43
54 58 55 444 56 224
83 28 84 47 114 491
921 pentachlorobenzene
m/z int. m/z int. m/z int.
73 160 108 239 125 102
217 106 248 648 250 1000
922 pentachloroethane
m/z int. m/z int.
47 203 60 398
95 165 117 1000
165 716 167 901
923 pentamethylbenzene
m/z int. m/z int. m/z int.
51 126 53 84 63 61
91 218 105 128 115 120
147 60 148 420
924 perylene
m/z int. m/z int. m/z int.
74 33 111 43 112 70
126 243 224 49 248 75
252 1000 253 219
925 phenacetin
m/z int. m/z int. m/z int.
43 443 51 33 52 112
65 47 79 31 80 179
110 50 137 461 138 40
m/z int.
44 1000
71 28
m/z int.
44 26
73 57
m/z int.
63 110
107 220
m/z int.
44 17
86 333
m/z int.
51 14
57 17
115 26
m/z int.
178 102
252 642
m/z int.
45 20
85 25
m/z int.
54 17
88 772
m/z int.
77 1000
212 137
m/z int.
54 85
87 14
m/z int.
52 12
67 21
m/z
213
254
int.
179
199
m/z int.
65 99
117 91
m/z int.
113 111
249 52
m/z int.
53 164
31 154
179 672
m/z
77
133
m/z
124
250
int.
145
1000
int.
132
284
m/z int.
56 189
89 20
m/z int.
78 194
m/z int.
55 95
116 337
m/z int.
53 32
82 26
m/z int.
215 218
m/z
62
119
169
int.
119
979
422
m/z
83
121
int.
378
306
m/z
85
130
int.
218
293
m/z
94
132
int.
114
272
m/z int.
63 39
108 1000
180 64
m/z int.
79 64
134 105
m/z int.
125 251
251 86
m/z int.
64 30
109 196
1625C E-222
-------
926 phenothiazine
m/z int. m/z. int. m/z. int.
50 145 51 120 63 134
166 240 167 607 198 186
927 i-phenylnaphthalene
m/z int. m/z int.
50 132 51 156
87 101 88 183
200 144 201 136
928 2-phenylnaphthalene
m/z int. m/z int. m/z int.
51 108 63 101 76 136
102 188 202 398 203 270
929 pronamide
m/z int. m/z int. m/z int.
41 270 66 109 74 112
145 334 147 198 173 1000
256 102 257 122
930 pyridine
m/z int. m/z int. m/z int.
40 45 48 11 49 62
53 112 54 12 55 16
78 151 79 1000 80 101
931 safrole
m/z int. m/z int. m/z int.
50 132 51 369 63 108
104 477 105 130 131 437
163 109
932 squalene
m/z int. m/z int. m/z int.
53 62 55 94 67 105
79 43 81 465 82 52
109 47 121 46 137 41
933 1,2,4,5-tetrachlorobenzene
m/z int. m/z int. m/z int.
47 125 49 176 61 127
84 197 108 284 109 231
181 224 214 791 216 1000
948 2,3,4,6-tetrachlorophenol
m/z int. m/z int. m/z int.
61 234 65 167 66 105
97 107 131 463 133 270
196 164 230 793 232 1000
934 thianaphthene
m/z int. m/z int. m/z int.
45 80 50 91 51 65
69 139 74 55 89 191
135 104 136 52
m/z
100
200
int.
128
143
m/z
154
int.
149
m/z
63
89
202
int.
148
162
643
m/z
74
100
203
int.
124
155
1000
m/z
75
101
204
int.
142
527
999
m/z
76
102
205
int.
136
111
159
m/z
88
204
m/z
75
175
int.
133
1000
int.
137
615
m/z int.
50 324
75 21
81 58
m/z int.
77 391
132 166
m/z int.
68 119
93 70
m/z
84
254
int.
194
133
m/z int.
51 414
76 19
m/z int.
78 228
161- 298
m/z
69
95
int.
1000
104
m/z
101
m/z
109
255
m/z
52
77
m/z
103
162
m/z
70
107
333
int.
186
211
int.
879
22
int.
348
'1000
int.
57
43
m/z
72
143
218
int.
183
194
482
m/z
73
145
220
int.
332
117
101
m/z
74
179
int.
448
237
m/z
83
166
234
int.
134
298
471
m/z
34
168
int.
178
273
m/2
96
194
int.
202
168
m/z int.
63 162
108 82
m/z
67
134
int.
78
1000
1625C
E-223
-------
935 thioacetamide
m/z int. ro/z int.
40 225 42 485
59 165 60 437
936 thioxanthone
m/z int. m/z int.
50 262 63 180
92 188 108 129
185 137 212 1000
937
m/z
40
52
65
78
104
o-toluidine
int.
51
164
59
113
45
m/z
41
53
66
79
106
int.
38
192
24
243
1000
m/z int.
43 44
75 1000
m/z int.
69 320
139 385
213 145
m/z int.
42 35
53 86
74 19
80 80
107 90
938 1,2,3-trimethoxybenzene
m/z int. m/z int. m/z int.
50 257 51 459 52 139
67 114 77 246 79 132
107 190 108 144 110 898
939 2,4,5-trimethylaniline
m/z int. m/z int. m/z int.
41 80 52 58 51 63
79 62 91 167 93 51
120 1000 121 87 134 670
940 triphenylene
m/z int. m/z int. m/z int.
74 52 87 55 100 107
114 181 200 67 202 56
227 132 228 1000 229 184
941 tripropylene glycol methyl ether
m/z int. m/z int. m/z int.
45 492 46 15 47 19
59 1000 60 34 71 16
103 57 117 92 161 21
942 1,3,5-trithiane
m/z int. m/z int. m/z int.
46 1000 47 150 48 98
73 102 91 92 92 111
m/z int.
46 18
76 25
m/z int.
74 116
152 227
m/z int.
49 10
62 26
65 14
89 107
m/z int.
53 276
82 117
125 578
m/z int.
101 108
224 84
m/z int.
55 17
72 44
m/z int.
59 93
110 58
m/z int.
57 36
77 43
m/z int.
69 176
183 112
m/z int.
50 88
63 68
76 21
90 76
m/Z
63
93
153
int.
112
483
759
m/z
112
225
int.
131
56
m/z int.
57 68
73 363
m/z int.
60 76
138 259
m/z int.
58 93
m/z int.
82 121
184 951
m/z int.
51 169
64 30
77 313
91 52
m/z int.
65 341
95 801
168 1000
m/z
53
117
135
int.
66
54
978
m/z
65
118
136
int.
150
65
99
m/z
67
119
int.
74
93
m/z int.
113 244
226 313
m/z int.
58 43
74 232
1625C E-224
-------
ATTACHMENT 8
E-225
-------
INSTRUCTIONS FOR USE OF LABELED COMPOUND SOLUTIONS
E-226
-------
Instructions for Use of Labeled Compound Solutions
1 Scope and application. These instructions define use of stable
isotope labeled pollutants provided by EPA for the analysis of
water and wastewater.
1.1 The solutions of mixtures listed in tables 1 through 11 for
volatiles, semi-volatiles (acids and base/neutrals), and
Appendix C compounds permit analysis of nearly all non-
pesticide organic priority pollutants by isotope dilution
methods.
1.2 These instructions were written explicitly for use with
Revision C of EPA Methods 1624 and 1625. The numbers in
brackets [ ] refer to specific section numbers in these
methods.
1.3 For accurate isotope dilution analyses, it is imperative
that identical concentrations of the labeled compounds be
used for calibration and for spiking into water samples.
1.4 Analysts unfamiliar with isotope dilution and/or GCMS
methods for analysis of organic priority pollutants in
waters should review references 1-3 before proceeding.
1.5 EPA may revise these instructions to account for new
labeled compounds, new compound concentrations, or new
mixtures of compounds.
2 Description of solutions
2.1 The solutions listed in tables 1-11 are contained in snap-
top, flame sealed ampuls. One mL is contained in each
ampule; however, this volume should not be relied upon
E-227
Rev: 10/28/86
-------
for precise measurement of solution concentrations or
total amounts of compounds present (see section 1.3).
2.1.1 EPA has discontinued the use of Mininert valves
with these solutions. It is the laboratory's
responsibility to provide valved ampules so that
changes in concentrations of the solutions by
evaporative loss are minimized.
2.2 A data sheet is attached for each solution (Tables 1-11)
giving exact concentrations of the constituents. These
concentrations are accurate to _+ 5 percent at the time
the solution was prepared. Solution concentrations are
to be monitored for changes by the laboratory [1624C:
6.5.4; 1625C: 6.15].
2.2.1 EPA may change the concentration and/or the mix-
ture and/or number of compounds in these solutions;
therefore, the laboratory shall observe the com-
pounds and concentrations in each and every solu-
tion prior to use, to insure consistency with the
compounds and concentrations in the methods.
2.3 Volatiles
2.3.1 Four solutions are provided: "purgeables/volatiles
E.I, F, G and H." (Tables 1-4)
2.3.1.1 The nominal concentration of solution G
is 250 ug/mL in methanol-d4.
2.3.1.2 Nominal concentrations of solutions E.I,
F, and H are 50 ug/mL in methanol-d4.
2.4 Semi-volatilesacids and base/neutrals.
E-228
Rev: 10/28/86
-------
2.4.1 Nominal concentrations are 5 mg/mL in benzene-dg.
2.4.2 Acidsone solution is provided: "acid extract-
ables 3. (Table 5)"
2.4.3 Base/neutralssix solutions are provided: "base/
neutrals 4.1, 4.3, 6.2, 6.3" (Tables 6-9) and
"base/ neutrals 5.1 (Table 10) " which contains
all of the priority pollutant, Appendix C, paragraph
4C, and synfuels amine compounds.
2.4.4 Appendix Cone solution is provided: "semi-
volatiles-1/Appendix C" (Table 11) , which contains
the nonamine Appendix C and synfuel base/neutral
compounds.
NOTE; In preparing this set of labeled compounds, it was
discovered that the alpha-terpineol-d3 was mis-
labeled, and was actually dibenzothiophene-d8.
Therefore, alpha-terpineol-d3 is not contained in
this solution, and dibenzothiophene-d8 is contained
at a concentration of 10 mg/mL.
2.5 The ampuls shall be opened per the procedure in section 5.
3 Storage
3.1 Unopened ampulsstore in a freezer at -20° to -10°C
until ready for use. Do not open until required.
3.2 Opened ampulsstore in a refrigerator at 0° to 4°C.
Mininert valved ampules should not be stored at tempera-
tures below 0°C as the Teflon seal on the ampule top is
not reliable below this temperature.
E-229
Rev: 2/22/85
-------
3.3 If the solutions are transferred from the ampul(s) to a
vial or other container, store below 4°C at as low a tem-
perature as practicable, consistent with a reliable seal.
3.4 Except for unopened ampuls, the storage appliance (e.g.,
refrigerator, freezer) for volatile solutions must be free
of solvent vapors which would interfere with the analysis
of either the labeled compounds or priority pollutants.
Do not store solutions of standards in methylene chloride,
benzene, dioxane or other solvents (except dilute solu-
tions in methanol) in the same appliance as the volatiles
solutions.
4 Obtaining mass spectra [1624C: 7.2; 1625C: 7.2]
4.1 If the laboratory does not have a mass spectrum of the
specific labeled compounds contained in the solutions
(tables 1-11), a spectrum should be obtained prior to
mixing the solutions (section 6) to minimize the necessity
to deconvolute multiple spectra.
4.2 Open the ampul per the procedure in section 5.
4.3 Inject 0.1 to 2 uL (or an amount as required) of the
solution into the GC. Alternatively, purge the volatiles
solution from 5 mL reagent water. Analyze the solution
under the GC conditions for the method [1624C: table 3;
1625C: tables 5 and 6] so that retention time data are
obtained.
5 Opening an ampulopen in a hood, while wearing gloves.
5.1 Materials required.
5.1.1 Needle-nosed pliers or tweezers.
E-230
Rev: 10/28/86
-------
5.1.2 Mininert valvesto be used if the solution is to
be retained in a valved ampule.
5.1.3 Syringe1 mL, cleaned, with 2 inch needle, to be
used if solution is to be removed from ampule.
5.2 Bring the ampul to room temperature. Inspect for damage
and possible loss of solvent. Notify the Sample Control
Center if loss or change has occurred.
5.3 If the solution is to be withdrawn from the ampule, be
certain that all precipitate has redissolved. Warm to no
more than 35°C (if required) before opening.
5.4 If liquid has collected in the flame seal tube area of the
ampul, tap the tube gently with a finger to dislodge the
solution from this area.
5,5 If the Mininert valve assembly is to be used, inspect the
valve for burrs or other defects which might preclude its
immediate use. If the solution is to be withdrawn from
the ampul, have the necessary syringe(s) and vial(s)
available so that loss by evaporation will be minimized.
5.6 Snap the top on the ampul. Inspect the broken edge
remaining on the ampul body. If any portion of the edge
protrudes above the rim of the ampul, this edge will cut
the bottom of the Mininert valve. Carefully break off
and remove this protruding edge using needle-nose pliers
or tweezers. Thread the Mininert valve onto the ampul
and tighten to form a seal.
5.7 Mark the solution level on the ampul label. Scrape off a
portion of the label if required for viewing the meniscus.
5.8 Document the date and operations in a standards log book.
E-231
Rev: 9/28/84
-------
6 Mixing and diluting. If a spectrum of each labeled compound
has not been obtained, refer to section 4.
6.1 The most efficient and precise use of the labeled solu-
tions results from mixing and diluting (if required) to
form single solutions for sample spiking [1624C: 6.6;
1625C: 6.8], calibration [1624C: 6.7.1; 1625C: 6.13],
and for performance verification [1624C: 6.7.2 and 11.1;
1625C: 6.14 and 12.1] .
6.2 Materials required.
6.2.1 Syringes1 mL, cleaned, with 2 inch needles.
6.2.2 Vials5 and 40 mL, cleaned, with Teflon-lined
screw caps.
6.2.3 Volumetric flask25 mL, cleaned, ground glass
stoppered.
6.2;4 Solventsmethylene chloride-d2» methanol-d4,
benzene-dg, and/or p-dioxane-dg. If p-dioxane-ds
is used, peroxides must be less than 25 ppm.
6.3 The following instructions apply if all compounds are
used at approximately the same concentration in standards,
blanks, and samples. If varied concentrations are to be
used, the volumes of solutions which are mixed need to be
suitably adjusted.
E-232
Rev: 10/28/86
-------
6.4 Volatiles
NOTE: These instructions are based on the assumption
that the volatile gases and water soluble compounds
(1624C: 6.6) will be employed at five times the level
(i.e., at 50, 100, 200, 500, and 1000 ug/L) of the other
volatile labeled compounds. If the gases and water
soluble compounds are to be employed at the same level
(i.e., at 10, 20, 50, 100, and 200 ug/L) as the other
volatile labeled compounds, the "purgeables/volatiles G"
solution must be diluted by a factor of five (5) prior
to mixing with the remaining purgeables/volatiles E.I,
F, and H solutions.
6.4.1 Open one ampul at a time per the instructions in
section 5. Withdraw the total volume of solution
in a one mL syringe. .If less than 0.8 mL is
present do not use the solution, repackage it
in the ampul and seal with the Mininert valve.
Report the shortage to the Sample Control Center.
6.4.2 Place the solution in a 5 mL vial and cap
immediately. Add the other three solutions
(table 1) to the vial and cap tightly.
6.4.3 The final nominal solution concentration in the
vial will be 62.5 ug/mL (250 ug/mL divided by 4)
for the gases and water soluble compounds and 12.5
ug/mL (50 ug/mL divided by 4) for the remaining
volatile compounds.
E-233
Rev: 10/28/86
-------
NOTE: If the "purgeables/volatiles G" solution
was divided by a factor of 5 per the "NOTE" under
section 6.4 above, all compounds in the vial will
be at a concentration of 12.5 ug/mL.
6.5 Semi-volatiles
6.5.1 Open one ampul at a time per the instructions in
section 5. Observe the caution in 5.3. Withdraw
the total volume of solution in a one mL syringe.
If less than 0.8 mL is present do not use the
solution, repackage it in the ampul and seal with
the Minimert valve. Report the shortage to the
Sample Control Center.
6.5.2 Place the solution in a 25 mL ground glass stop-
pered volumetric flask. Add the other solutions
(tables 2-4) to the flask. Bring to the mark with
benzene-dg, p-dioxane-ds^ or a mixture of these
two solvents. Note; it was not known at the time
of writing of these instructions if all compounds
would be soluble in methylene chloride-d2 at the
dilute (200 ug/L) level. The laboratory should
test this solubility on unlabeled compounds if use
of methylene chloride is desired.
6.5.3 Transfer the solution to a 40 mL vial with Teflon-
lined screw cap.
6.5.4 The final solution concentration will be nominal
200 ug/mL [1625C: 6.8] (5000 ug/mL divided by 25).
Spike 0.5 mL of this solution into each sample
aliquot (1625C: 10.2.1.3, 10.2.2.6, or 10.2.5.6).
E-234
Rev: 10/28/86
-------
6.6 Label the above solution and place a mark at the solvent
level.
6.7 Document the date and operations in a standards log book
7 Questions comments/problems.
7.1 Contact the Sample Control Center if difficulties arise
in the use of the labeled compound solutions or these
instructions.
8 References
8.1 Methods 1624 and 1625, Revisions C, USEPA, Industrial
Technology Division, WH-552, 401 M Street, SW,
Washington, D.C. 20460.
8.2 Methods 601-625, July 1982 Revisions, USEPA, EMSL,
Cincinnati, OH 45268, 49 FR 41234 (26 October, 1984).
8.3 "Performance Tests for the Evaluation of Computerized
Gas Chromatography/Mass Spectrometry Equipment and
Laboratories," USEPA, EMSL Cincinnati, OH 45268,
EPA-600/4-80-025 (April 1980).
E_235 Rev: 10/28/86
-------
Table 1
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E-236
-------
MW- 2946 PURGEABLES/VOLATILES-F
(50 Mg each component/I mL methanol-d/ solution)
Lot No. O-642
Packaging sub-lot 1971-1
EPA No.
4V
47V
10V
38V
15V
86V
11V
Compound
Benzene-d,
Bromof orm-^-*C
1,2-Dichloroethane-d^
Ethylbenzene-djQ
1,1, 2, 2-Tetrachloroethane-d2
Toluene-dg
J , 1,1-Trichloroethane-do
MSD No.
MD-6
MS-2313
MD-103
MD-1766
MD-1416
MD-40
«
MD-1150
Chemical
Purity %
>99.5
>99
>99
>98
>99
>99
>99
Isotoplc
Purity Atom
99.7
92.5
99.22
98.34
99.56
99.64
97.15
Concentration In solution
pg/ml
50
50
50
50
50
50
50
M
I
Footnotes: 1. lsoi»|ilc purity, atom Z U or atom % 13C, determined by NMR and/or MS, ± 0.2%
2. Actii;il concentration, confidence limit - 5%
-------
Lot
H
I
OJ
00
MW- 294 7 I'UKGK ABLKS/ VOLAT I LliS-u
(250 ug each coroponent/1 raL methanol-d^ solution)
EPA No.
516V
2V
3V
46V
514V
16V
45V
515V
88V
Compound
Acetone-d^
Acrolein-d/,
Acrylonitrile-d-j
Bromomethane-d3
2-Butanone-4,4,4-d3
Chloroethane-d^
Chiorometliane-d-j
Diethyl-djQ Ether
Vinyl-d3 Chloride *
MSD No.
MD-2
MD-2604
MD-1455
MD-23
MD-2402
MD-334 ,
MD-324
MD-267
MD-965
Chemical
Purity %
>99.5
£99
*99
>98
^99
>99
£99
>99
^99
Isotopic
Purity Atom
99.6
97.7
99.01
99.5
99.27
>99
99.55
99.1
99.75
Packaging sub-lot 1972-1
Concentration in solution
250
250
250
250
250
250
250
250
250
Footnotes: i. Jaoiopic purity, atom % 0, determined by NMR and/or MS, - 0.2Z
2. Actual concentration, confidence limit * 5%
J. Until products stabilized with hydroqulnone
H
to
-------
MW- 2948 PURGEABLES/VOLATTI.ES-H
(50 pg each component/1 UIL methanol-d^ solution)
Lot No.u~fa44
Packaging sub-lot 1964-1
M
ro
u>
vo
EPA No.
48V
51V
30V
33V
527V
85V
87V
Compound
jlromodichloromethane-l-'c
Chlorodibromomethane-l^C
1 , 2-Dichloroethy lene-1 , 2-d2
(cis/trans mixture)
1 , 3-Dichloropropene-d^
(cis/trans mixture)
p-Dioxane-dg
Tetrachloroethylene-l,2-13C2
1,1,2-Trichloroethy lene-1, 2-13C2
MSD No.
MS-2368
MS- 2 36 4
MD-2526
MD-2669
MD-426
MS- 24 11
MS-2410
Chemical
Purity %
>99
>99
*99
>99
>99
>99
/99
Isotopic
Purity Atom
*92. 57
92.33
99.57
99.27
99.03
98.94
99.28
Concentration in solution
|jg/nil
50
50
50
50
50
50
50
I
Footnotes: Isotopic purity, atom Z D or atom Z l^c, determined by NMR and/or MS - 0.2%
Actual concentration, confidence limit -^ 5%
fa
T
-------
MW-2949 ACID LXTRACTAHLES - 3
(5 mg each component/1 mL benzene-dg solution)
Lot No.0-645
Packaging sub-lot 2155-1
M
I
M
EPA No.
22A
24A
31A
34A
60A
59A
57A
58A
64A
65A
21A
53IA
Compound
4-Chloro-3-raethylphenol-2,6-d2
2-Chlorophenol-3 , 4 , 5 ,6-d^
2,4-Dlchlorophenol-3,5,6-d.j
2,4-Dimethylphenol-3,5,6-d3
4,6-Dlnitro-2-methylphenol-3,5-d2
2,4-Dinltrophenol-3,5,6-d2
2-Nitrophenol-3,4,5,6-d4
4-Nit rophenol-2, 3, 4, 5-d,
13
Pontnrhlorophenol- C^
Phenol-2,3,4.5.6-d5
2,4,6-Trlchlorophenol-3,5-d2
2,4 ,5-Trichlorophenol-3,6-d2
MSD No.
MD-2355
MD-2280
MD-2281
MD-2284
MD-2357
MD-228S
MD-2290
MD-2356
MS- 2 29 3
MD-1502
MD-2279
MD-2935
Chemical
Purity %
> 99.5
99
99.5
98
> 99.5
£ 99
99.5
99
> 99
> 98.5
> 99.5
99
Isotoplc
Purity Atom
98.2
98.5
99.0
98.2
98.7
97.9
99.0
98.7
98.4
98.8
98.2
96.7
Concentration In solution
ing /ml
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
Footnotes: 1. Isotoplc purity, atom % D or atom % 13C. determined by NMR and/or MS, - 0.2X
H
pi
T
(-
(D
Ul
2. Actual concentration, confidence limit - 5Z.
-------
MW- 2764 BASE NEUTUALS-4.1
(5 rag each component/1 mL benzene-d, solution)
Lot No. 0-635
Packaging sub-lot 1965-1
EPA No.
77B
74B
79B
73B
42B
26B
35B
39B
52B
53B
81B
Compound
Acenaphthylene-dg
Benzo(b)l Iuoranthene-dj9
Benzo(ghi)perylene-dj2
Benzo(a)pyrene-dj2
Uisi(2-cliloroisopropyl)-d|2 l'-ll|ur
1 , 3-DicliJorobenzene-d/
2,4-Dinitrotoluene-3,5,6-d3
Fluoranthene-djQ
1 3
Hexachloro-1 , 3-butadiene- C^
Hexachlorocyclopentadiene-1 ,2, 3, 4-l^C
Phenanthrene-d,0
MSD No.
MD-128
MD-2360
MD-830
MD-1956
MD-2702
MD-2405
'^
MD-2407
MD-2361
MS-2408
iMS-2710
MD-120
Chemical
Purity %
* 99
^ 98
98
* 97
^ 98
£ 99
> 99
> 98
99
>' 95
> 99.5
Isotopic
Purity Atom
99.4
99.39
98.5
99.2
99.2
98.34
98.17
99.34
98.74
96.9
98.52
Concentration in solution
nig /ml
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
. j
Footnotes: j. Isotopic purity, atom X D or atom % l^c, determined by NMR and/or MS, - 0.2%.
H
fu
T
2. Actual concentration, confidence limit - 5%.
-------
MW- 2942 BASE NEUTRALS-A.3
(5 nig ciirh rtnii|>oiu-iil/ I ntL benzcno-d sn I ui Ion)
Lot No.0-636
er,In}- .sub-lot 1966-1
M
I
M
EPA No.
41B
20B
40B
68B
70B
69B
9B
12B
54B
8B
Compound
4-Bromophenyl Phenyl-dj
2-Chloronaphthalena-dy
4-Chlorophenyl Phenyl-d5
Di-n-butyl Phthalate-3,4
Diethyl Phthalate-3,4, 5,
Dl-n-octyl Phthalate-3,4
Hexachlorobenzene-^-'Cg
llexachloroethane-l-*-'C
Isophorone-dg
1 , 2 ,4-Trichlorobenzene-3
Ether
Ether
,5,6-d4
6-dA
,5.6-d4
,5,6-d3
MSD No.
MD-2936
MD-2462
MD-2312
MD-2310
MD-2726
MD-2291
MS-2354 '
MS-2406
MD-2304
MD-2706
Chemical
Purity %
> 98
> 99
> 99
> 99
> 99
> 99
> 99
> 99
> 99.5
> 99
Isocopic
Purity Atom
96.95
98.54
97.0
98.64
99.54
98.62
98.3
92.52
99.4
98.73
Concentration in solution
mg /ml
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
H
T
(
n>
Footnotes: K laoiopic purity, atom % I) ur atom % 13C, determined by NMR and/or MS, - 0.2%.
2. Actii.il concentration, conlidence limit - 52.
-------
MU-2768 IIASIC NIiUTKALS-6. 2
(5 mg each component/1 mL bcuzcne-dg solution)
Lot No.0-639
snli-loi 2I!)4-J
EPA No.
IB
78B
75B
18B
76B
SOB
55B
SAB
Compound
Acenaphthene-d,Q
Anthracene-djQ
Benzo(k) f Iuoranthene-dj2
Bis(2-chloroethyl)-dQ Ether
o
Chryaene-d12
Fluorene-djQ
Naphthalene-dg
Pyrene-d1Q
MSD No.
MD-A2
MD-A6
MD-2362
MD-2A79
MD-A02
MD-1298
MD-26
MD-363
Chemical
Purity %
> 99.5
> 99
> 97.5
> 98
> 99.5
> 98
99.5
> 99.5
Isotopic
Purity Atom
97.97
99.13
99.53
98.17
99.05
98.98
99.52
98.9
Concentration in solution
ing /ml
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
w
I
N)
I-ootnotes: i. Isotopic purity, atom % D, determined by NMR and/or MS, - 0.2%.
2. Actual concentration, confidence limit - 5%.
fu
T
IT)
OO
-------
Table 9
GO
en
sO
i
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ea
so
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cj
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a,
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o
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o
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e
ai
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C
41
I
en
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w
hi
en
e
o
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o
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P* O 00
00 ^ft CO
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Px
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^^ C^ ^^
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/» /»
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*^ ^^ ^3
vO Q\ f^
en «N esi
s £ i
^
73
vO
(^
4) *
C
to en
£ 1
u eg
cu u
r ^
oo s a.
4) X ^s
C 3 -+
«U J= >»
U 4J X
ea cu 4)
u 0 J=
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ca j= "3
x-v U 41
ea 1 1
~s tM «M
N N^ >W
c ca ca
CU *-4 *H
a a a
a a a
4
\O
oo
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ON
ON
in
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en
e>4
i
^y
a
\
vO
m
*
^
en
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4)
u
CO
|
-H
^
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4J
i
H
a
a
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o
m
CM
en
ON
ON
m
ON
ON
ON
m
en
,
A
T3
4)
S
U
cu
4J
5J
3
*
am
5s?
£
O
±*
*y
.
>\
^j
<
w
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H
O.
3
^
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Jl
i i
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s
0
E-244
-------
HW-29A3 BASli NI£UTRALS-5.1
(5 mg each component/1 mL benzene-dg solution)
Lot No. 0-637
PackaRing sub-lot 1967-1
EPA No.
SB
528B
28B
507B
37B
503B
502 B
61 »
621)
63B
Compound
Benzidiue-dy (rlngs-dg)
Curbazole-dg.NH
3, 3'-Dichlorobenzidine-d6 (rings-d^)
Diphenyl-djQ-amine
1 , 2-Diphenyl-djQ-hydrazine
2-Methylpyridine-d7 (d-Picoline)
2-Naphthyl-dy-amine
N-Nitrosodimethyl-dft-amine
N-Nitrnsndiphcnyl-2.2l.4,4'.6,6'-d6-
uinlne
N-Nitrosodi-n-propyl-dj^-amine
MSU No.
MD-2330
MD-2700
MD-2703
MD-2704
MD-2705
MD-2320
MD-191
MD-2937
MD-2311
MD-2938
Chemical
Purity %
> 98
> 98
98
? 99
> 99
^ 99
> 98
99
98.1
99
Isotoplc
Purity Atom
99.3
99
99.3
98.4
98.0
99.0
98.0
99.6
98.6
98.8
Concentration in solution
mg/ml
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
M
01
Footnotes: 1. Isotoplc purity, atom \ D, determined by NMR and/or MS * 0.2Z
2. Actual concentration, confidence limit - 5%
(D
t
O
-------
M
4>
CT.
MW- 2769 SEMI-VOLATI1.ES- I/APPENDIX C
(5 rag each component/1 mL benzene-dg solution)
Lot No. 0-599
Packaging sub-lot 196'J-I
EPA No.
513B
517B
505B
504B
512B
508B
506B
521B
519B
510B
509 B
523B
526B
Compound
p-Cymene-d, ,
n-Decane-d22
Dibenzof uran-dg
Dibenzothiophene-dg
Diphenyl-djQ
Dlphenyl-d10 Ether
n-Dodecane-d26
n-Eicosane-dA2
n-Hexadecane-d-j^
Styrene-2,3,4,5,6-d5
o-Terpineol-d-j
n-Tetracosane-djo
MSD No.
MD-2709
MD-960
MU-2316
MD-2315
MD-208
MD-373
MD-882
MD-1532
MD-821
MD-126
MD-2707
MD-883
MD-2708
Chemical
Purity %
> 99
* 99
> 98.5
> 99
> 99.6
? 99
> 99
* 99
> 99
} 99
supplied
* 99
* 99
Isotopic
Purity Atom
99.4
99.1
99.1
99.5
99.4
99.3
98.2
98.8
98.7
> 98.4
by EPA. Was)
99.5
99.2
Concentration in solution
mg/ml
5.0
5.0
5.0
10.0*
5.0
5.0
5.0
5.0
5.0
5.0
Ington DC.* 0.0
5.0
5.0
Footnotes: Isotopic purity, atom % D, determined by NMR and/or MS
Actual concentration, confidence limit * 5%
0.2%
* Material supplied to MSD by EPA labelled as "a-Terpineol-dj" turned out to be
(telecon with Dale Ruslmeck, December 20, 1984)
H
T
I-1
(D
-------
ATTACHMENT 9
E-247
-------
QUANTITATION REPORTS ON MAGNETIC TAPE
NOTE: Quantitation report types have been simplified. Please see section 3.1.3 on
the sample line for further information.
E-248 10/28/86
-------
Quantitation Reports on Magnetic Tape
1. Tape Characteristics
a. Tape - 9 Track; 800/1600 BPI; 600, 1200, or 2400 foot reels
b. Code - ASCII
c. Labels - no internal labels
d. Blocksize - 800 decimal words/block or bytes/block
2. File Characteristics
a. Each quantitation report represents a file on the submitted tape. A tape
will contain multiple files. Each of these files must end with an end of file
(tape mark).
b. Each line of the quantitation report constitutes a record. Records/lines
can be variable in length from one to 80 characters. Each record/line must
end with a carriage return (Octal 15 or Hexidecimal OD). A blank line is
interpreted as two consecutive carriage returns. A form feed character
(Octal 1* or Hexidecimal OC) must be used after the last record in the file
to signify the end of all records.
c. Records/lines must be combined into fixed length blocks of 800 bytes in
length. Blocks should not include any prefixes or postfixes. Records may
span blocks. A file will consist of multiple blocks. Blocks are separated on
the tape by inter-record gaps.
E-249 10/28/86
-------
3. Data Format
The quantitation report is divided into four basic sections for information
reporting. The sections in the order in which they appear within the quantitation
report are cailed:
o Header Section
o Compound List Section
o Technical Data Section
o Reference Data Section
Each of these sections must be present in each quantitation report submitted on
tape. The absence of any one of these sections from a quantitation report is cause for
the non acceptance of the quantitation report. Tables 1A, IB and 1C provide examples
of quantitation reports for volatiles, semi-volatiles and dioxins, respectively. These
tables are examples only, and are not meant to show the exact format in which data
are to be submitted.
3.1 Header Section
The header section provides descriptive information about the analysis and
the conditions under which it was performed. This section consists of three
mandatory lines of descriptive information and one optional line. The four lines
and the reporting requirements for each are identified as follows.
Line Identification Reporting Requirement
Title Line Mandatory
Date/Time Analyzed Line Mandatory
Sample Line Mandatory
Condition Line Optional
E-250 10/28/86
-------
Although the mandatory lines of information must be present in each
header section, there is no actual limit as to the total number of lines that may
be present. Laboratories are permitted to use this section to record any
additional information deemed necessary to properly identify the analysis. The
mandatory and optional lines however must appear in the order specified above,
but additional lines may be interspersed between them. The complete
specifications for each of these four lines is provided in subsequent paragraphs.
Examples of the Sample and Condition Lines in the Header Section for methods
162^C, 1625C and 613 are given at the end of each respective section.
3.1.1 Title Lines
This must be the first line within the header section and as such
represents the first line of each quantitation report submitted. Only one
title line is permitted within the Header Section. The line must contain
the value QUANTITATION REPORT starting in position one (left most
position) of the line. Other information may appear after this value on the
line but must be separated from the value by at least one space (blank).
3.1.2 Date/Time Analyzed Line
This line must contain the date and time that the analysis was
performed. This line must preceed any other date lines within the header
section. The format of this line is as follows:
Line Position Data Element Format
1-8 Date Analyzed MM/DD/YY
MM = month; 01-12
DD = day; 01-31
YY = year; 83-99
9 Field Delimiter Space
10-17 Time Analyzed HH:MM:SS
HH = hour; 00-24
MM = minute; 00-59
SS = second; 01-59
E-251 10/28/86
-------
3.1.3 Sample Line
The Sample line contains the following data elements. Data elements
are recorded on the line in the order specified. Data elements are separate
from each other by means of a comma (,). The end of the data element list
is signified by a dollar sign ($). The specifications for the sample line are:
10/28/36
E-252
-------
Line Position
Data Element
Format
1 - 7
8
9
Literal Value
Field Delimiter
Instrument
Field Delimiter
Shift
Field Delimiter
Quan Report Type
Field Delimiter
Sample Number
Field Delimiter
Bottle Number
Field Delimiter
Fraction
SAMPLE:
Space
2 positions; alphanumeric
Comma (,)
1 position; alpha
Code Meaning
G Graveyard
D Day
S Swing
Comma (,)
3 positions; alphanumeric
Code Meaning
CAL Calibration
VER Calibration
Verification for extraction
methods only
EPA EPA Sample
BLK Laboratory Blank
FBK Field Blank
IPR -Initial Precision and Accuracy
OPR Ongoing Precision and
Accuracy
Comma (,)
5 positions; alphanumeric
Comma (,)
2 positions; numeric
For EPA Samples -
Range: 01-98
Analysis of TCLP
Leachate: 99
All others: 00
Comma (,)
I position; alphanumeric
Code Meaning
A Acid
B Base
C Combined acid base/
neutral
D Dioxin
P Pesticide
V Volatile
All quantitation files for calibration, precision and recovery, standards and
blanks will be tracked by this instrument number within a given laboratory.
Changing of this instrument number by the laboratory would necessitate the
submittal of new calibration and initial precision and recovery quantitation
reports by the laboratory.
For volatiles, calibration verification and ongoing precision and recovery tests
are performed with the OPR report.
E-253
10/28/86
-------
Line Position Data Element Format
Field Delimiter Comma (,)
Cone/Dilution Factor 11 positions maximum;
numeric with colon (:)
separating initial and final
sample volume
NA:NA - used for calibration
standards and other runs
that are not extracted
Field Delimiter Comma (,)
Date Extracted MM/DD/YY - X; 10 positions
MM - month; 01-12
DD-day; 01-31
YY - year; 83-99
X - shift; G (graveyard)
D (day), S (swing)
NA - used for calibration
standards and other runs
that are not extracted
Dollar Sign ($) End of data delimiter
Examples - example Sample Lines in headers for volatiles are given
below, the examples are ordered to simulate initial and on-going use of the
methods. The actual data used in these examples represent synthetic
values and cannot be used for data submission. Numbers in brackets ( )
reference paragraph numbers in the methods.
3.1.3.1 Volatile Examples
a. Initial calibration (1624C: 6.7.1, 7.4, 7.5, and 7.6).
(1) For a 10 ug/L initial calibration
SAMPLE: A1,D,CAL,00010,00,V,NA:NA,NA$
(2) For a 20 ug/L initial calibration
SAMPLE: A1,D,CAL,00020,00,V,NA:NA,NA$
(3) For a 50 ug/L initial calibration
SAMPLE: Ai,D,CAL,00050,00,V,NA:NA,NA$
(4) For a 100 ug/L initial calibration
SAMPLE: A1,D,CAL,00100,00,V,NA:NA,NA$
(5) For a 200 ug/L initial calibration
SAMPLE: A1,D,CAL,00200,00,V,NA:NA,NA$
b. Initial precision (1624C: 6.7.2, 8.2).
(1) SAMPLE: A1,D,IPR,00020,00,V,NA:NA,NA$
(2) SAMPLE: Ai,D,IPR,00020,00,V,NA:NA,NA$
E-254 10/28/86
-------
(3) SAMPLE: A1,D,IPR,00020,00,V,NA:NA,NA$
(4) SAMPLE: A1,D,IPR,00020,00,V,NA:NA,NA$
c. Calibration verification (1624C: 6.7.2, 11.5) and on-
going precision.
SAMPLE: A1,S,OPR,00020,00,V,NA:NA,NA$
d. Laboratory Blank (1624C: 8.5)
SAMPLE: Al,S,BLK,00000,00,V,l:l,NA$
e. Analysis of samples (typical).
SAMPLE: A1,S,EPA,NNNNN,NN,V,1:1,NA$
SAMPLE: Al,S,EPA,NNNNN,NN,V,i:10,NA$ (is
one in 10 dilution of sample above).
f. Analysis of Field Blanks.
(1) With EPA Sample Number
SAMPLE: A1,S,FBK,NNNNN,NN,V,1:1,NA$
(2) Laboratory Composite
SAMPLE: A1,S,FBK,NNNNN,NN,V,1:1,NA$
(where NNNNN represents the 1st sample number
of a set for a given day)
3.1.3.2 Semi-volatile Examples
a. Initial calibration (1625C: 6.13, 7.4, 7.5 and 7.6)
(1) For 10 ug/ml initial calibration
SAMPLE: A2,D,CAL,00010,00,C,NA:NA,NA$
(2) For a 20 ug/ml initial calibration
SAMPLE: A2,D,CAL,00020,00,C,NA:NA,NA$
(3) For a 50 ug/ml initial calibrattion
SAMPLE: A2,D,CAL,00050,00,C,NA:NA,NA$
(4) For a 100 ug/ml initial calibration
SAMPLE: A2,D,CAL,00100,00,C,NA:NA,NA$
(5) For a 200 ug/ml initial calibration
SAMPLE: A2,D,CAL,00200,00,C,NA:NA,NA$
E-255 10/23/36
-------
b. Initial precision and accuracy (1625C: 8.2).
(1) SAMPLE: A2,D,IPR,00100,00,C, 1000:1,MM/DD/YY-G$
(2) SAMPLE: A2,D,IPR,00100,00,C, 1000:1,MM/DD/YY-G$
(3) SAMPLE: A2,D,IPR,00100,00,C,1000:1,MM/DD/YY-G$
(4) SAMPLE:
A2,D,IPR,00100,00,C,1000:0.95,MM/DD/YY-G$
c. Calibration verification (1625C: 12.5).
SAMPLE: A2,S,VER,00100,00,C,NA:NA,NA$
d. On-going precision and accuracy (1625C: 12.7).
SAMPLE: A2,S,OPR,00100,00,C,1000:1,MM/DD/YY-D$
e. Laboratory Blank (1625C: 8.5)
SAMPLE: A2,S,BLK,00000,00,C,1000:1,MM/DD/YY-D$
f. Field Blank
SAMPLE: A2,S,FBK,NNNNN,NN,C,1000:1,MM/DD/YY-D$
g. Analysis of samples.
(1) SAMPLE:
A2,S,EPA,NNNNN,NN,B, 1000:1, MM/DD/YY-D$
(2) SAMPLE:
A2,S,EPA,NNNNN,NN,A,1000:1,MM/DD/YY-D$
(3) SAMPLE:
A2,S,EPA,NNNNN,NN,A,10:1,MM/DD/YY-D$
(employs the dilute aliquot (1625C: 10.1 and 14.4)
for analysis).
E-256 10/28/86
-------
(4) SAMPLE:
A2,S,EPA,NNNNN,NN,B,1000:10,MM/DD/YY-D$
(employs dilution of the extract (1625C: U.4) for
analysis).
g. Analysis of Field Blanks.
SAMPLE: A2,S,FBK,NNNNN,NN,C,1000:1,MM/DD/YY-D$
3.1.3.3 Dioxin Examples* (Methods 613 and 613 extended to 10 liter
samples)
a. Initial Calibration (613: section 7)
(1) . For 200 ng/mi (200 pg/ul, 0.2 ng/uJ)
SAMPLE: A2,D,CAL,00200,0,D,NA:NA,NA$
(2) For 1000 ng/mi
SAMPLE: A2,D,CAL,01000,00,D,NA:NA,NA$
(3) For 5000 ng/ml
SAMPLE: A2,D,CAL,05000,00,D,NA:NA,NA$
(H) For 20000 ng/ml
SAMPLE: A2,D,CAL,20000,00,D,NA:NA,NA$
(5) For 40000 ng/ml
SAMPLE: A2,D,CAL,40000,00,D,NA:NA,NA$
* Note: Requirements may vary between contracts. Unless specified otherwise in
the contract, the compound concentrations given in these examples are to be
used.
E-257 10/2S/S6
-------
b. Initial precision and accuracy
(1) For Method 613 (613: 8.2)
(a) SAMPLE:
A2,D,PAR,01000,00,D,1000:0.05,MM/DD/YY-G$
(2) For Method 613 extended to 10 liter samples
(a) SAMPLE:
A2,D,PAR,01000,00,D,10000:0.05,MM/DD/YY-G$
c. Calibration Verification (613: 7.1.3)
SAMPLE: A2,D,VER,01000,00,D,NA:NA,NA$
d. Ongoing Precision and Accuracy
(1) Method 613 (613: Replaces 8.*)
(a) SAMPLE:
A2,D,PAR,01000,00,D,1000:0.05,MM/DD/YY-G$
(2) Method 613 Extended to 10 liter samples
(a) SAMPLE:
A2,D,PAR,01000,00,D,10000:0.05,MM/DD/YY-G$
e. Laboratory Blank
(1) Method 613 (613: 8.5)
(a) SAMPLE:
A2,D,BLK,00000,00,D,1000:0.05,MM/DD/YY-G$
(2) Method 613 Extended to 10 liter samples (613E: 4.3)
(a) SAMPLE:
A2,D,BLK,01000,00,D,10000:0.05,MM/DD/YY-G$
f. Analysis of Samples
(1) SAMPLE:
A2,G,EPA,NNNNN,NN,D,1000:0.05,MM/DD/YY-G$
(2) SAMPLE:
A2,G,EPA,NNNNN,NN,D,10000:0.05,MM/DD/YY-G$
(for 10 liter sample)
E_258 10/28/86
-------
3.1.4 Condition Line
The Condition line contains the following data elements. As with the
sample line, data elements are recorded on the line in the order indicated.
Data elements are separated from each other by means of a comma (,).
The end of the data element list is signified by a dollar sign ($). The
specifications for this type of line are:
Line Position
Data Element
Format
1 -7
3
9
Literal Value
Field Delimiter
Method
Field Delimiter
Column Length
Field Delimiter
Column Inside Diameter
Field Delimiter
Column Initial
Temperature
Field Delimiter
CONDS.:
Space
5 positions; alphanumeric
1624C or 1625C, 613 or 613A, 713
Comma (,)
6 positions; alphanumeric
expressed in meters Le.
2.5 M or 35 M;
Volatile Range 2.8-3.1 M
Semi Volatile Range 25-35 M
Dioxin Range 25-65 M
Comma (,)
6 positions; alphanumeric
expressed in millimeters
ie. 2 mm or .3 mm;
Volatile Range: 1-3 mm
Semi Volatile Range:
0.2 - 0.35 mm
Dioxin Range 0.2-0.35 mm
Comma (,)
7 positions; numeric
an at sign ((3) is
used to separate
Hold and Temperature
ie Hold (§ Temp
Volatile Hold Range: 2-4 min
Semi Vol Hold Range: 4-6 min
Dioxin Hold Range: 0-10 min
Volatile Temp Range:
Semi Vol Temp Range:
Dioxin Temp Range: 50-200°C
Comma (,)
25-50°C
25-35°C
E-259
10/23/36
-------
Line Position
Data Element
Format
Column Temperature
Program
Field Delimiter
Column Final
Temperature
Field Delimiter
Carrier Gas Flow Rate
End of Data Delimiter
10 positions; numeric
with a dash (-) separating
initial and final
temperatures and with
an at sign ((§) separating
temperature program rate
ie. 45-250 @ 8
Comma (,)
7 positions; numeric with
an at sign ((§) separating
hold and temperature ie.
Hold @ Temp
Volatile Hold Range: 0-20 min
Semi Vol Hold Range: 10-20 min
Dioxin Hold Range: 10-30 min
Volatile Temp Range: 200-250°C
Semi Vol Temp Range: 240-290°C
Dioxin Temp Range: 200-300°C
Comma (,)
9 positions; alphanumeric
Format: 30ML/M or
30 CM/S;
Volatile range: 20-40 ml/min
Semi Volatile range: 20-60 cm/sec
Dioxin Range: 20-60 cm/sec
Dollar sign ($)
3.1.4.1 Volatile Example
CONDS.: 1624C,3.0M,2MM,3@45,45-250@8,1@250,20ML/M$
3.1.4.2 Semi-Volatile Example
CONDS.: 1625C,30M,0.25MM,5@30,30-2SO@8,15
-------
3.2 Compound List Section
The compound list section is the second basic section of information
appearing on the quantitation report. It identifies the actual compounds that
were determined during analysis. This section is made up of two types of lines:
o Title Line
o Compound Identification Line
3.2.1 Title Line
The title line must appear first within the Compound List Section.
Only one title line may be present in the section. This line is formatted as
follows:
Line Position Data Element Format
1 Field Delimiter Space
2-3 Literal Value NO
Field Delimiter
Spaces (At Least 2)
Literal Value NAME
E-261 10/28/36
-------
3.2.2 Compound Identification Line
A compound identification line is included in this section for each
compound that was determined during analysis. Compound lines should be
shown in the order in which they were determined. Each compound
identification line is made up of three data elements specified in the
following order within the line:
o Compound Order Number
o EGD Compound Number
o Com pound Name
The compound order number is a numerical code that establishes the
order of compound determination by the GC/MS. The code is used on the
Quantitation Report to match up compound identification with compound
analysis and reference data appearing in subsequent sections of the report.
On each quantitation report this number always starts with 1. The number
I is always assigned to the first compound that is determined, the number 2
to the second compound that is determined and so on.
Table 4 contains a list of valid compound names and EGO compound
numbers.
Each compound identification line will appear in the following
format:
Line Position
1-3
Data Element
Compound Order
Number
Field Delimiter
EGD Compound
Number
Format
1 to 3 character number;
right justified in field;
range 1-250
Spaces (At Least 2)
3 positions; numeric
Range Meaning
001-129 Quantitated by internal
standard
130-199 Misc., internal standard
and surrogate compound
201-299 Labeled Compound (isotope)
Quantitated by internal
standard
E-262
10/23/86
-------
Line Position Data Element Format
Range Meaning
301-399 Quantitated by
isotope dilution
Wl-*29 Labeled compound (isotope)
quantitated by internal
standard.
501-599 Non-priority
Pollutant Compounds
quantitated by internal
standard
601-699 Synfuel specific and
Appendix C labeled com-
pounds (isotopes) quan-
titated by internal
standard
701-799 Synfuel specific and
Appendix C compounds
quantitated by isotope
dilution.
800-829 Pollutants 100-129
quantitated by isotope
dilution.
900-999 Non-priority
Pollutant Compounds
quantitated by internal
standard
Field Delimiter Spaces (At Least 2)
Compound Name 70 positions; alphanumeric
E~263 10/28/86
-------
3.3 Technical Data Section
The technical data section provides measurement data for each compound
that is determined. It is the third section within the quantitation report. This
section is made up of two types of lines:
o Title Line
o Compound Technical Data Line
3.3.1 Title Line
The title line must appear first within the Technical Data Section.
Only one title line may be present in the section. This line is formatted as
follows:
Line Position
Data Element
Format
1
2-3
First non-blank
character at or past
position 41.
Field Delimiter
Literal Value
Field Delimiter
Literal Value
Field Delimiter
Literal Value
Field Delimiter
Literal Value
Field Delimiter
Literal Value
Field Delimiter
Literal Value
Free Area
Literal Value
Field Delimiter
Literal Value
Free Area
Space
NO
Spaces (At Least 2)
M/E
Spaces (At Least 2)
SCAN
Spaces (At Least 2)
TIME
Spaces (At Least 2)
REF
Spaces (At Least 2)
RRT
Spaces or other
literal values
AREA
Spaces (At Least 2)
AMOUNT
Spaces or other
literal values
E-264
10/23/86
-------
3.3.2 Compound Technical Data Line
A compound technical data line is included in this section for each
compound that is determined. Compound technical data lines are ordered
the same as the compound identification lines in the compound list section.
The compound order number is used for this purpose and serves to connect
compound identification with the technical data. The compound technical
data line at a minimum must contain the following data elements.
o Compound Order Number
o Mass to Charge Ratio
o Scan Number
o Retention Time
o Reference Compound
o Relative Retention Time
o Peak Area
o Amount
o Unit of Measure
The specific format for this line is as follows:
Line Position Data Element Format
1-3 Compound Order 3 positions; numeric; right-
Numberjustified; Range l-
250
Field Delimiter Spaces (At Least 1)
Mass to Charge Ratio * positions; numeric;
(M/Z) Volatile range: 20-250;
Semi Volatile range: 35-450
Dioxin (Selected Ion Monitoring):
257, 320, 322, 323, 32S, 332,
and 33*.
Field Delimiter Spaces (At Least I)
Scan Number 5 positions; numeric;
range 1-9999
Field Delimiter Spaces (At Least 1)
Retention Time 6 positions; numeric
with colon; format;
MM:SS
Field Delimiter Spaces (At Least 1)
Reference Compound 3 positions; numeric;
range 1-250
E-265 10/28/36
-------
Line Position
Data Element
Format
First non-blank
character at or
past position
Field Delimiter
Relative Retention Time
Field Delimiter
Open Field
Peak Area
Field Delimiter
Amount
Field Delimiter
Unit of Measure
Field Delimiter
Open Area
Spaces (At Least 1)
5 positions; numeric
with decimal point and
3 decimal places
Spaces (At Least 1)
Spaces or other
field value
10 positions; numeric
Spaces (At Least 1)
10 positions; numeric
with decimal point
and 3 decimal
places
Spaces (At Least 1)
5 positions; alphanumeric
Valid codes: uG/L, uG/ml, or ng/mi
Spaces (At Least 1)
Spaces or other
field values.
E-266
10/23/86
-------
3.* Reference Data Section
The reference data section is the fourth section that must appear on each
Quantitation Report. It provides reference and library data about the analysis
that was performed. It is made up of two types of lines:
o Title Line
o Compound Reference Data Line
3.*.1 Title Line
The title line must appear first within this section. Only one title
line is permitted within the section. Subsequent title lines will be deleted
if present. The line is formatted as follows:
Line Position
Data Element
Format
1
2-3
First non-blank
character at or past
position 19.
First non-blank
character at or
past position *3
Field Delimiter
Literal Value
Field Delimiter
Literal Value
Field Delimiter
Open Area
Literal Value
Field Delimiter
Open Area
Literal Value
Field Delimiter
Literal Value
Field Delimiter
Literal Value
Open Area
Space
NO
Spaces (At Least 2)
RET (L)
Spaces (At Least 1)
Spaces or other
literal values
Spaces (At Least 1)
RRT (L)
Spaces (At Least 1)
Spaces or other
literal values
AMNT (L)
Spaces (At Least 1)
R.FAC
Spaces (At Least 1)
R.FAC (L)
Spaces or other
literal values
E-267
. 10/28/86
-------
3.4.2 Compound Reference Data Line
A compound reference data line is included in this section for each
compound that is determined. These lines are ordered the same as the
compound identification lines in the compound list section. The compound
order number is used for this purpose and serves to connect the compound
identification with the reference data. This means that there is a one to
one correspondence between the compound identification lines and the
reference data lines. The reference data line at a minimum must contain
the following data elements.
o Compound Order Number
o Library Retention Time
o Library Relative Retention Time
o Library Amount
o Response Factor
o Library Response Factor
The specific format for this line is as follows:
Line Position
Data Element
Format
1-3
First non-blank
character starting
at or past
position 18.
Compound Order
Number
Field Delimiter
Library Retention Time
Field Delimiter
Open Area
Library Relative Retention
Time
3 positions; numeric;
Range 1-250
Spaces (At Least 2)
6 positions; numeric
with colon; format -
MM:SS
Spaces (At Least 1)
Spaces or other
data values
5 positions
E-268
10/28/86
-------
Line Position
Data Element
Format
First non-blank
character starting
at or past
position 41.
Field Delimiter
Open
Library Amount
Field Delimiter
Response Factor
Field Delimiter
Library Response Factor
Field Delimiter
Open Area
3.5 Associated Quantitation Reports
Spaces (At Least 1)
Spaces or other
data values
9 positions; numeric
with decimal
point and 2 decimal
places
Spaces (At Least 1)
7 positions; numeric
with decimal point
and 3 decimal
places
Spaces (At Least 1)
7 positions; numeric
with decimal point
and 3 decimal
places.
Space.s (At Least 1)
Spaces or other
data values.
Some GCMS data .systems will not permit all data from an analysis to be
given in a single quantitation report when the number of compounds analyzed
exceeds a certain limit (cases reported to date are 80, 110, 125 entries).
Because the semi-volatiles1 analysis requires data for more than 125 entries, only
the semi-volatiles1 quantitation report may be divided-into more than one report.
These multiple quantitation reports are called "Associated quantitation reports."
In these reports, the header shall be identical, except that a different name may
appear after the word "FILE" (see, e.g., the associated quantitation reports given
by example in Table IB). If associated quantitation reports are submitted, data
for all compounds except the 2,2'-difluorobiphenyl internal standard shall appear
only once in the totality of the associated quantitation reports. The data for the
2,2'-difluorobiphenyl internal standard shall be identical on each of the associ-
ated quantitation reports, except for the data in the "%TOT" column. No more
than three associated quantitation reports are permitted for any analysis.
E-269
10/2S/86
-------
3.6 Non-alphanumeric Characters
Sections 3.1 through 3.4 define the character type (alphabetical or num-
eric) permitted in each field on the quantitation report. Other characters are
prohibited. Specifically, the minus sign (-) and the asterisk (*) are not permitted
in any field in the Technical Data Section (Section 3.3) or any Reference Data
Section (Section 3.4). Negative numbers are prohibited because they have no
meaning in quantitation or retention time; asterisks are prohibited because they
indicate an overflow condition in most FORTRAN language systems, and are
usually the result of an attempt to divide by zero. If the amount for a given
compound is negative, and the amount is to be interpreted as "not found," the
quantitation report shall conform to the "Reporting of Compounds Not Found" in
Section *.b. If an overflow condition exists, and is the result of an attempt to
divide by zero, an alternate means of reporting shall be used which provides an
accurate estimate of the amount for the compound.
E.270
-------
*. Reporting of Quantitatlon Data
a. Unit of Work
Each tape submitted must be a complete unit of work, processable within
itself.
1) Each tape submitted must begin with either a calibration (CAL) or
calibration verification (OPR for volatiies, VER for semi-voiatiles)
run.
2) All quantitation reports from a single shift must be reported on the
same tape.
3) All associated calibration (CAL) runs and initial precision and recov-
ery (IPR) runs must be on the same tape.
4) The number of quantitation reports contained on a single tape must
not exceed 300.
b. Reporting of Compounds Not Found
Compounds not appearing within a quantitation report (e.g. all data lines
for a compound have been deleted from the report) are assumed to be not
found. If a not found compound is reported within the body of the
quantitation report the following specifications are to be followed for
reporting of these compounds.
1) The Compound Identification Line must be complete.
2) The Compound Technical Data Line must be reported in one of the
following formats:
E-271 10/28/86
-------
a) Compound order number, 1-3 spaces, and the literal value 'NOT
FOUND'. All other data elements in the line must be blank or
space filled on the data line.
b) Compound Order Number, the Mass to Charge Ratio dM/Z) and
the Reference Compound. Ail other data elements must be
blank or space filled on the data line.
3) The Compound Reference Data Line must contain, at a minimum,
only the Compound Order Number.
c. Alternate Reporting for Problem Compounds
If an interference or other problem precludes automated quantitation
by the GCMS software, Report Form I (attached as Table 3) shall be used
and shall supercede data on magnetic tape, the "note" column on this form
shall be used to reference a comment which describes the inteference or
problem, and Report Form I shall be submitted with data for the sample to
which it applies.
E-272 10/28/86
-------
5. Packaging and Shipping Instructions
Packaging Requirements:
Each tape reel shall bear a tape label containing the laboratory tape
ID, the laboratory name, the tape density, the block size, and the
number of files.
Each tape package shall contain in addition to the tape reel(s) at
least one Quantitation Report Magnetic Tape Transmittal Form for
each tape reel (see Table 2 for a sample transmittal form and
transmittal form description), ail Lab Chronicle Reports associated
with the reported samples, and BFB or DFTPP spectra analysis
required per shift per machine.
Tape reels with their associated transmittal forms and chronicle
reports shall be packaged in such a way to ensure their safety and
integrity. The outside of ail packages should be marked with a 'DO
NOT X-RAY' label. It will be the laboratory's responsibility to
replace any tape, quantitation report data, and accompanying docu-
ments damaged during shipping to the Sample Control Center.
E-273 10/28/36
-------
Shipping Requirements:
Tape packages shall be shipped either by the U.S. Postal Service or by any
carrier with direct delivery.
Shipping address by U.S. Postal Service:
Industrial Technology Division
Sample Control Center
P.O. Box U07
Alexandria, VA 22313
Shipping address by other carriers:
Industrial Technology Division
Sample Control Center
Suite 200
300 N. Lee St.
Alexandria, VA 2231*
E-274 10/28/86
-------
TABLE lA EXAMPLE OF VOLATILES QUANTITATION REPORT
QUANTITATION REPORT FILE: 7VMIX200
DATA: TVMIXZOO.TI
07/07/86 22:24:00
SAMPLE: SI, S,CAL,00200,00,V,NA:NA,NA$
CONDS.: 1624B,
AMOUNT=AREA * REF.AMNT/CREF.AREA)* RESP.FACT)
RESP. FAC. FROM AVERAGE OF WHOLE .RL
NO NAME
1 181 IS**BROMOCHLOROMETHANE**
2 245 (D3) 45V METHYL CHLORIDE
3 345 45V METHYL CHLORIDE
4 246 (D3J46V METHYL BROMIDE
5 346 46V METHYL BROMIDE
6 288 (D3)88V VINYL CHLORIDE
7 388 88V VINYL CHLORIDE
8 216 (D5) 16V CHLOROETHANE
9 316 16V CHLOROETHANE
10 244 (D2) 44V METHYLENE CHLORIDE
11 344 44V METHYLENE CHLORIDE
12 616 (06) ACETONE
13 516 ACETONE
14 202 (D2)2V ACROLEIN
15 002 ACROLEIN
16 203 (D3)3V ACRYLONITRILE
17 303 3V ACRYLONITRILE
18 229 (D2)29V 1,1-DICHLOROETHYLENE
19 329 29V 1,1-DICHLOROETHYLENE
20 213 (D3)1,1-DICHLOROETHANE
21 313 13V 1,1-DICHLOROETHANE
22 230 (D2)TRANS-1,2-DICHLOROETHYLENE
23 330 TRANS-1.2-DICHLOROETHYLENE
24 615 (010) DIETHYL ETHER
25 715 DIETHYL ETHER
26 223 (C13) 23V CHLOROFORM
27 323 23V CHLOROFORM
28 210 (D4)1,2-DICHLOROETHANE
29 310 10V 1,2-DICHLOROETHANE
30 614 (D3> MEK
31 514 METHYL ETHYL KETONE
32 211 (D3H1V 1,1,1-TRICHLOROETHANE
33 311 11V 1,1,1-TRICHLOROETHANE
34 627 (D8) 1,4-DIOXANE
35 527 1,4-DIOXANE
36 182 IS **«2-BROMO-l-CHLOROPROPANE»**
37 206 (130CARBONTETRACHLORIDE
38 306 6V CARBONTETRACHLORIDE
39 248 (13048V DICHLOROBROMOMETHANE
40 348 48V DICHLOROBROMOMETHANE
41 232 (D6)32V 1,2-DICHLOROPROPANE
42 332 32V 1,2-DICHLOROPROPANE
43 233 (D4)33V TRANS 1,3-DICHLOROPROPYLENE
44 333 33V TRANS-1,3-DICHLOROPROPYLENE
45 287 (13C2J87V TRICHLOROETHYLENE
46 387 87V TRICHLOROETHYLENE
47 204 (D6)4V BENZENE
48 304 4V BENZENE
49 251 (13051V CHLORODIBROMOMETHANE E-275
-------
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
NO
1
2
3
4
5.
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
351
214
314
019
247
047
183
215
315
285
085
286
386
207
307
238
338
185
M/E
128
53
50
99
96
65
62
71
64
88
84
NOT
58
NOT
56
56
53
65
61
66
63
65
61
84
74
86
85
67
62
NOT
72
102
97
NOT
88
77
48
47
86
83
67
TABLE lA EXAMPLE OF VOLATILES QUANTITATION REPORT
51V CHLORODIBROHOMETHANE
(13C2)14V 1,1,2-TRICHLOROETHANE
14V 1,1,2-TRICHLOROETHANE
19V 2-CHLOROETHYL VINYL ETHER
(13C) 47V BROMOFORM
47V BROMOFORM
IS *«*1,4-DICHLOROBUTANE***
(D2) 15V 1,1,2,2-TETRACHLOROETHANE
15V 1,1,2,2-TETRACHLOROETHANE
(13C2) 85V TETRACHLOROETHYLENE
85V TETRACHLOROETHYLENE
(05) TOLUENE
86V TOLUENE
(D5) 7V CHLOROBENZENE
7V CHLOROBENZENE
(010) 38V ETHYLBENZENE
38V ETHYLBENZENE
BFB BROMOFLUOROBENZENE
SCAN
251
60
60
93
94
115
117
140
143
184
185
FOUND
204
FOUND
205
212
216
248
249
272
273
289
291
296
301
296
296
313
315
FOUND
317
344
345
FOUND
343
456
356
355
359
359
393
TIME
12:46
3:03
3:03
4:44
4:47
5:51
5:57
7:07
7:16
9:21
9:24
10:22
10:25
10s47
10:59
12:36
12:39
13?50
13:53
14:41
14:48
15:03
15:18
15:03
15:03
15:55
16:01
16:07
17:29
17:32
17:26
23:11
18:06
18:03
18:15
18:15
19:59
REF
1
1
2
1
4
1
6
1
8
1
10
1
1
1
16
1
18
1
20
1
22
1
24
1
26
1
28
1
1
32
1
36
36
37
36
39
36
RRT
1.000
0.239
1.000
0.371
1.011
0.458
1.017
0.558
1.021
0.733
1.005
0.813
0.817
0.845
1.019
0.988
1.004
1.084
1.004
1.151
1.007
1.179
1.017
1.179
1.000
1.247
1.006
1.263
1.371
1.003
1.367
1.000
0.781
0.997
0.787
1.000
0.862
METH
A BB
A7BB
RXRY
A BB
RXRY
A BB
RXRY
A BB
A BB
A?BB
RXRY
QEDT
QEDT
QEDT
RXRY
A BB
RXRY
A BB
RXRY
QEDT
RXRY
A BB
RXRY
A BB
RXRY
A BB
RXRY
A BB
A BB
RXRY
A BB
A?BB
QEDT
RXRY
A BB
RXRY
A BB
AREA(HGHT) AMOUNT
45612.
161108.
1797960.
102000.
1441280.
200409.
2102360.
37562.
1057170.
178840.
2904630.
257295.
472521.
106044.
962244.
41974.
1194350.
170999.
1828310.
50772.
974562.
272891.
3928690.
112008.
1191490.
39392.
957344.
339211.
85173.
1276290.
23247.
163747.
28437.
255185.
123738.
1505850.
lassso.
20.
19.
200.
21.
199.
21.
203.
23.
201.
32.
203o
944.
1007.
37.
453.
20.
203.
21.
205.
22.
187.
24.
982.
23.
203.
20.
201.
1010.
20.
206.
1278.
20.
29.
182.
25.
167.
20.
000
253
559
427
944
743
499
147
312
976
212
069
150
106
130
878
878
431
744
747
085
933
383
337
036
254
271
870
481
138
140
000
538
656
016
841
708
U6/L
U6/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
XTOT
0. 17
0.17
1.72
. 0.18
1.71
0.19
1.74
0.20
1.73
0.28
1.74
8.09
3.63
0.32
3. 88
0.13
1.75
0.18
1.76
0.19
1.60
0.21
8.42
0.20
1.74
0.17
1.72
8.66
0.18
1.77
10.95
0.17
0.25
1.57
0.21
1 .44
0.18
E-276
-------
TABLE 1A
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
NO
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
13
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
63
79
75
136
95
84
78
130
129
84
83
106
176
173
55
84
83
172
164
97
92
117
112
116
106
396 20
396 20
399 20
412 20
412 20
426 21
429 21
419 21
420 21
426 21
425 21
453 23
479 24
479 24
544 27
530 26
531 27
537 27
537 27
570 28
573 29
597 30
600 30
652 33
659 33
:08 41
:08 36
:17 43
:57 36
:57 45
:39 36
:48 47
:18 36
:21 49
:39 36
:36 51
:02 36
21 36
:21 36
:39 56
:56 56
:00 57
:18 56
US 56
:58 56
:08 61
:21 56
:30 63
:09 56
:30 65
EXAMPLE OF VOLATILES QUANTI
1.008
0.868
1.008
0.904
1.000
0.934
1.007
0.919
1.002
0.934
0.998
0.993
1.050
1.050
1.000
0.974
1.002
0.987
0.987
1.048
1.005
1.097
1.005
1.199
1.011
RXRY
A?BB
RXRY
A BB
RXRY
A BB
RXRY
A?VB
RXRY
A BB
RXRY
A BB
A BB
A BB
A?BB
A?BB
RXRY
A BB
A BB
A BB
RXRY
A?BB
RXRY
A BB
RXRY
1068560.
111843.
2832010.
63685.
1997970.
385811.
2979110.
109992.
686162.
385811.
730003.
139858.
5954.
124971.
119766.
95140.
976982.
18666.
831510.
172719.
1806000.
191790.
2106290.
93772.
843200.
TATION REPORT
210.
28.
193.
30.
193.
21.
192.
26.
161.
21.
190.
212.
42.
299.
20.
21.
213.
30.
220.
20.
202.
20.
203.
19.
205.
283
327
967
408
946
912
241
522
048
912
113
542
778
567
000
419
446
772
038
224
499
124
388
921
244
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
1 .30
0.24
1.66
0.26
1.66
0.19
1.65
0.23
1.38
0.19
1.63
1.82
0.37
2.57
0.17
0. 18
1.83
0.26
1.89
0.17
1.74
0.17
1.74
0.17
1.76
NOT FOUND
RETCL
12:42
3:03
3:06
4:47
4:53
5:54
6:00
7:10
7:19
9:24
9:27
10:19
10:25
10:34
10:34
11:02
11 :08
12:36
12:39
13:50
13:53
14:32
14:48
15:03
15:18
15:03
15:03
15:55
16:04
15:45
16:07
17:29
17:35
) RATIO
1.00
1.00
0.98
0.99
0.98
0.99
0.99
0.99
0.99
0.99
0.99
1.00
0.99
0.98
0.99
1.00
1.00
1.00
1.00
1.01
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
RRT(L)
1.000
0.238
0.242
0.373
0.381
0.460
0.468
0.560
0.571
0.734
0.738
0.306
0.813
0.825
0.825
0.861
0.869
0.984
0.988
1.079
1.083
1.135
1.155
1.175
1.194
1.175
1.175
1.242
1.254
1.230
1.258
1.365
1.373
RATIO
1.00
1.00
4.13
0.99
2.65
1.00
2.17
1.00
1.79
1.00
1.36
1.00
0.99
0.98
1.17
1.00
1.02
1.00
0.93
1.01
0.87
1.00
0.85
1.00
0.85
1.00
0.80
1.00
1.00
0.73
AMNT
20.00
19.26
200.56
21.43
199.94
21.74
203.50
23.15
201.31
32.98
203.21
944.07
1007.15
37.11
453.13
20.83
203.88
21.43
205.74
22.75
187.08
24.93
982.38
23.34
203.04
20.25
201.27
1010.87
20.48
206.14
AMNT(L)
20.00
20.00
20.00
20.00
20.00
20.00
20.00
20.00
20.00
20.00
20.00
20.00
100.00
20.00
100.00
20.00
100.00
20.00
20.00
20.00
20.00
20.00
20.00
20.00
100.00
20.00
20.00
20.00
20.00
20.00
100.00
20.00
2.0j0OJ)
R
1
3
11
2
14
4
10
0
28
3
16
1
2
2
1
0
28
3
10
1
19
5
2
2
10
0
24
1
1
14
.FAC
.000
.532
.160
.236
.130
.394
.490
.824
.145
.921
.241
.128
.072
.325
.815
.920
.455
.749
.692
.113
.195
.983
.879
.456
.638
.864
.303
.487
.867
.985
R.FAC(L)
1
3
1
2
1
4
1
0
2
2
1
1
0
1
0
1
0
0
2
3
1
0
2
4
0
2
1
0
2
1
0
1
1
.000
.668
.113
.087
.413
.042
.031
.712
.796
.378
.598
.000
.120
.000
.206
.253
.401
.882
.791
.499
.039
.979
.052
.799
.293
.104
.048
.853
.415
.000
.147
.824
.454
RATIO
1 .00
0.96
10.03
1.07
10.00
1.09
10.17
1.16
10.07
1.65
10.16
9.44
10.07
1.86
4.53
1 .04
10.19
1.07
10.29
1.14
9.35
1.25
9.82
1.17
10.15
1.01
10.06
10.11
1.02
10.31
E-277
-------
TABLE lA EXAMPLE OF VOLATILES QUANTITATION REPORT
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
18:30
17:23
23:11
18:06
18:03
18:15
18:15
19:59
20:08
20:11
20:17
20:57
20:57
21:39
21:48
21:21
21:21
21:39
21:36
23:02
24:21
24:21
27:36
26:56
27:00
27:18
27:18
28:58
29:08
30:21
30:30
33:09
33:30
27:24
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.357
1.357
1.000
0.779
0.779
0.787
0.787
0.862
0.862
0.871
0.875
0.904
0.904
0.941
0.941
0.921
0.921
0.934
0.932
0.993
1.050
1.050
1.000
0.976
0.978
0.989
0.989
1.050
1.055
1.099
1.105
1.201
1.214
1.342
1.01
1.00
1.00
1.28
1.00
1.27
1.00
1.17
1.00
1.15
1.00
1.11
0.99
1.07
1.00
1.09
1.00
1.07
1.00
1.00
1.00
1.00
1.00
1.02
1.00
1.00
1.00
0.95
1.00
0.91
1.00
0.83
1278.15
20.00
29.54
182.66
25.02
167.84
20.71
210.28
28.33
193.97
30.41
193.95
21.91
192.24
26.52
161.05
21.91
190.11
212.54
42.78
299.57
20.00
21.42
213.45
30.77
220.04
20.22
202.50
20.12
203.39
19.92
205.24
20
100
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
10
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
0
1
0
8
0
12
0
10
0
25
0
31
2
7
0
6
2
1
0
0
0
1
0
10
0
6
1
10
1
10
0
8
.102
.000
.174
.974
.756
.170
.643
.153
.683
.321
.389
.373
.356
.722
.672
.238
.356
.892
.854
.036
.763
.000
.794
.269
.156
.943
.442
.456
.601
.982
.783
.992
1 .000
0.008
1.000
0.118
0.983
0.604
1.450
0.621
0.966
0.482
2.611
0.256
3.235
2.151
0.803
0.507
0.775
2.151
0.199
0.080
0.017
0.051
1.000
0.742
0.962
0.101
0.631
1.426
1.033
1.592
1.080
0.786
.0.876
1.000
12.78
1.00
1.48
9.13
1.25
8.39
1.04
10.51
1.42
9.70
1.52
9.70
1.10
9.61
1.33
8.05
1.10
9.51
10.63
2.14
14.98
1.00
1.07
10.67
1.54
11.00
1.01
10.12
1.01
10.17
1.00
10.26
E-278
-------
TABLE IB EXAMPLE OF SEMIVOLATILES QUANTITATION REPORT
QUANTITATION REPORT FILE: OPR808
DATA: OPR808.TI
08/25/86 17:52:00
SAMPLE: S3,S,OPR,00100,00,C,1000:l,08/08/86-D$
CONDS.: 1625B,
AMOUNT=AREA * REF.AMNT/CREF.AREA)* RESP.FACT)
RESP. FAC. FROM AVERAGE OF WHOLE .RL
NO NAME
1 164 2,2'-DIFLUOROBIPHENYL
2 201 (OIO)ACENAPHTHENE
3 301 ACENAPHTHENE
4 277 (D8JACENAPHTHYLENE
5 377 ACENAPHTHYLENE
6 281 (OIO)PHENANTHRENE
7 381 PHENANTHRENE
8 278 (DIO)ANTHRACENE
9 378 ANTHRACENE
10 205 (OS)BENZIDENE
11 305 BENZIOENE
12 272 (D12)BENZO(A)ANTHRACENE
13 372 BENZO
-------
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
68
69
70
71
72
73
74
75
76
NO
1
2
3
4
" 5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
320
240
340
613
713
605
705
604
704
268
368
226
326
227
327
225
325
228
328
270
370
271
371
235
335
236
336
M/E
190
164
154
160
152
188
178
188
178
192
184
240
228
240
228
264
252
264
252
264
252
288
276
276
278
164
154
101
93
93
131
121
TABLE IB EXAMPLE OF SEMI VOLATI LES QUANTITATION REPORT
2-CHLORONAPHTHALENE
( 05 )4-CHLOROPHENYLPHENYL ETHER
4-CHLOROPHENYLPHENYLETHER
(D14)P-CYMENE
P-CYMENE
(DS)DIBENZOFURAN
DIBENZOFURAN
(DS)DIBENZOTHIOPHENE
DIBENZOTHIOPHENE
(D4)DI-N-BUTYLPHTHALATE
DI-N-BUTYLPHTHALATE
(04)1,3 DICHLOROBENZENE
1,3 OICHLOROBENZENE
(04)1,4 OICHLOROBENZENE
1,4 DICHLOROBENZENE
(04)1,2 DICHLOROBENZENE
1,2 DICHLOROBENZENE
(08) 3,3' OICHLOROBENZIOINE
3,3'DICHLOROBENZIDINE
(D4)DIETHYLPHTHALATE
DIETHYLPHTHALATE
(D4)DIMETHYLPHTHALATE
DIMETHYLPHTHALATE
(03)2,4 DINITROTOLUENE
2,4 DINITROTOLUENE
(03)2,6 DINITROTOLUENE
2,6 DINITROTOLUENE
SCAN
1060
1184
1190
1153
1156
1443
1447
1452
1455
1698
1700
1913
1918
1921
1926
2100
2105
2105
2108
2151
2158
2470
2485
2412
2417
1084
1087
623
632
853
712
722
TIME
18:33
20:43
20:49
20:11
20:14
25:15
25:19
25:25
25:28
29:43
29:45
33:29
33:34
33:37
33:42
36:45
36:50
36:50
36:53
37:39
37:46
43:13
43:29
42:13
42:18
18:58
19:01
10:54
11:04
14:56
12:28
12:38
REF
1
1
2
1
4
1
6
1
8
1
10
1
12
1
14
1
16
1
18
1
20
1
22
1
1
1
26
1
28
1
1
31
RRT
1.000
1.117
1.005
1.088
1.003
1.361
1.003
1.370
1.002
1.602
1.001
1.805
1.003
1.812
1.003
1.981
1.002
1.986
1.001
2.029
1.003
2.330
1.006
2.275
2.280
1.023
1.003
0.588
1.014
0.805
0.672
1.014
METH
A BB
QEDT
A BB
A BB
A BB
A?BV
QEDT
A?VB
A7BB
QEDT
RXRY
A?BV
QEDT
A?VB
A BB
QEDT
RXRY
QEDT
RXRY
A BB
RXRY
A BB
RXRY
QEOT
QEDT
A BB
RXRY
A BB
A?BB
A BB
QEDT
A BB
AREA(HGHT) AMOUNT
107460.
70129.
123654.
50064.
186728.
110518.
185306.
105243.
175722.
10270.
14501.
98172.
171666.
93726.
169461.
90405.
146838.
105743.
154233.
89381.
142419.
60675.
118967.
80395.
19622.
132581.
297557.
12473
79499
84974
18621
100
91
141
73
176
92
144
97
136
55
115
115
135
129
133
120
119
122
129
142
125
143
127
129
195
101
152
80
143
125
98
129
.000
.860
.982
.990
.889
.334
. 103
.668
.884
.499
.217
.999
.839
.095
.483
.360
.497
.339
.900
.435
.263
.628
.058
.628
.056
.468
.349
.978
.827
.253
.662
.493
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
XTOT
1.08
0.99
1.54
0.80
1.91
1.00
1.56
1.06
1.48
0.60
1.25
1.26
1.47
1.40
1.44
1.30
1.29
1.33
1.41
1.54
1.36
1.55
1.37
1.40
2.11
1.10
1.65
0.88
1.56
1.36
1.07
1.40
E-280
-------
TABLE IB
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
43
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
68
69
70
71
72
73
74
75
76
NO
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
1' ^
,-,
248
149
66
55
66
55
66
55
66
55
66
55
66
55
169
162
209
204
J'Q
^
1/6
168
192
184
153
149
152
146
152
146
152
146
258
252
153
149
167
163
168
165
167
165
RETCL
18:38
21:59
21:59
21:26
21:26
26:34
26 i*e
26:4b
26:43
30:56
30:56
35:01
35:01
34:54
34:54
1960
1962
1371
1845
631
651
878
898
1268
1290
1581
1606
1845
1872
2187
2227
1081
1084
1285
1288
669
681
1215
1219
1422
1425
1579
1581
647
650
657
660
688
660
1923
1924
1288
1290
1159
1160
1237
1239
1166
1169
34:18
34:20
24:00
32:17
11:03
11:24
15:22
15:43
22:11
22:34
27:40
28:06
32:17
32:46
38:16
38:58
18:55
18:58
22:29
22:32
11:42
11:55
21:16
21:20
24:53
24:56
27:38
27:40
11*19
11:22
11:30
11:33
12:02
11:33
33:39
33:40
22:32
22:34
20:17
20:18
21:39
21:41
20:24
20:27
) RATIO RRT(L
1.00
0.94
0.95
0.94
0.94
0.95
0.95
0.95
0.95
0.96
0.96
0.96
0.96
0.96
0.97
1.000
1.113
1.115
1.086
1.086
1.351
1.355
1.365
1.363
1.577
1.579
1.786
1.788
1.792
1.795
EXAMPLE
1
33
1
1
1
37
1
39
1
41
1
43
1
45
1
47
1
49
1
51
1
53
1
55
1
57
1
59
1
61
1
63
1
65
1
67
1
69
1
71
1
73
1
75
1.849
1.001
1.293
1.741
0.595
1.032
0.828
1.023
1.196
1.017
1.492
1.016
1.741
1.015
2.063
1.018
1.020
1.003
1.212
1.002
0.631
1.018
1.146
1.003
1.342
1.002
1.490
1.001
0.610
1.005
0.620
1.005
0.649
0.959
1.814
1.001
1.215
1.002
1.093
1.001
1.167
1.002
1.100
1.003
) RATIO
1
1
0
1
0
1
0
1
0
1
0
1
0
1
0
.00
.00
.90
.00
.92
.01
.74
.00
.74
.02
.63
.01
.56
.01
.56
OF SEMIVOLATILES QUANTITATION
A BB
A BB
A?BB
A BB
A?VV
RXRY
QEDT
RXRY
A BB
RXRY
A BB
RXRY
QEDT
QEDT
A BB
RXRY
A BB
RXRY
A BB
A?BB
QEDT
A BB
A?BB
QEDT
A?BB
QEDT
A BB
RXRY
A?BB
A?BV
QEDT
A BB
QEDT
QEDT
A?BB
RXRY
QEDT
QEDT
QEDT
A BB
QEDT
QEDT
A BB
A?VB
83029.
133048.
36900.
88137.
29963.
14490.
46577.
17707.
70158.
25524.
61077.
30946.
59993.
25671.
57395.
36742.
77165.
92149.
37993.
65993.
70927.
96523.
109759.
164942.
207620.
164667.
131129.
201667.
13868.
48563.
16980.
56032.
20105.
51042.
28439.
31307.
47300.
99372.
48416.
87639.
27625.
44185.
21713.
32491.
AUNT AMNT(L)
100.00
91.86
141.98
73.99
176.89
92.38
144.10
97.67
136.88
55.50
115.22
116.00
135.84
129.09
133.48
E-281
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
1 Q.Q. 04J
117
138
138
161
30
218
51
210
89
142
92
153
97
135
107
167
89
138
86
147
68
117
89
135
180
150
99
136
41
202
47
183
59
151
106
96
57
182
47
172
94
144
96
130
R.FAC
1.000
0.653
1.763
0.466
3.730
1.028
1.677
0.979
1.670
0.096
1.412
0.914
1.749
0.872
1.808
.971
.838
.603
.249
.748
.974
.076
.159
.423
.746
.696
.675
.947
.639
.938
.273
.813
.562
.243
.660
.837
.571
.708
.998
.495
.116
.932
.684
.343
.809
.511
.677
.045
.967
.412
.514
.280
.594
.168
.882
.980
.654
.545
.179
REPORT
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
R.FAC(L)
1.
0.
1.
0.
2.
1.
1.
1.
1.
0.
1.
0.
1.
0.
1.
000
710
242
630
109
113
164
003
220
172
226
788
287
676
355
1.28
1.50
1.50
1.74
0.33
2.37
0.55
2.27
0.97
1.54
1.00
1.66
1.06
1.47
1.17
1.81
0.97
1.50
0.93
1.60
0.74
1.27
0.97
1.47
1.95
1.62
1.08
1.48
0.45
2. 19
0.51
1.99
0.64
1 .64
1.15
1 .04
0.62
1.98
0.51
1.87
1.03
1.57
1.04
1.41
RATIO
1.00
0.92
1.42
0.74
1 .77
0.92
1.44
0.98
1.37
0.55
1. 15
1.16
1 . 36
1 .29
1.33
-------
TABLE IB EXAMPLE OF SEMIVOLATILES QUANTITATION REPORT
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
68
69
70
71
72
73
74
75
76
38:22
38:22
38:29
38:29
39:34
39:34
46:43
46:43
49:56
50:21
20:10
12:39
12:08
10:53
15:46
13:39
12:17
35:37
34:00
23:35
31:50
12:16
11:09
16:30
16:41
23:22
24:06
30:22
27:39
33:35
32:16
40:15
38:14
20:07
20:10
23:44
22:07
12:57
12:57
22:31
22:31
26:12
26:12
28:54
28:54
12:37
12:37
12:45
12:45
13:17
13:17
35:00
35:00
23:43
23:43
21:27
21:27
22:47
22:47
21:34
21:34
0.96
0.96
0.96
0.96
0.95
0.95
0.93
0.93
0.85
0.84
0.94
1.50
0.90
1.02
0.95
0.91
1.03
0.96
1.01
1.02
1.01
0.90
1.02
0.93
0.94
0.95
0.94
0.91
1.02
0.96
1.02
.0.95
1.02
0.94
0.94
0.95
1.02
0.90
0.92
Oo94
0.95
0.95
0.95
0.96
0.96
0.90
0.90
0.90
0.91
0.91
0.87
0.96
0.96
0.95
0.95
0.95
0.95
0.95
0.95
0.95
0.95
1.957
1.957
1.962
1.965
2.012
2.015
2.326
2.334
2.269
2.283
1.022
1.025
0.606
0.607
0.808
0.684
0.695
1.827
1.829
1.285
1.724
0.600
0.620
0.836
0.855
1.190
1.212
1.497
1.503
1.723
1.747
2.044
2.083
1.020
1.019
1.206
1.210
0.643
0.649
1.141
1.141
1.327
1.335
1.478
1.478
0.629
0.629
0.637
0.639
0.664
0.666
1.792
1.795
1.206
1.207
1.090
1 092
1 159
1 160
1 095
1 098
1.01
0.51
1.01
0.51
1.01
0.50
1.00
0.43
1.00
1.00
1.00
0.98
0.97
1.67
1.00
0.98
1.46
1.01
0.55
1.01
1.01
0.99
1.66
0.99
1.20
1.01
0.84
1.00
0.68
1.01
0.58
1.01
0.49
1.00
0.98
1.01
0.83
0.98
1.57
1.00
0.88
1.01
0.75
1.01
0.68
0.97
1.60
0.97
1.57
0.98
1.44
1.01
0.56
1.01
0.83
1.00
0.92
1.01
0.86
1.00
0.91
120.36
119.50
122.84
129.90
142.43
125.26
143.63
127.06
129.63
195.06
101.47
152.35
80.98
143.83
125.25
98.66
129.49
117.97
138.84
138.60
161.25
30.75
218.97
51.08
210.16
89.42
142.75
92.70
153.68
97.95
135.64
107.94
167.27
89.81
138.56
86.24
147.66
68.84
117.57
89.71
136.00
180.49
150.12
99.93
136.68
41.34
202.81
47.51
183.68
59.04
151.97
106.41
96.51
57.28
182.59
47.17
172.88
94.98
144.65
96.55
130.18
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
200.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
IftC? M
0.841
1.624
0.984
1.459
0.832
1.593
0.565
1.961
0.748
0.183
1.234
2.244
0.116
6.374
0.791
0.173
1.218
0.773
1.602
0.343
0.820
0.279
0.484
0.433
0.380
0.653
0.364
0.568
0.507
0.558
0.428
0.534
0.640
0.718
1.194
0.354
1.737
0.660
1.361
1.021
1 503
0.966
1.586
1.220
1.538
0.129
3.502
0.158
3.300
0.187
2.539
0.265
1.101
0.440
2.101
0.451
1.810
0.257
1.599
0.202
1.496
0.699
1.359
0.801
1.123
0.584
1.272
0.393
1.543
0.577
0.094
1.216
1.473
0.143
4.431
0.631
0.176
0.941
0.655
1.154
0.248
0.509
0.907
0.221
0.849
0.181
0.730
0.255
0.613
0.330
0.570
0.315
0.495
0.383
0.800
0.862
0.410
1.176
0.959
1.157
1.139
1.105
1.070
1.057
1.221
1.125
0.312
1.727
0.333
1.797
0.317
1.671
0.249
1.141
0.768
1.151
0.955
1 047
0 271
1 106
0 209
1 149
1.20
1.19
1.23
1.30
1.42
1.25
1.44
1.27
1.30
1.95
1.01
1.52
0.81
1.44
1.25
0.99
1.29
1.18
1.39
1.39
1.61
0.31
2.19
0.51
2.10
0.89
1.43
0.93
1.54
0.98
1.36
1.08
1.67
0.90
1.39
0.86
1.48
0.69
1.18
0.90
1.36
0.90
1.50
1.00
1.37
0.41
2.03
0.48
1.84
0.59
1.52
1.06
0.97
0.57
1.83
0.47
1.73
0.95
1.45
0.97
1.30
E-282
-------
TABLE la (CONTINUED) SEMIVOLATILES ASSOCIATED QUANTITATION REPORT
QUANTITATION REPORT FILE: OPR808
DATA: OPR808.TI
08/25/86 17:52:00
SAMPLE: S3,S,OPR,00100,00,C,1000:1,08/08/86-0$
CONDS.: 16258,
AMOUNT=AREA * REF.AMNT/CREF.AREA)* RESP.FACT)
RESP. FAC. FROM AVERAGE OF WHOLE .RL
NO NAME
1 164 2,2'-DIFLUOROBIPHENYL
2 269 (04) DI-N-OCTYLPHTHALATE
3 369 DI-N-OCTYLPHTHALATE
4 607 CD10) DIPHENYLAMINE
5 707 DIPHENYLAMINE
6 608 (DIO)DIPHENYLETHER
7 708 DIPHENYLETHER
8 237 (DIO)DIPHENYLHYDRAZINE
9 337 1,2 DIPHENYLHYDRAZINE
10 239 (DIO)FLUORANTHENE
11 339 FLUORANTHENE
12 284 (DIO)PYRENE
13 384 PYRENE
14 280 (DIQ)FLUORENE
15 380 FLUORENE
16 209 (13C6)HEXACHLOROBENZENE
17 309 HEXACHLOROBENZENE
18 252 (13C4)HEXACHLOROBUTADIENE
19 352 HEXACHLOROBUTADIENE
20 212 (13CDHEXACHLOROETHANE
21 312 HEXACHLOROETHANE
22 253 (13C4)HEXACHLOROCYCLOPENTADIENE
23 053 HEXACHLOROCYCLOPENTADIENE
24 254 (DS)ISOPHORONE
25 354 ISOPHORONE
26 255 (OS)NAPHTHALENE
27 355 NAPHTHALENE
28 602 (D7)B-NAPHTHYLAMINE
29 702 B-NAPHTHYLAMINE
30 256 (DS)NITROBENZENE
31 356 NITROBENZENE
32 061 N-NITROSODIMETHYLAMINE
33 063 N-NITROSODI-N-PROPYLAMINE
34 262 (06)N-NITROSODIPHENYLAMINE
35 362 N-NITROSODIPHENYLAMINE
36 265 (DS)PHENOL
37 365 PHENOL
38 603 (D7) A-PICOLINE
39 703 A-PICOLINE
40 610 (DS)STYRENE
41 710 STYRENE
42 609 (DS)A-TERPINEOL
43 509 A-TERPINEOL
44 208 (03)1,2,4 TRICHLOROBENZENE
45 308 1,2,4 TRICHLOROBENZENE
46 222 (02) 4-CHLORO-3-METHYLPHENOL
47 322 4-CHLORO-3-METHYLPHENOL
48 224 (04) 2-CHLOROPHENOL
49 324 2-CHLOROPHENOL E 283
-------
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
63
69
70
71
72
73
74
NO
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
TABLE IB (CONTINUED) SEMIVOLATI
231 (03) 2,4 DICHLOROPHENOL
331 2,4 DICHLOROPHENOL
259 (D3)2,4 DINITROPHENOL
359 2,4 DINITROPHENOL
260 (D2) 2-METHYL-4,6-DINITROPHENOL
360 2-METHYL-4,6-DINITROPHENOL
257 (04) 2-NITROPHENOL
357 2-NITROPHENOL
258 (04) 4-NITROPHENOL
358 4-NITROPHENOL
264 (13C6)PENTACHLOROPHENOL
364 PENTACHLOROPHENOL
221 (D2)2,4,6 TRICHLOROPHENOL
321 2.4,6 TRICHLOROPHENOL
234 (02) 2,4 DIMETHYLPHENOL
334 2,4 DIMETHYLPHENOL
531 2,4,5 TRICHLOROPHENOL
530 2,3,6 TRICHLOROPHENOL
529 1,2,3 TRICHLOROBENZENE
518 N-TETRADECANE
520 N-OCTAOECANE
522 N-OOCOSANE
524 N-HEXACOSANE
525 N-OCTACOSANE
528 CARBAZOLE
M/E
190
153
149
179
169
180
170
82
77
212
202
212
202
176
166
292
284
231
225
204
201
241
237
88
82
136
128
150
143
128
123
74
70
175
SCAN
1060
2067
2068
1309
1314
1105
1110
1310
1316
1656
1660
1694
1698
1274
1280
1391
1392
915
916
740
740
1041
1041
802
809
874
877
1248
1251
758
761
234
748
1312
TIME
18:33
36:10
36U1
22:54
23:00
19:20
19:25
22:55
23:02
28:59
29:03
29:39
29:43
22:18
22:24
24:21
24:22
16:01
16:02
12:57
12:57
18:13
18:13
14:02
14:09
15:18
15:21
21:50
21:54
13:16
13:19
4:06
13:05
22:58
REF
1
1
2
1
4
1
6
1
8
1
10
1
12
1
14
1
16
1
18
1
20
1
1
1
24
1
26
1
28
1
30
1
1
1
RRT
1.000
1.950
1.000
1.235
1.004
1.042
1.005
1.236
1.005
1.562
1.002
1.598
1.002
1.202
1.005
1.312
1.001
0.863
1.001
0.698
1.000
0.982
0.982
0.757
1.009
0.825
1.003
1.177
1.002
0.715
1.004
0.221
0.706
1.238
METH
A BB
A BB
A BB
QEDT
RXRY
A?BB
QEDT
A BB
A BB
A BB
A BB
A BB
A BB
QEDT
A BB
A?BB
RXRY
A BB
RXRY
A BB
RXRY
A BB
A BB
QEDT
RXRY
A BB
RXRY
A?BB
A BB
A?BB
A BB
A BB
QEDT
A?BB
LES ASSOCIATED QUANTI
TATION
AREA(HGHT) AMOUNT
107460.
143775.
240328.
64139.
120649.
55859.
85654.
.98702.
172069.
109709.
179722.
109394.
185183.
80181.
140832.
18979.
34019.
9961.
28306.
3245.
13715.
1697.
8490.
95203.
160471.
105146.
180320.
14520.
49135.
23684.
35461.
41740.
63489.
*gy3«.
100.
135.
135.
85.
137.
84.
138.
82.
157.
98.
147.
100.
141.
101.
129.
94.
123.
72.
150.
35.
222.
55.
67.
87.
142.
79.
143.
46.
316.
83.
143.
107.
130.
85.
000
457
396
889
544
978
999
535
483
307
826
739
871
325
170
277
320
803
926
116
595
062
086
342
082
885
467
703
879
687
975
944
887
454
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
REPORT
XTOT
1.19
1.61
1.61
1.02
1.63
1.01
1.65
0.98
1.87
1.17
1.75
1.20
1.68
1.20
1.53
1.12
1.46
0.86
1.79
0.42
2.64
0.65
0.80
1.04
1.69
0.95
1.70
0.55
3.76
0 99
1 71
1 28
1 55
1 01
E-284
-------
TABLE IB (CONTINUED) SEMIVOLATILES ASSOCIATED QUANTITATION REPORT
35
36
37
38
39
40
41
42
43
44
45
46
47
43
49
50
51
52
53
54
55
56
57
53
59
60
61
62
63
64
65
66
67
63
69
70
71
72
73
74
NO
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
169
71
94
100
93
109
104
1314
634
636
339
344
473
476
23:00
11:06
11:08
5:56
6:01
8:17
8:20
34
1
36
1
38
1
40
1.002
0.598
1.003
0.320
1.015
0.446
1.006
RXRY
QEDT
RXRY
A BB
A BB
A BB
A BB
103729.
13368.
71975.
38307.
41582.
25038.
54823.
132.720
87.694
127.512
69.071
136.715
35.453
201.822
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
1.57
1.04
1.51
0.82
1.62
0.42
2.39
NOT FOUND
59
183
180
109
107
132
128
167
162
187
184
200
198
143
139
143
139
272
266
200
196
124
122
196
196
180
55
55
55
55
55
167
RETCL
18:52
37:33
29U7
19:07
25:27
15:37
15:34
24:11
24:17
24:11
23:30
24:11
24:03
18:06
18:00
20:23
19:37
13:11
12:42
891
863
870
999
998
631
634
862
863
1212
1216
1309
1310
814
816
1246
1246
1429
1430
1061
1062
842
843
1069
1092
910
1106
1455
1743
1988
2099
1492
15:36
15:11
15:13
17:29
17:28
11:03
11:06
15:05
15:06
21:13
21:17
22:54
22:55
14:15
14:17
21:43
21:48
25:00
25:01
18:34
13:35
14:44
14:45
18:42
19*:07
15:55
19:21
25:28
30:30
34:47
36:44
26:07
) RATIO RRTCL
0.98
0.96
1.24
1.20
0.90
1.24
1.25
0.95
0.95
1.20
1.24
1.23
1.24
1.23
1.24
1.19
1.24
1 .22
1.26
1.000
1.924
1.927
1.222
1.227
1.041
1.046
1.225
1.229
1.546
1.550
1.580
1.585
1.194
1.199
1.305
1.305
0.872
0.872
1
1
44
1
46
1
48
1
50
1
52
1
54
1
56
1
58
1
60
1
62
1
64
1
1
1
1
1
1
1
1
1
0.841
0.819
1.002
0.942
0.999
0.595
1.005
0.813
1.001
1.143
1.003
1.235
1.001
0.768
1.002
1.175
1.000
1.348
1.001
1.001
1.001
0.794
1.001
1.008
1.030
0.858
1.043
1.373
1.644
1,875
1.980
1.408
) RATIO
1
1
0
1
0
1
0
1
0
1
0
1
0
1
0
1
0
0
1
.00
.01
.52
.01
.82
.00
.96
.01
.82
.01
.65
.01
.63
.01
.84
.01
.77
.99
.15
A?BB
QEDT
RXRY
A BB
RXRY
A BB
RXRY
QEDT
QEDT
QEDT
RXRY
QEDT
QEDT
A BB
QEDT
A?BV
RXRY
A BB
RXRY
A?BV
RXRY
QEDT
RXRY
QEDT
QEDT
A BB
A BB
A BB
A BB
QEDT
QEDT
A?BB
AMNT;
100.00
135.46
135.40
85.89
137.54
84.98
139.00
82.53
157.48
98.31
147.33
100.74
141.87
101.33
129.17
94.28
123.32
72.80
150.93
79586.
39227.
63032.
36837.
57225.
42815.
61913.
19970.
42143.
2300.
2709.
12529.
17624.
24818.
34296.
9620.
10847.
7731.
10703.
33775.
61945.
17300.
26104.
40489.
40067.
55181.
23518.
29798.
28663.
30552.
29190.
140684.
AMNT(L)
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
10-0*800
R
1
1
1
0
1
0
1
0
1
1
1
1
1
0
1
0
1
0
2
131.130
81.887
143.393
96.536
136.043
33.308
136.137
31.558
129.050
21.528
133.703
77.720
135.614
87.204
133.171
69.945
108.875
64.074
143.443
105.940
143.180
44.540
131.328
142.543
148.899
116.012
109.253
136.221
143.459
161.644
151.641
140.405
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
UG/ML
.FAC R.FAC(L)
.000 1.
.338 0.
.672 1.
.597 0.
.331 1.
.520 0.
.533 1.
.913 1.
.743 1.
.021 1.
.633 1.
.018 1.
.693 1.
.746 0.
.756 1
.177 0
.792 1
.093 0
.842 1
000
983
235
695
363
612
103
113
107
039
108
Oil
193
736
360
187
453
127
883
1.56
0.97
1.70
1.15
1.61
0.99
1.62
0.97
1.53
0.26
1.59
0.92
1.61
1.03
1.53
0.33
1.29
0.76
1.70
1.26
1.70
0.53
1.56
1.69
1.77
1.38
1.30
1.62
1.70
1.92
1.30
1.67
RATIO
1.00
1.35
1.35
0.86
1.38
0.85
1.39
0.83
1.57
0.98
1.48
1.01
1.42
1.01
1.29
0. 94
1 . 23
0 . 73
1.51
E-285
-------
TABLE IB (CONTINUED) SEMIVOLATILES ASSOCIATED QUANTITATION REPORT
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
5*
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
68
69
70
71
72
73
74
10:36
10:14
15:06
12:01
8:29
11U4
12:18
12:11
17:40
17:39
10:38
10:32
2:58
10:50
18:36
18:34
8:46
8:41
2:13
2:36
10:16
10:21
17:36
12:22
17:17
12:04
11:03
13:51
8:50
8:45
12:01
11:55
14:24
17:04
15:36
18:32
11:26
13:58
23:11
22:44
17:21
17:23
14:56
14:49
16:18
11:36
18:17
18:42
15:36
18:56
24:59
30:00
34:33
38:09
25:40
1.22
1.26
1.21
1.52
1.65
1.26
1.24
1.26
1.24
1.24
1.25
1.26
1.38
1.21
1.23
1.24
1.27
1.28
2.67
2.31
0.81
0.81
1.26
0.88
1.26
1.58
1.26
1.25
1.27
1 25
1.27
1.47
1.25
1.47
1.24
1.25
1.02
0.94
0.96
1.44
1.44
1.24
1.25
0.90
1.27
1.02
1.02
1.02
1.02
1.02
1.02
1.01
0.96
1.02
0.706
0.706
0.986
0.986
0.761
0.768
0.830
0.833
1.168
1.171
0.720
0.722
0.267
0.710
1.228
1.230
0.614
0.617
0.360
0.376
0.478
0.481
0.844
0.843
0.830
0.826
0.938
0.938
0.612
0.615
0.81'4
0.816
1.131
1.130
1.224
1.225
0.772
0.774
1.159
1.162
1.338
1.341
0.999
1.000
0.799
0.800
1.005
1.027
0.863
1.039
1.364
1.630
1.855
1.958
1.398
0.99
1.42
1.00
1.00
0.99
1.31
0.99
1.20
1.01
0.86
0.99
1.39
0.83
0.99
1.01
0.81
0.97
1.63
0.89
2.70
0.93
2.09
1.00
0.99
1.21
1.00
1.07
0.97
1.63
1.00
1.23
1.01
0.89
1.01
0.82
0.99
1.29
1.01
0.86
: 1.01
0.75
1.00
1.00
0.99
1.25
1.00
1.00
0.99
1.00
1.01
1.01
1.01
1.01
1.01
35.12
222.59
55.06
67.09
87.34
142.08
79.89
143.47
46.70
316.88
83.69
143.97
107.94
130.89
85.45
132.72
87.69
127.51
69.07
136.72
35.45
201.82
131.13
81.89
143.39
96.54
136.04
83.81
136.14
81.56
129.05
21.53
133.70
77.72
135.61
87.20
133.17
69.95
108.88
64.07
143.44
105.94
143.18
44.54
131.33
142.54
148.90
116.01
109.26
136.22
143.46
161.64
151.64
140.41
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
0.030
4.226
0.016
0.079
0.886
1.686
0.978
1.715
0.135
3.384
0.220
1.497
0.388
0.591
0.656
1.471
0.129
5.190
0.356
1.085
0.233
2.190
0.741
0.365
1.607
0.343
1.551
0.398
1.446
0.186
2.110
0.021
1.178
0.117
1.407
0.231
1.382
0.090
1.128
0.072
1.384
0.314
1.834
0.161
1.509
0.377
0.373
0.514
0.219
0.277
0.267
0.284
0.272
1.309
0.086
1 .899
0.029
0.118
1.014
1.186
1.225
1.195
0.289
1.068
0.263
1.040
0.360
0.451
0.768
1.108
0.147
4.070
0.516
0.794
0.657
1.085
0.462
0.565
0.446
1.121
0.356
1.140
0.475
1.062
0.228
1.635
0.099
0.881
0. 150
1.037
0.265
1.038
0.128
1.036
0.112
0.965
0.297
1.281
0.361
1.149
0.264
0.250
0.443
0.200
0.204
0.186
0.176
0.179
0.932
0.35
2.23
0.55
0.67
0,87
1.42
0.80
1.43
0.47
3.17
0.84
1.44
1.08
1.31
0.85
1.33
0.88
1.28
0.69
1.37
0.35
2.02
1.31
0.82
1.43
0.97
1.36
0.84
1.36
0.82
1.29
0.22
1.34
0.78
1.36
0.87
1.33
0.70
1.09
0.64
1.43
1.06
1.43
0.45
1.31
1.43
1.49
1.16
1.09
1.36
1.43
1.62
1.52
1.40
E-286
-------
TABLE 1C EXAMPLE OF DIOXIN QUANTITATION REPORT
OUANTITATION REPORT FILEI TCDDOTA
DATA! TCD0074
02/06/84 2li35fOO
SAMPLES 02,S«CAt,Ol006«00,0,NAtNA,NAf
CONDS.I 6i3E»60M,0.2SMM,3*100,100-250*15,15f250,30CM/3S
FORMULAI
SUBMITTED BYI
AMOUNTwAREA
INSTRUMENTi 02
ANALYST! SH
REF.AMNT/CREF.AREA)* RESP.
HEICHTI
ACCT.NO.I
0.000
NO NAME
1 184 2,3t7,8-TCDD-37CL4
2 429 ?,3,7,8-TCOO-l3C12
3 029 2,3,7,8-TCDO
NO
1
2
3
w/E
326
332
320
SCAN
1517
1515
1517
TIME
20|24
2^122
24i24
REF
1
1
2
RRT M£TH
1.000 * BB
0.994 A B6
1.001 A 98
NO RET(L) RATIO RRTCLJ RATIO AUNT
01 20(26 1.00 1.000 1.00 1000.00
02 2«I24 t.OO 0,999 1.00 985,41
03 2<>t26 1.00 1,001 1.00 1011.62
AMOUNT XTOT
15020. 1000.000 N6/ML 33.37
131«6. 965.413 NG/ML 32.86
11382. 1011.62fl NG/HL 33.75
P.FAC R.FAC(L) RATIO
1000.00 1.000 1.000 1.00
1000.00 0.875 0.8«8 0.99
1000.00 0.758 0.7"9 1.01
E-287
-------
TABLE 2 - Quantitation Report Magnetic Tape Transmittal Form Description
The main purpose of the tape transmittal form is to ensure the complete and
correct data processing of a tape volume (reel). Depending upon the number of files
per volume at least one tape transmittal form must accompany each tape volume sent
to the Sample Control Center. Field descriptions are as follows.
Laboratory
Return Tape To
External Tape //
Lab Tape ID
Tape Density
Block Size
Number of Files
Contact Person and Phone Number
File Position
Lab Data File
The laboratory name.
The address to which the tape volume is to be
returned after processing by the SCC.
The tape number assigned by the SCC.
The laboratory tape identification.
Either 800 or 1600 bpi.
800 decimal words or bytes per block.
The number of Quantitation report files on
the tape.
Whom to contact at the laboratory, regarding
any difficulties in the processing of the tape
volume, and their phone number including
area code.
The relative file position of the Quantitation
Report File on the tape volume. The first
file on the tape has a relative file position of
1. The second file on the tape has a relative
file position of 2.
The laboratory data file identification.
E-288
10/28/86
-------
Instrument ID
Note:
The laboratory assigned instrument specific 2
digit alphanumeric code that is used to
identify a GC/MS instrument.
All quantitation files for calibration, preci-
sion and recovery, standards and blanks will
be tracked by this instrument number within
a given laboratory. Changing of this instru-
ment number by the laboratory would necess-
itate the submittal of new calibration and
initial precision and recovery quantitation
reports by the laboratory.
EPA Sample Number
The 5 digit sample number for the sample:
Sample Type Sample Number
IPR20
IPR 100
BLK
BLK 1000
CAL 10
CAL20
CAL 50
CAL 100
CAL 200
CAL 1000
CAL 5000
CAL 20000
CAL 40000
EPA
FBK
VER
VER 1000
00020
00100
00000
01000
00010
00020
00050
00100
00200
01000
05000
20000
40000
SCC Assigned
Sample Number
SCC Assigned
Sample Number
00100
01000
E-289
10/28/36
-------
Bottle Number
: The 2 digit (numeric) bottle number used to
identify each individual aliquot of the sample.
Sample Type
EPA
EPA (analysis of
TCLP Leachate)
All Others
Bottle Number
01-98
99
00
Type
The 3 position EGLD code signifying the
sample or quantitation type. Required.
Sample Type
IPR
BLK
CAL
EPA
FBK
OPR
VER
Meaning
Initial Precision
and Accuracy
Blank
Calibration
EPA Sample
Field Blank
Ongoing Precision
and Accuracy
Calibration Verification
for extraction methods
Fraction
1 position code:
A = Acid
B = Base/Neutral
C = Combined Acid Base/Neutral
D = Dioxin
V = Volatile
P = Pesticide
N/A if not applicable.
E-290
10/28/86
-------
Conc/Dilu : The concentration or dilution ratio of the
sample fraction before analysis. N/A if not
applicable.
Date Analyzed : The date of analysis.
E~291 10/28/36
-------
USEPA Industrial Technology Division Revision: C
Quantitation Report Magnetic Tape Transmittal Form Date: 10 October 36
Laboratory: External Tape //:
Return Tape To: Lab Tape ID:
Tape Density (BPI):
Block Size:
Number of Files:
Contact Person and Phone Number: ( )
Lab Instrument EPA Bottle Cone Date
File Position Data File ID Sample // // Type Fraction Dilu Analyzed
The data recorded on this tape have been verified and are true and complete.
Date: Analyst: QA:
E-292 10/23/86
-------
Table 2a - Quantitation Report Magnetic Tape Additional Files Transmittal Form
This form is only to be used when there are more than 14 quantitation report
files on a tape and it must be used with a Quantitation Report Magnetic Tape
Transmittal Form. As many Additional Files Transmittal Forms can be used to
accommodate all of the files on the tape. The field definitions are identical to those
on the Quantitation Report Magnetic Tape Transmittal Form.
E-293 10/28/86
-------
USEPA Industrial Technology Division Revision: C
Quantitation Report Magnetic Tape Date: 10 October 86
Additonal Files Transmittal Form
(This form must be used with the Quantitation
Report Magnetic Tape Transmittai Form)
Laboratory: External Tape //:
Lab Instrument EPA Bottle Cone Date
File Position Data File ID Sample // // Type Fraction Dilu Analyzed
E_294 10/28/86
-------
TAB 3
Report Form I
oo
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
001
002
003
004
005
006
007
008
009
010
Oil
012
013
014
015
016
017
018
019
020
021
022
023
024
025
026
027
028
029
030
031
032
033
034
035
036
037
038
039
040
041
042
043
044
045
046
047
048
049
050
B ACENAPHTHENE
V ACROLEIN
V ACRYLONITRILE
V BENZENE
B BENZIDINE
V CARBON TETRACHLORIDE
V CHLOROBENZENE
B 1,2,4-TRICHLOROBENZENE
B HEXACHLOROBENZENE
V 1,2-DICHLOROETHANE
V 1,1,1-TRICHLOROETHANE
B HEXACHLOROETHANE
V 1,1-DICHLOROETHANE
V 1,1,2-TRICHLOROETHANE
V 1,1,2,2-TETRACHLOROETHANE
V CHLOROETHANE
V BIS (CHLOROMETHYL) ETHER (NR)
B BISC2-CHLOROETHYDETHER
V 2-CHLOROETHYLVINYL ETHER
B 2-CHLORONAPHTHALENE
A 2,4,6-TRICHLOROPHENOL
A 4-CHLORO-3-METHYLPHENOL
V CHLOROFORM
A 2-CHLORQPHENOL
B 1,2-DICHLOROBENZENE
B 1,3-DICHLOROBENZENE
B 1,4-DICHLOROBENZENE
B 3,3'-DICHLOROBENZIDINE
V 1,1-DICHLOROETHENE
V TRANS-1,2-DICHLOROETHENE
A 2,4-DICHLOROPHENOL
V 1,2-DICHLOROPROPANE
V T-1.3-DICHLOROPROPENE
B 2,4-DIMETHYLPHENOL
B 2,4-DINITROTOLUENE
B 2,6-DINITROTOLUENE
B 1,2-DIPHENYLHYDRAZINE
V ETHYLBENZENE
B FLUORANTHENE
B 4-CHLOROPHENYL PHENYL ETHER
B 4-BROMOPHENYL PHENYL ETHER
B BIS (2-CHLOROISOPROPYL) ETHER
B BIS (2-CHLOROETHOXY) METHANE
V METHYLENE CHLORIDE
V CHLOROMETHANE
V BROMOMETHANE
V BROMOFORM
V BROMODICHLOROMETHANE
V TRICHLOROFLUOROMETHANE (NR)
V DICHLORODIFLUOROMETHANE (NR)
P 0154 Y
P 0056 Y
0053 Y
0078 Y
0184 Y
0047 Y
0112 Y
0180 Y
0284 Y
0062 Y
0097 Y
P 0201 Y
P 0063 Y
P 0083
P 0083
0064
P
P
P
P
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
0093 Y
0106 Y
P 0162 Y
P 0196 Y
P 0107 Y
P 0085
P 0128
P 0146
P 0146
P 0146
P 0252
P 0061
P 0061
P 0162 Y
P 0063 Y
P 0075 Y
P 0122 Y
P 0165 Y
P 0165 Y
P 0077 Y
P 0106 Y
P 0202 Y
P 0204 Y
P 0248 Y
0121 Y
0093 Y
0084 Y
0050 Y
P 0096 Y
P 0173 Y
P 0083
P
P
Y
Y
Y
E-296
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
051
052
053
054
055
056
057
058
059
060
061
062
063
064
065
066
067
068
069
070
071
072
073
074
075
076
077
078
079
080
081
082
083
084
085
086
087
088
089
090
091
092
093
094
095
096
097
098
099
100
V DIBROMOCHLOROMETHANE
B HEXACHLORO-1.3-BUTADIENE
B HEXACHLOROCYCLOPENTADIENE
B ISOPHORONE
B NAPHTHALENE
B NITROBENZENE
A 2-NITROPHENOL
A 4-NITROPHENOL
A 2,4-DINITROPHENOL
A 2-METHYL-4,6-DINITROPHENOL
B N-NITROSODIMETHYLAMINE
B N-NITROSODIPHENYLAMINE
B N-NITROSODI-N-PROPYLAMINE
A PENTACHLOROPHENOL
B PHENOL
B BIS (2-ETHYLHEXYL) PHTHALATE
B BUTYL BENZYL PHTHALATE
B DI-N-BUTYL PHTHALATE
B DI-N-OCTYL PHTHALATE
B DIETHYL PHTHALATE
B DIMETHYL PHTHALATE
B BENZO(A)ANTHRACENE
B BENZO(A)PYRENE
B BENZO(B)FLUORANTHENE
B BENZO(K)FLUORANTHENE
B CHRYSENE
B ACENAPHTHYLENE
B ANTHRACENE
B BENZO(GHI)PERYLENE
B FLUORENE
B PHENANTHRENE
B DIBENZO(A,H)ANTHRACENE
B INDENO(1,2,3-CD)PYRENE
B PYRENE
V TETRACHLOROETHENE
V TOLUENE
V TRICHLOROETHENE
V VINYL CHLORIDE
P ALDRIN
P DIELDRIN
P CHLORDANE
P 4,4'-DDT
P 4,4'-DDE
P 4,4'-DDD
P ALPHA-ENDOSULFAN
P BETA-ENDOSULFAN
P ENDOSULFAN SULFATE
P ENDRIN
P ENDRIN ALDEHYDE
P HEPTACHLOR
P 0129 Y
P 0225 Y
P 0237 Y
P 0082 Y
P 0128 Y
P 0123 Y
P 0139 Y
P 0139 Y
P 0184 Y
P 0198 Y
P 0074 Y
P 0169 Y
P 0070 Y
P 0266 Y
P 0094 Y
P 0149 Y
P 0149 Y
P 0149 Y
P 0149 Y
P 0149 Y
P 0163 Y
P 0228 Y
P 0252 Y
P 0252
P 0252
P 0228 Y
P 0152 Y
P 0178 Y
0276 Y
0166 Y
P 0178 Y
P 0278 Y
P 0276 Y
P 0202 Y
P 0164 Y
P 0092 Y
P 0095 Y
P 0062 Y
P
P
P
P
P
P
P
P
P
P
P
P
P
P
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
E-297
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
101
102
103
104
105
106
107
108
109
110
111
112
113
129
130
150
151
152
153
154
155
156
157
158
159
160
161
162
163
164
165
166
167
168
169
170
172
173
174
175
176
177
178
179
180
181
182
183
184
185
P HEPTACHLOR EPOXIDE
P ALPHA-BHC
P BETA-BHC
P 6AMMA-BHC
P DELTA-BHC
P PCB-1242
P PCB-1254
P PCB-1221
P PCB-1232
P PCB-1248
P PCB-1260
P PCB-1016
P TOXAPHENE
D 2,3,7,8-TCDD
V XYLENES
A PHENOL-D5
A PENTAFLUOROPHENOL
V PENTAFLOUROBENZENE
A TRIFLUORO-M-CRESOL
V 2,2-DIFLUOROTETRACHLOROETHANE
B 2-FLUOROBIPHENYL
B 1-FLUORONAPHTHALENE
A 2-FLOUROPHENOL
B 2-FLUORONAPHTHALENE
B PYRIDINE-D5
B ANILINE-OS
B NAPHTHALENE-OS
V TOLUENE-D8
B NITROBENZENE-05
B 2,2'-DIFLUOROBIPHENYL
V BENZENE-D6
B OECAFLUOROBIPHENYL
V M-DIFLUOROBENZENE
V METHYLENE CHLORIDE-D2
V 1,1,2,2-TETRACHLOROETHANE-D2
V ETHYLBENZENE-D10
V 1,2 DICHLOROETHANE-D4
V 2,2 DICHLOPROPANE-D6
V CHLOROBENZENE-D5
B 1,2 DICHLOROBENZENE-D4
B CHRYSENE D12
B FLUORENE D10
A 2-NITROPHENOL D4
B DI-N-BUTYL-PHTHALATE-D4
B 4-FLUOROANILINE
V BROMOCHLOROMETHANE
V 2-BROMO-l-CHLOROPROPANE
V 1,4-DICHLOROBUTANE
D 2,3,7,8-TCDD-37CL4
V BROMOFLUOROBENZENE
P
P
P
P
P
P
P
P
P
P
> 0320
S
S
S
S
S
S
S
S
S
S
S
S
S
S
I 0190
S
S
S
S
S
S
S
S
S
S
S
S
S
S
S
I 0128
I 0077
I 0055
I 0328
I 0095
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
E-298
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
186
187
188
189
201
202
203
204
205
206
207
208
209
210
211
212
213
214
215
216
217
218
219
220
221
222
223
224
225
226
227
228
229
230
231
232
233
234
235
236
237
238
239
240
241
242
243
244
245
246
CODE
DESCRIPTION
B DFTPP
P 2f-CHLOROBIPHENYL-D5
P 3*,4' ,5'-TRICHLOROBIPHENYL-D5
P 3,3' ,4,4'-TETRACHLOROBIPHEN-D6
B ACENAPHTHENE-D10
V ACROLEIN-D4
V ACRYLONITRILE-D3
V BENZENE-D6
B BENZIDINE (RINGS-OS)
V CARBON TETRACHLORIDE-13C
V CHLOROBENZENE-D5
B 1,2,4-TRICHLOROBENZENE-D3
B HEXACHLOROBENZENE-13C6
V 1,2-DICHLOROETHANE-D4
V 1,1,1-TRICHLOROETHANE-D3
B HEXACHLOROETHANE-1-13C
V l,l-DICHLOROETHANE-2,2,2-D3
V 1,1,2-TRICHLOROETHANE-13C2
V 1,1,2,2-TETRACHLOROETHANE-D2
V CHLOROETHANE-D5
V
B BIS(2-CHLOROETHYL)ETHER-D8
V
B 2-CHLORONAPHTHALENE-D7
A 2,4,6-TRICHLOROPHENOL-3,5-D2
A 4-CHLORO-3-METHYLPHENOL-2.6-D2
V CHLOROFORM-13C
A 2-CHLOROPHENOL-3,4,5f6-D4
B 1,2-DICHLOROBENZENE-D4
B 1,3-DICHLOROBENZENE-D4
B 1.4-DICHLOROBENZENE-D4
B 3,3'-DICHLOROBENZIDINE-D6
V 1,1-DICHLOROETHENE-D2
V TRANS-1,2-DICHLOROETHENE-D2
A 2,4-DICHLOROPHENOL-3,5,6-D3
V 1,2-DICHLOROPROPANE-D6
V T-1,3-DICHLOROPROPENE-1,2-D4
B 2,4-DIMETHYLPHENOL-3, 5,6-03
B 2,4-DINITROTOLUENE-3,5,6-D3
B 2,6-DINITROTOLUENE-A,A,A-D3
B 1,2-DIPHENYL-DlO-HYDRAZINE
V ETHYLBENZENE-D10
B FLUORANTHENE-D10
B 4-CHLOROPHENYL PHENYL-D5 ETHER
B
B BISC2-CHLOROISOPROPYDETHERD12
B
V METHYLENE CHLORIDE-D2
V CHLOROMETHANE-D3
V BROMOMETHANE-D3
I
s
s
s
D
D
D
D
D
D
D
D
D
D
D
D
D
D
D
D
D
D
D
D
D
D
D
D
D
D
D
0
D
D
D
D
D
D
D
D
D
D
D
D
D
D
D
D
D
D
0198
0164
0060
0056
0084
0192
0048
0117
0183
0292
0067
0102
0204
0066
0084
0084
0071
0101
0113
0169
0200
0109
0086
0132
0152
0152
0152
0258
0065
0065
0167
0067
0079
0125
0168
0167
0082
0116
0212
0209
0131
0088
0053
0099
N
N
N
N
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
N
Y
N
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
N
Y
N
Y
Y
Y
E-299
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
247
248
249
250
251
252
253
254
255
256
257
253
259
260
261
262
263
264
265
266
267
268
269
270
271
272
273
274
275
276
277
278
279
280
281
282
283
284
285
286
287
288
289
290
291
292
293
294
295
296
V BROMOFORM-13C
V BROMODICHLOROMETHANE-13C
V
V
V DIBROMOCHLOROMETHANE-13C
B HEXACHLORO-1.3-BUTADIENE-13C4
B HEXACHLOROCYCLOPENTADIENE-13C4
B ISOPHORONE-D8
B NAPHTHALENE-OS
B NITROBENZENE-OS
A 2-NITROPHENOL-3,4,5,6-04
A 4-NITROPHENOL-2,3,5,6-04
A 2,4-DINITROPHENOL-3,5,6-03
A 2-METHYL-4,6-DINITROPHENOL-D2
B
B N-NITROSODIPHENYLAMINE-D6
B
A PENTACHLOROPHENOL-13C6
B PHENOL-2,3,4,5,6-05
B BIS(2-ETHYLHEXYL)PHTHALATE-D4
B
B DI-N-BUTYL PHTHALATE-D4
B DI-N-OCTYL PHTHALATE-D4
B DIETHYL PHTHALATE-3,4,5,6-04
B DIMETHYL PHTHALATE-3,4,5,6-04
B BENZO(A)ANTHRACENE-012
B BENZO(A)PYRENE-D12
B BENZO(B)FLUORANTHENE-D12
B BENZO(K)FLUORANTHENE-012
B CHRYSENE-012
B ACENAPHTHYLENE-D8
B ANTHRACENE-DIO
B BENZO(6HI)PERYLENE-D12
B FLUORENE-D10
B PHENANTHRENE-D10
B
B
B PYRENE-D10
V TETRACHLOROETHENE-1.2-13C2
V TOLUENE-2,3,4,5,6-D8
V TRICHLOROETHENE-13C2
V VINYL CHLORIDE-D3
P ALDRIN-13C4
P DIELDRIN-13C4
P
P 4,4'-DDT-D8
P 4,4'-DDE-D8
P 4,4'-DDD-D8
P ENDOSULFAN-I-D4
D
D
0
D
D
D
D
D
D
D
D 0176
D 0086
D
D
D 0130
D 0231
D 0241
D 0088
0 0136
D 0128 Y
D 0143 Y
D 0143 Y
D 0187 Y
0 0200 Y
D N
D 0175 Y
D N
D 0272 Y
D 0071 Y
D 0153 Y
0 N
0 0153 Y
D 0153
D 0153
D 0167 Y
D 0240 Y
D 0264 Y
D 0264 Y
D 0264 Y
D 0240 Y
D 0160 Y
D 0188 Y
D 0288 Y
D 0176 Y
D 0188 Y
Y
Y
D 0212 Y
D 0172 Y
D 0098 Y
D 0136 Y
D 0065 Y
N
N
N
N
N
N
N
N
E-300
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
297
298
299
301
302
303
304
305
306
307
308
309
310
311
312
313
314
315
316
317
318
319
320
321
322
323
324
325
326
327
328
329
330
331
332
333
334
335
336
337
338
339
340
341
342
343
344
345
346
347
p
p
p
B ACENAPHTHENE
V ACROLEIY
V ACRYLONITRILE
V BENZENE
B BENZIDINE
V CARBON TETRACHLORIDE
V CHLOROBENZENE
B 1,2,4-TRICHLOROBENZENE
B HEXACHLOROBENZENE
V 1,2-DICHLOROETHANE
V 1,1,1-TRICHLOROETHANE
B HEXACHLQROETHANE
V 1,1-DICHLOROETHANE
V 1,1,2-TRICHLOROETHANE
V 1,1,2,2-TETRACHLOROETHANE
V CHLOROETHANE
V
B BISC2-CHLOROETHYDETHER
V
B 2-CHLORONAPHTHALENE
A 2,4,6-TRICHLOROPHENOL
A 4-CHLORO-3-METHYLPHENOL
V CHLOROFORM
A 2-CHLOROPHENOL
B 1,2-DICHLOROBENZENE
B 1,3-DICHLOROBENZENE
B 1,4-DICHLOROBENZENE
B 3,3'-DICHLOROBENZIDINE
V 1,1-DICHLOROETHENE
V TRANS-1.2-DICHLOROETHENE
A 2,4-DICHLOROPHENOL
V 1,2-DICHLOROPROPANE
V T-1,3-DICHLOROPROPENE
B 2t4-DIMETHYLPHENOL
B 2,4-DINITROTOLUENE
B 2,6-DINITROTOLUENE
B 1,2-DIPHENYLHYDRAZINE
V ETHYLBENZENE
B FLUORANTHENE
B 4-CHLOROPHENYL PHENYL ETHER
B
B BIS (2-CHLOROISOPROPYL) ETHER
B
V METHYLENE CHLORIDE
V CHLOROMETHANE
V BROMQMETHANE
V BROMOFORM
D N
D N
D N
P 0154 Y
P 0056 Y
P 0053 Y
P 0078 Y
P 0184 Y
P 0047 Y
P 0112 Y
P 0180 Y
P 0284 Y
P 0062 Y
0097 Y
0201 Y
0063 Y
0083 Y
0083 Y
0064 Y
N
0093 Y
0106 N
0162 Y
0196 Y
0107 Y
0085 Y
0128 Y
0146
0146
0146
0252
0061 Y
0061 Y
0162 Y
0063 Y
0075 Y
P 0122 Y
P 0165 Y
P 0165 Y
P 0077 Y
P 0106 Y
P 0202 Y
P 0204 Y
P N
P 0121 Y
Y
Y
Y
Y
P
P
P
N
0084 Y
0050 Y
P 0096 Y
P 0173 Y
E-301
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
0
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
398
399
400
402
404
429
500
501
502
503
504
505
506
507
503
509
510
511
512
513
514
515
516
517
518
519
520
521
522
523
524
525
526
527
528
529
530
531
532
533
534
535
536
537
538
539
540
541
542
543
P
P
P HEPATACHLOR-13C4
P ALPHA-BHC-D6
P GAMMA-BHC-D6
D 2,3,7,8-TCDD-13C12
A BEN20IC ACID
A HEXANOIC ACID
B B-NAPHTHYLAMINE
B ALPHA-PICOLINE
B DIBENZOTHIOPHENE
B DIBENZOFURAN
B N-OODECANE (N-C12)
B DIPHENYLAMINE
B DIPHENYL ETHER
B ALPHA-TERPINEOL
B STYRENE
B DI-N-BUTYL AMINE
B BIPHENYL
B P-CYMEME
V 2-BUTANONE (MEK)
V DIETHYL ETHER
V ACETONE
B N-DECANE (N-CIO)
B N-TETRADECANE (N-C14)
B N-HEXADECANE (N-C16)
B N-OCTADECANE (N-C18)
B N-EICOSANE (N-C20)
B N-DOCOSANE (N-C22)
B N-TETRACOSANE (N-C24)
B N-HEXACOSANE (N-C26)
B N-OCTACOSANE (N-C28)
B N-TRIACONTANE (N-C30)
V P-DIOXANE
B CARBAZOLE
B 1,2,3-TRICHLOROBENZENE
A 2,3,6-TRICHLOROPHENOL
A 2,4,5-TRICHLOROPHENOL
V ALLYL ALCOHOL
V CARBON DISULFIDE
V 2-CHLORO-l,3-BUTADIENE
V CHLOROACETONITRILE
V 3-CHLOROPROPENE
V CROTONALDEHYDE
V 1,2-DIBROMOETHANE (EDB)
V DIBROMOMETHANE
V TRANS-l,4-DICHLORO-2-BUTENE
V 1,3-DICHLOROPROPANE
V CIS-1,3-DICHLOROPROPENE
V ETHYL CYANIDE
P
P
D
D
D
N
N
N
N
N
D 0332 Y
P Y
P Y
P 0143 Y
P 0093 Y
P 0184 Y
P 0168 Y
P 0055 Y
P 0169 Y
P 0170 Y
P 0059 Y
P 0104 Y
P 0086 N
P 0154 Y
P 0119 Y
P 0072 Y
0074 Y
0058 Y
0055 Y
0055 Y
0055 Y
0055 Y
0055 Y
0055 Y
P 0055 Y
P 0055 Y
P 0055 Y
P 0055 Y
P 0088 Y
P 0167 Y
P 0180 Y
P 0196 Y
P 0196 Y
P 0057 Y
P 0076 Y
P 0053 Y
P 0075 Y
0076 Y
0070 Y
P 0107 Y
P 0093 Y
P 0075 Y
P 0076 Y
P 0075 Y
P 0054 Y
P
P
E-303
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
544
545
546
547
548
549
550
551
552
553
554
555
556
557
558
559
560
561
562
563
564
565
566
567
568.
569
570
571
572
573
574
575
576
577
578
579
580
581
582
583
584
585
586
587
588
589
590
591
592
593
V ETHYL METHACRYLATE
V 2-HEXANONE
V IODOMETHANE
V ISOBUTYL ALCOHOL
V METHACRYLONITRILE
V METHYL METHACRYLATE
V 4-METHLY-2-PENTANONE
V 1,1,1,2-TETRACHLOROETHANE
V TRICHLOROFLUOROMETHANE
V 1,2,3-TRICHLOROPROPANE
V VINYL ACETATE
B ACETOPHENONE
B 4-AMIN08IPHENYL
B ANILINE
B 0-ANISIDINE
B ARAMITE
B BENZANTHRONE
B 1,3-BENZENEDIOL (RESORCINOL)
B BENZENETHIOL
B 2,3-BENZOFLUORENE
B BENZYL ALCOHOL
B 2-BROMOCHLQROBENZENE
B 3-BROMOCHLOROBENZENE
B 4-CHLORO-2-NITROANILINE
B 5-CHLORO-O-TOLUIDINE
B 4-CHLOROANILINE
B 3-CHLORONITROBENZENE
B 0-CRESOL
B CROTOXYPHOS
B 2,6-DI-TERT-BUTYL-P-BENZOQINO
B 2,4-DIAMINQTOLUENE
B l,2-DIBROMO-3-CHLOROPROPANE
B 2,6-DICHLORO-4-NITROANILINE
B 1.3-DICHLORO-2-PROPANOL
B 2,3-DICHLOROANILINE
B 2,3-DICHLORONITROBENZENE
B 1,2:3,4-DIEPOXYBUTANE
B 3t3'-DIMETHOXYBENZIDINE
B DIMETHYL SULFONE
B P-DIMETHYLAMINOAZOBENZENE
B 7,12-DIMETHYLBENZ(A)ANTHRACENE
B N.N-DIMETHYLFORMAMIDE
B 3,6-DIMETHYLPHENANTHRENE
B 1,3-DINITROBENZENE
B DIPHENYLDISULFIDE
B ETHYL METHANESULFONATE
B ETHYLENETHIOUREA
B ETHYNYLESTRADIOL 3-METHYL ETHE
B HEXACHLOROPROPENE
B 2-ISOPROPYLNAPHTHALENE
Y
Y
Y
Y
P 0069 Y
P 0058 Y
P 0142 Y
P 0074 Y
P 0067 Y
P 0069
P 0058
P 0131
P 0101
P 0075 Y
P 0086 Y
P 0105 Y
P 0169 Y
P 0093 Y
P 0108 Y
P 0185 Y
P 0230 Y
P 0110 Y
P 0110 Y
P 0216 Y
P 0079 Y
P 0111 Y
P 0192 Y
P 0172 Y
P 0106 Y
P 0127 Y
P 0157 Y
P 0108 Y
P 0127 Y
P 0220 Y
P 0122 Y
P 0157 Y
P 0124 Y
P 0079 Y
P 0161 Y
P 0191
P 0055
P 0224 Y
0079 Y
0120 Y
0256 Y
0073 Y
0206 Y
0168 Y
0218 Y
0109 Y
0102 Y
P 0227 Y
P 0213 Y
P 0170 Y
Y
Y
E-304
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
0
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
CODE
DESCRIPTION
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
712
713
714
715
716
717
718
719
720
721
722
723
724
725
726
727
728
729
730
731
829
900
901
902
903
904
905
906
907
908
909
910
911
912
913
914
915
916
917
918
919
920
921
922
923
924
925
926
927
928
B BIPHENYL
B P-CYMENE
V 2-BUTANONE CMEK)
V DIETHYL ETHER
V ACETONE
B N-DECANE (N-C10)
B
B N-HEXAOECANE (N-C16)
B
B N-EICOSANE (N-C20)
B
B N-TETRACOSANE (N-C24)
B
B
B N-TRIACONTANE (N-C30)
V P-DIOXANE
B CARBAZQLE
B 1,2,3-TRICHLOROBENZENE
A 2,3,6-TRICHLOROPHENOL
A 2,4,5-TRICHLOROPHENOL
D 2,3,7,8-TCDD
B 3-METHYLCHOLANTHRENE
B 4,4'-METHYLENEBIS(2-CHLOROANI)
B 4,5-METHYLENEPHENANTHRENE
B 1-METHYLFLUORENE
B 2-METHYLNAPHTHALENE
B 1-NETHYLPHENANTHRENE
B 2-(METHYLTHIO)BENZOTHIAZOLE
B 1,5-NAPHTHALENEDIAMINE
B 1,4-NAPHTHOQUINONE
B ALPHA-NAPHTHYLAMINE
B 5-NITRO-O-TOLUIDINE
B 2-NITROANILINE
B 3-NITROANILINE
B 4-NITROANILINE
B 4-NITROBIPHENYL
B N-NITROSODI-N-BUTYLAMINE
B N-NITROSODIETHYLAMINE
B N-NITROSOMETHYLETHYLAMINE
B N-NITROSOMETHYLPHENYLAMINE
B N-NITROSOMORPHOLINE
B N-NITROSOPIPERIDINE
B PENTACHLOROBENZENE
B PENTACHLQROETHANE
B PENTAMETHYLBENZENE
B PERYLENE
B PHENACETIN
B PHENOTHIAZINE
B 1-PHENYLNAPHTHALENE
B 2-PHENYLNAPHTHALENE
0154 Y
0119 Y
0072 Y
0074 Y
0058 Y
0055 Y
N
0055 Y
N
0055 Y
N
0055 Y
N
N
0055 Y
0088 N
0167 N
0180 N
0196 N
0196 N
0320 Y
0263 Y
0231 Y
0190 Y
0180
P 0142
P 0192
P 0181
P 0158 Y
P 0158 Y
P 0143 Y
P 0152 Y
P 0138 Y
P 0138 Y
P 0138 Y
P 0199 Y
P 0084 Y
P 0102 Y
P 0088 Y
P 0106 Y
P 0056 Y
P 0114 Y
P 0248 Y
P 0117 Y
P 0148 Y
P 0252 Y
P 0108 Y
P 0199 Y
P 0204 Y
P 0204 Y
Y
Y
Y
Y
E-306
-------
10/30/86 ISOTOPE DILUTION
COMPOUND CODE TABLE
TABLE
NUMBER
TABLE
CODE
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
04
929
930
931
932
933
934
935
936
937
938
939
940
941
942
943
944
945
946
947
948
TABLE COUNT:
CODE
DESCRIPTION
B PRONAMIDE P 0173 Y
B PYRIDINE P 0079 Y
B SAFROLE P 0162 Y
B SQUALENE P 0069 Y
B 1,2,4,5-TETRACHLOROBENZENE P 0216 Y
B THIANAPHTHENE P 0134 Y
B THIOACETAMIDE P 0075 Y
B THIOXANTHONE P 0212 Y
B 0-TOLUIDINE P 0106 Y
B 1,2,3-TRIMETHOXYBENZENE P 0168 Y
B 2,4,5-TRIMETHYLANILINE P 0120 Y
B TRIPHENYLENE P 0228 Y
B TRIPROPYLENEGLYCOL METHYL ETHE P 0059 Y
B 1,3,5-TRITHIANE P 0138 Y
A BENZOIC ACID P 0105 Y
A P-CRESOL P 0108 Y
A 3,5-DIBROMO-4-HYDROXYBENZONITR P 0227 Y
A 2,6-DICHLOROPHENOL P 0166 Y
A HEXANOIC ACID P 0060 Y
A 2,3,4,6-TETRACHLOROPHENOL P 0232 Y
570
E-307
-------
E-308
-------
ATTACHMENT 10
E-309
-------
APPENDIX G
STORAGE. PREPARATION AND SHIPMENT OF SAMPLE EXTRACTS
E-310
10/28/86
-------
APPENDIX G
STORAGE, PREPARATION AND SHIPMENT OF SAMPLE EXTRACTS
A. Storage
1. All samples/sample extracts shall be stored in a dark contaminant-free area
at 20 to 10°C, except when samples/sample extracts are being analyzed.
A line shall be marked on sample containers at the solvent level, per the
method. Extracts shall be tightly capped with unpierced septa or cap liners
to prevent sample loss by evaporation.
B. Preparation
1. Contractor shall label each extract with the EPA Episode and Sample (Traffic
Report) number, in addition the information on the Sample Extract Trans-
mittal Form (Figure 1) shall be completed in full and signed by the
appropriate persons. EPA Episode and Sample numbers on the extract labels
shall agree with the numbers on the "Transmittal" form.
2. Sample containers shall be packed in foam or other material which will
preclude breakage during shipment. Packaging in "Vial File" or other
compartmentalized container is recommended. NOTE: If breakage occurs
during shipment, and it is determined that such breakage is due to improper
packaging on the part of the Contractor, the Contractor shall be subject to
liquidated damages as specified in the contract.
E~311 10/28/36
-------
C. Shipment
1. Contractor shall ship sample extracts via approved ground carrier (i.e. UPS
or equivalent) in consideration of solvents used in extraction. All containers
in the shipment shall be marked according to applicable DOT regulations for
the concerned compounds.
2. Contractor shall ship sealed vials containing labeled extracts and the
applicable "Sample Extract Transmittal Form" to:
AquAir Corporation
13300 Sam Neely Drive
P.O. Box 70*8
Charlotte, North Carolina 28217
Attn: James H. Pugh
E-312 10/28/86
-------
USEPA Industrial Technology Division
Sample Extract Transmitta
Episode) Industrial
Number Category
L Form
Sample Number
EPA
Lab
Extraction
Frac
Type
Cone
factor
Dates
Rec
Extr
Analy
Revised Octc
Int std
Type
Cone*
>ber 1986
Initials
Spec I
J£_
M
Co
i-1
Co
The extracts in this shipment were estracted and concentrated per all contract specifications.
Date: . Extraction Specialist: QA:
-------
M
-------
ATTACHMENT 11
E-315
-------
APPENDIX F
GC/MS RAW DATA ON MAGNETIC TAPE
E-316 10/28/86
-------
APPENDIX F
GC/MS RAW DATA ON MAGNETIC TAPE
A. All GC/MS mass intensity data from analyses of samples, sample dilutions,
blanks, calibration standards, initial and ongoing precision and recovery, and BFB
and DFTPP shall be reporded on magnetic tape per the specifications below:
1. Data Format
Type:
Record Length:
Block Size
Code:
9-track BPI, 2,*00 foot reels
80
4,000 (specify)
ASCII
2. The first two (2) records shall contain the sample identification and other
information necessary to rigorously identify the sample. Subsequent
records shall contain eight (8) mass-intensity pairs, each of which shall be
ten (10) characters long. Each mass and each intensity shall be five (5)
characters long and left justified. At the end of each spectrum in a single
run, the last mass-intensity pair shall be "zero Zero" (00) to denote the end
of the spectrum. An end-of-file mark shall be placed at the end of each
GC/MS run. For example:
2 Records Sample 1 identification
N Records: Spectrum 1 of sample, last mass-intensity pair is "00"
to denote end of spectrum
M Records: Spectrum 2 of sample, last mass intensity pair is "00" to
denote end of spectrum
End of File
2 Records: Sample 2 identification
STC
E-317
10/28/86
-------
3. Contractor shall package magnetic tapes carefully to ensure that they are
not damaged in shipment and ship them by first class mail or equivalent.
Contractor shall complete a GC/MS Raw Data Tape Transmittal Form for
each magnetic tape submitted.
Contractor shall ship magnetic tapes containing GC/MS raw data and the
applicable GC/MS Raw Data Transmittal Form to:
ITD Sample Control Center
300 N. Lee Street, Suite 200
Alexandria, Virginia 22313
E-318 10/28/86
-------
USIiPA Industrial Technology Division
GCMS Raw Data Tape Transmitta1
Revised October 1986
Episode
Number
Industrial
Category
Sample Number
Analysis
Date
Initials
EPA
Lab
CO
Data File Name Frac Type Analyzed Analyst
The data recorded on this tape has been verified and meets all contract specifications.
Date: Analyst: QA:
-------
E-320
-------
ATTACHMENT 12
E-321
-------
LABORATORY RESULTS
METALS ANALYSIS
EPISODE NO.
SAMPLE NO.
Lab Name
Industrial Category_
Date Analyzed
ICP RESULTS
1. Calcium
2. Mag
nesium
3. Sodium
-------
ATTACHMENT 13
E-323
-------
SCC TAPE PROCESSING STEPS
STEP 1. DEBLOCK tope.
STEP 2. REVIEW Lab Transmittal/Error Report.
STEP 3. ACCEPT or REJECT Tape:
* REJECTED return Tapes to Lab.
" ACCEPTED Continue to STEP 4.
STEP 4. ARCHIVE Original Guantitation Reports received.
STEP 5. Make Quantitation Report Corrections as required:
* POST CHANGES in individual Quantitation Reports.
* RERUN Lab Transmittal/Error Report.
" REPEAT UNTIL NO ERRORS.
STEP 6. Run Tracking File Merge.
STEP 7. Run LEVEL 1 Edits on Data':
* VERIFY all Edit Runs to insure
successful completion.
" RESOLVE Processing Problems with DP,
STEP 8. Run LEVEL 1 Error Summary Report,
STEP 9. Run LEVEL 2 Edits,*
" VERIFY all Edit Runs to insure
successful completion.
* RESOLVE Processing Problems with DP.
STEP 10. MaKe LEVEL 1 Edits, LEVEL 1 Error Summary Report
and LEVEL 2 Edits avaijjible for QC Review.
STEP 11. Results of QC Review.'
" TOTAL NON-COMPLIANCE
(1) Return Tapes to Lab.
(2) Retain original archived
Quantitation Reports until
data is resubmitted, When
received, replace with new
submission.
* INDIVIDUAL QUANTITATION CORRECTIONS
(1) Make corrections to individual
Quantitations.
(2) Changes to header information
iriust be coordinated with DP*
(3) Repeat procedure from STEP 5.
" TOTAL COMPLIANCE Continue with STEP 12.
STEP 12. Run Remedial Report and moKe available to EGD,
STEP 13. ARCHIVE Modified Quantitation Files ( P010 ).
E-324
-------
Inform Lab of
Tape Resubmit
Determine
Tape Status
( Reanalysis)
( Crucial )
Receive Tape
From Lab
Assign
VOLSER Number!
Ship Tape NCC
Receive SLOT
Number;
DEBLOCK Tape
Replace OLD
Files/Tapes
rfith New Files
^
f
lebuild &
large Corrected
Tapes
^
f
Resubmit Tape
for LEVEL 1
EDITS
,Y XTapeaS/
i^esubmit^X^
N
Submit Tape
for LEVEL 1
EDITS
-------
f- Jo- -d Y
VIAR HANDLING PROCEDURE FOR INCOMING DATA TAPE PACKAGES ~ SCC
1. TAPE IS RECEIVED FROM LAB.
" Assign External Tape Number ( 6 digit )» also called VOLSER Nunber
VOLSER > lab consecutive
Number ID Number « Lab-Specific »
XXX XXX
2. SEND TAPE ( with VIAR - assigned documentation ) to NCC.
* Affix TAG to each tape: EPATQS (S.HancocK),EGLDSSCSP,C81A,
<703> 557-5040, VOLSER » XXX XXX.
" Send by overnight courier ( FED EXPRESS ) to NCC in North Carolina
ADDRESS:
TAPE LIBRARIAN
EPA ~ NCC
MD - 24
RESEARCH TRIANGLE PARK, NC
27711
3. NCC WILL ASSIGN A SLOT NUMBER ( B Number ) to
each tape, and will transmit
This Nunber to VIAR by telephone the next day ( by 12:00 )
4. TAPE DEBLOCKING PROCESS ( Selection 1 on LAB TAPE TRACKING SYSTEM nenu (Selection
4 on SAMPLE CONTROL CENTER MAIN MENU >
~ Use the SLOT NUMBER and the VOLSER NUMBER to DeblocK the Tape.
" Only 8 files are deblocked at a ti*e, using Selection 1 on
the LAB TAPE TRACKING SYSTEM menu « TAPE TRACKING FILE
DEBLOCK AND BUILD PROCEDURE »
* Transmittal Reports are produced as deblocking Job output.
LAB TAPE TRACKING REPORTS are produced separately,
using Selection S on the LAB TAPE TRACKING SYSTEM nenu.
" Two types of files produced:
(1) Multiple quantitative report files
(2) a ftaster file/list of these quantitative
report files ( CONTROL )
E-326
-------
5, Quantitative Report Corrections are made.
* Contact lab for solving discrepancies if needed*
" HaKe necessary changes to Header Information
* Compare tape transmittal for* (Master List fro*
tape) with hard copy transmittal foms and resolve
all discrepancies.
" Can't do Level 1 Edits until header information
corrected*
" ChecK DATE/TIME
" Check for duplicate compound entries
6. 00 LEVEL 1 EDITS
" If the Tape is a NEW TAPE, and not a resubmittal tape
(to correct erroneous files in previously subnitted tapes ),
the next step is to submit the tape for LEVEL 1 EDITS.
~ If the Tape is a resubmittal, see Procedure 7.
" Uhen scanning the LAB TAPE TRACKING REPORT, produced
by Selection 5 on the LAB TAPE TRACKING SYSTEM main
menu? a 'G' indicates a no-error status.
" Level 1 Edits of disk quantitation files
are performed!
(1) tape specs verified
(2) data completeness checked
(3) retention times* RRTs checked
" If no errors detected, data from disk
quantitation files are merged with output
data set. ( Selection 3, LAB TAPE TRACKING
SYSTEM MENU « TAPE TRACKING FILE MERGE
PROCEDURE » )
" Level 2 Edits may be performed.
* Level 1 Summary Error Listing may be produced
if desired.
" If REJECTED, tapes are returned to lab, and corrected
tape is resumbitted.
E-327
-------
7. TAPE RESUBMISSION PROCEDURE.
After the RESUBMISSION TAPE is Deblocked, the old
files ( from the tapes in error ) are replaced with
corrected files fro* the replacement tape? Selection 5
on the QUANTITATION REPORT CORRECTION PROCESSING menu,
« ' Quantitation Report Processing} Quantitation File
Replacement Procedure * »
After replacing the erroneous files with the correct
files fro* the new tape* the corrected tapes are
Rebuilt Selection 2 on the LAB TAPE TRACKING
SYSTEM Menu; then
Merged Selection 3 on the LAB TAPE TRACKING
SYSTEM Menu.
Corrected Tapes can then be resubmitted for LEVEL 1 Edits,
Selection 2 on the LABORATORY PROCESSING Menu, Resub.it
DisK Quantitation Files *. Files are edited one file
a tii*.
" Only 1 file at a ti*e is edited» except for
ASSOCIATED files ( have same ID, done at
same tine and date )
E-328
-------
ATTACHMENT 14
E-329
-------
QUALITY ASSURANCE TESTS OF DATA ELEMENTS ON QUANTITATION REPORTS
This document describes tests of data fields which occur when a gas
chromatography-mass spectrometry (GCMS) quantitation report is processed
through EPA's computerized quality assurance system at the Agency's
National Computer Center (NCC). GCMS quantitation reports are received on
magnetic tape from laboratories performing chemical analyses of organic
pollutants. The specifications for these quantitation reports are
contained in an EPA document titled "Quantitation Reports on Magnetic
Tape." The data elements tested are defined in an EPA document titled "EGD
Data Elements," and an outline of the tape processing steps is given in an
EPA Sample Control Center document titled "SCC Tape Processing Steps."
1. General Tests
1.1 Multiple header records (type 10) may be present. If present, the
records must be equal. If not equal, an error condition exists.
1.2 There must be only one compound record for each compound analyzed.
Duplicate records for a given compound are prohibited with one
exception: duplicate records for internal standards. With this
exception, duplicate records constitute an error condition.
1.3 Multiple compound records for internal standards may be present.
If present, all records for each internal standard must be equal.
If not equal, an error condition exists.
1.4 All isotope compounds (200 and 600 series) for the fraction
analyzed must be present in the quan report. If any are missing,
an error condition exists.
1.5 For scmi-volatiles, the only valid internal standard is compound
E-330
-------
164 (2,2'-difluorobiphenyl). For volatiles, the only valid
internal standards are compounds J81, 182, and 183 (bromochloro-
methane; 2-bromo, 1-chloropropane; and 1,4-dichlorobutane). Each
of these three must be present in the quan report for volatiles.
1.6 For quan reports submitted in multiple parts (termed "Associated
Quans"), there must be identical internal standard compounds
present in each part. The number of identical header records
shall be used to establish the number of parts present. If the
multiple internal standard records are not present, an error
condition exists.
1.7 There must be at least one header record present for a
quantitation report. If no header record is present, an error
condition exists.
2. Processing of "Not Found" compounds
2.1 The following fields must be present for a compound not found:
CMPD Number
CMPD Order Number
M/Z
REF CMPD Number
RT (LIB)
RRT (LIB)
AMT (LIB)
R. FAC (LIB)
The above fields will be edited.
2.2 The following fields must not be present. If present, an error
condition exists:
SCAN
RT
Rev: 30 Dec 86
E-331
-------
RRT
AREA
AMOUNT
UNITS of Measure
R. FAC
2.3 The above fields will not be edited.
2.4 A Not Found condition is determined all above fields not being
present.
3. Detailed Tests--the following table summarizes the data fields tested.
The numbers are used to reference the detailed tests described below:
Field
Data Field Number
Amount 26
Amount (Library) 30
Bottle Number 7
Carrier Gas Flow Rate 17
Column Final Hold 16
Column Initial Hold 14
Column Inside Diameter 13
Column Length 12
Column Temperature Program 15
Compound Number 19
Compound Reference Number 18
Concentration/Dilution Factor 9
Date Analyzed 1
Date Extracted 10
Fraction 8
Rev: 30 Dec 86
E-332
-------
Instrument 3
Mass to Charge Ratio 20
Method 11
Peak Area 25
Quantitation Report Type 5
Reference Compound 23
Relative Retention Time 24
Relative Retention Time (Library) 29
Response Factor 31
Response Factor (Library) 28
Sample Number 6
Scan Number 21
Analysis Shift 4
Time Analyzed 2
Unit of Measure 27
1 Date Analyzed
1.1 Must be present
1.2 Format: MM/DD/YY
1.3 Limits: MM-01-12 DD=01-31 YY=83-99
2 Time Analyzed
2.1 Must be present
2.2 Format: HH:MM:SS or H:MM:SS or MM:SS
2.3 Limits: HH=00-24 MM=00-59 SS=00-59
3 Instrument
3.1 Must be present
3.2 Must be a valid instrument code for the lab (Table II)
4 Shift
Rev: 30 Dec 86
E-333
-------
4.1 Must be present
4.2 Must be a valid code: D=Day S=Swing G=Graveyard
5 Quan Report Type
5.1 Must be present
5.2 Must be a valid code (Table 12)
5.3 Must be valid for Method (Table 12)
6 Sample Number
6.1 Must be present
6.2 For quan report type EPA:
6.2.1 Must be valid number in Episode/Sample File
6.3 For quan report type CAL or VER:
6.3.1 Must be valid concentration: 00010; 00020; 00050; 00100;
00200 (or 5x these amounts for volatile gases and water
soluble compounds).
6.4 For quan report type BLK:
6.4.1 Must be 00000
6.5 For remaining quan report types: must be numeric
7 Bottle Number
7.1 Must be present
7.2 For quan report type EPA:
7.2.1 Must be in range of 00 to 99
7.2.2 For TCLP: must be 99
7.3 For remaining quan report types: must be 00
8 Fraction
8.1 Must be present
8.2 Must be a valid code: A, B, C, P, V
8.3 Must be valid for the method and quan report type
8.3.1 For 1624: V only
Rev: 30 Dec 86
E-334
-------
8.3.2 For 1625, type EPA: A, B, C, P
8.3.3 For 1625, all others: C
9 Concentration/dilution factor
9.1 Must be present
9.2 Format: XXXXX:XXXXX
9.3 For volatile fraction (V):
9.3.1 For aqueous samples: must be 1:XXXXX
9.3.1.1 For quan types CAL, APS, VER, BLK, must be 1:1
9.3.2 For solid samples: must be S(.)N(.)N(.)N:XXXXX, where S
indicates a solid sample and (.) indicates that decimal point
must appear somewhere in the field.
9.3.2.1 For quan types CAL, APS, VER, BLK, must be S5.0:l
9.4 For semi-volatile fraction
9.4.1 For quan types CAL and VER, must be NA:NA
9.4.2 Aqueous samples:
9.4.2.1 For quan types APS, PAR, OPR, and BLK: must be
1000:1
9.4.3 Solid samples:
9.4.3.1 For quan types APS, PAR, OPR, and BLK: must be
530.0:1
9.4.3.2 For quan types EPA, FBK: must be
S(.)N(.)N(.)N:XXXXX, where S indicates a solid sample and (.)
indicates that a decimal point must appear somewhere in the
field.
10 Date Extracted
10.1 Must be present for semi-volatile quan report types EPA, BLK,
IPR, PAR, and OPR
10.2 Format: MM/DD/YY-X
Rev: 30 Dec 86
E-335
-------
10.3 Limits: MM=00-12 DD=00-31 YY=83-99
11 > x=Shift: D, S, G
10.4 For semi-volatiles quan report types CAL, VER or for volatiles
fraction, must be NA
12 Method
12.1 If present must equal 1624A, 1624B, 1624C, 1625A, 1625B, 1625C
12.2 If fraction V, must be 1624A, 1624B, or 1624C
12.3 If fraction A, B, or C, must be 1625A, 1625B, or 1625C
13 Column length
13.1 If present must be as follows:
13.1.1 If fraction V, must be in range 2.8-3.1 M
13.1.2 If fraction A, B, or C, must be in range 25-35 M
13.2 Unit of measure must be meters (M)
14 Column inside diameter
14.1 If present must be as follows:
14.1.1 If fraction V, must be in range 1-3 mm
14.1.2 If fraction A, B, or C, must be in range 0.2-0.35 mm
14.1.3 Unit of measure must be mm
15 Column initial hold
15.1 If present must be as follows:
15.1.1 Format: Hold @ temp: MM@TTT
15.1.2 Temperature ranges:
15.1.2.1 Volatile: 25-50
15.1.2.2 Semi-volatile: 25-35
15.1.3 Hold ranges:
15.1.3.1 Volatile: 2-4
15.1.3.2 Semi-volatile: 4-6
16 Column temperature program
Rev: 30 Dec 86
E-336
-------
16.1 If present must be as follows:
16.1.1 Format: initial temp - final temp @ rate: TTT-TTT@RR
16.1.2 Rate must be 8
16.1.3 Initial temp must equal initial hold temp (item 15)
16.1.4 Final temp must equal column final hold temp (item 17)
17 Column final temp/hold
17.1 li present must be as follows:
17.1.1 Format: Hold @ temp: MM@TTT
17.1.2 Temperature ranges:
17.1.2.1 Volatile: 200-250
17.1.2.2 Semi-volatile: 270-290
17.1.3 Hold ranges:
17.1.3.1 Volatile: 5-25
17.1.3.2 Semi-volatile: 10-20
18 Carrier gas flow rate
18.1 If present must be as follows:
18.1.1 Volatile:
18.1.1.1 Range: 20-40
18.1.1.2 Unit of measure: ML/MIN
18.1.2 Semi-volatile:
18.1.2.1 Range: 20-60
18.1.2.2 Unit of measure: CM/S
19 Compound order number
19.1 Must be present
19.2 Range: 001-250
20 Compound number
20.1 Must be present
20.2 Must be valid number in compound table (Table 4)
Rev: 30 Dec 86
E-337
-------
20.3 Fraction on quan report must agree with number in compound table.
If fraction on quan report = C, then table value can be A or B
only
20.4 If compound order number = 001, then tabled compound type must be
I (internal standard)
21 Mass to charge ratio (M/Z)
21.1 Must be present
21.2 Format: NNN
21.3 Range:
21.3.1 Volatile: 20-250
21.3.2 Semi-volatile: 35-450
21.4 Must equal tabled value for compound (Table 4)
22 Scan number
22.1 Must be present
22.2 Format: NNNN
22.3 Range (retention time/scan):
22.3.1 Volatile: no greater than 3.00
22.3.2 Semi-volatile: no greater than 1.00
22.4 Test performed on internal standard
23 Retention time
23.1 Must be present
23.2 Must be within range of tabled value for compound (Table 50)
24 Reference compound
24.1 Must be present
24.2 Must be numeric
24.3 If compound number is 001-299, 500-699, or 900-1000, reference
compound number must be number for an internal standard
24.4 If compound number is 300-429 or 700-829, reference compound
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number must be:
24.4.1 Compound number minus 100 for numbers in range of 300-499
and 700-799
24.4.2 Compound number minus 300 for numbers in range of 400-429
24.4.3 Compound number minus 400 for numbers in range of 800-829
25 Relative retention time
25.1 Must be present
25.2 Format: MMM:SS M=minutes S=seconds
25.3 Must be within range of table value for the compound (Table 51)
26 Peak area
26.1 Must be present
26.2 Format: NNNNN
26.3 Must be within range of table value for the compound (Table 52)
27 Amount
27.1 Must be present
27.2 Format: NNNNNNN.NNNNN
27.3 Must be within range of tabled value for the compound (Table 53)
27.4 For quan report types EPA, labeled compounds (compound numbers
201-299 and 600-699), amount must be greater than 10 and less than
401.
27.5 For quan report types BLK, amount for all pollutants (compound
numbers 001-088, 301-388, 500-599, 700-799, and 900-1000), must be
less than 10
28 Unit of measure
28.1 Must be present
28.2 Format:
28.2.1 Volatiles: UG/L
28.2.2 Semi-volatiles: UG/ML
Rev: 30 Dec 86
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29 Retention time (library)
29.1 Must be present
29.2 Must be within range of tabled value for the compound (Table 50)
29.3 No test on quan report type CAL
30 Relative retention time (library)
30.1 Must be present
30.2 Must be within range of tabled value for the compound (Table 51)
30.3 No test on quan report type CAL
31 Amount (library)
31.1 Must be present
31.2 Must be within range of tabled value for the compound (Table 53)
31.3 No test on quan report type CAL
32 Response factor
32.1 Must be present
32.2 Must be within range of tabled value for the compound (Table 54)
32.3 No test on quan report type CAL
33 Response factor (library)
33.1 Must be present
33.2 Must be within range of tabled value for the compound (Table 54)
33.3 No test on quan report type CAL
U s. Environmental
Rev: 30 Dec 86
E-340
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