Preparation of a
U.S. EPA Region 9 Sample Plan
for
EPA-Lead Superfund Projects
Quality Assurance Management Section
U.S. EPA, Region 9
November, 1992
(Document Control No. 9QA-05-92)
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CONTENTS
Page
Introduction 1
Required Sections 2
Section I - Objective 3
Section II - Background 3
Section III - Maps 3
Section IV - Rationale 3
Section V - Request for Analysis 4
Section VI - Field Methods and Procedures 7
A) Sample Collection 8
B) Disposal of Contaminated Materials 9
C) Equipment Decontamination 9
D) Sample Containers 9
E) Sample Preservation 10
F) Sample Packaging and Shipment 10
G) Sample Documentation 11
H) Quality Control Samples 11
Section VII - Health and Safety Plan 13
Bibliography 14
APPENDICES
Appendix A.
Appendix B.
Appendix C.
Appendix D.
Appendix E.
Appendix F.
Environmental Services Branch Referral List
Field Investigation Flow Chart
Sample Plan Cover Sheet
CLP Target Compound List and Quantitation Limits
SAS Client Request Form SOP and Examples
Request for Analysis Example Table
Sample Container Requirements for CLP Analyses
Sample Holding Times, Treatment and Preservation
for RAS and Common SAS Analyses
Appendix G. U.S. EPA Region 9 CLP Paperwork Instructions
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INTRODUCTION
* The purpose of the Sample Plan is to document all field and
laboratory activities associated with a sampling effort.
The Sample Plan is used by field personnel as a reference
during sampling, and is used by EPA Quality Assurance
Management Staff to contract for laboratory analyses.
This guidance document describes the requirements for con-
tractors and EPA staff preparing Sample Plans for EPA-lead
projects. These requirements, with or without modification,
may also apply to other sampling projects EPA is involved
with, such as split sampling at PRP-lead projects and
State-lead projects that use the CLP. A separate document,
Preparation of a U.S. EPA Region 9 Sample Plan for Private
and State Lead Projects, is available for projects not led
by EPA.
This Sample Plan guidance has been prepared by the EPA
Quality Assurance Management Section (QAMS). Questions on
the guidance or on site specific field or laboratory con-
cerns should be directed to QAMS staff listed in Appendix A.
Some general guidelines and information on Sample Plan
preparation are listed below.
* The Sample Plan is a "stand alone" document. DO NOT INCLUDE
IT AS PART OF ANY OTHER DOCUMENT!11
* The Regional guidelines for preparing Sample Plans and QA
Project Plans (QAPjPs) are designed to minimize overlap be-
tween the two documents. As a result, some QAPjP elements
which are also required in the Sample Plan may be addressed
in the QAPjP by reference. The Sample Plan, however, may
not reference field procedures in the QAPjP or any other
document, except as background information.
* Separate Sample Plans must be prepared for every sampling
episode. An exception may be granted to Sample Plans for
periodic monitoring, such as quarterly groundwater monitor-
ing, or when a new sampling proposal involves the same tech-
niques as a previous Sample Plan. In both cases, an amend-
ment to an existing Sample Plan is required. The amendment
must outline any new sampling proposals, objectives and
rationales, and any other changes to the original plan. All
amendments must include a new request for analysis section
including the narrative, table, and SAS Client Request
Forms. Call QAMS to determine if a new Sample Plan is re-
quired or for more information on the requirements of a
Sample Plan amendment.
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* The Sample Plan is reviewed and approved by QAMS and the EPA
Remedial Project Manager. The normal turnaround times for
Sample Plan review, contracting a CLP laboratory, laboratory
analyses and data validation are provided in a flow chart in
Appendix A. Longer turnaround times may be required for
more complex sampling proposals involving unusual analytical
parameters or sample matrices, such as many air analyses or
radiochemical analyses.
* QAMS will also review and approve the locations and con-
struction details for new monitoring wells. In order to ex-
pedite the construction phase of the project, the informa-
tion on new wells can be provided for review in a separate
document, such as the work plan or 2APP. Allow two weeks
for the review and time for any revisions. (Also see Sec-
tion VI.)
* See page 14 for a bibliography of useful references for
preparing a Sample Plan.
REQUIRED SAMPLE PLAN SECTIONS
COVER SHEET (EPA format required)
Section I
Section II
Section III
Section IV
Section V
OBJECTIVE
BACKGROUND
MAPS
RATIONALE FOR SAMPLE LOCATIONS, NUMBERS OF
SAMPLES, AND ANALYTICAL PARAMETERS
REQUEST FOR ANALYSIS
(Narrative and Table required)
Section VI - FIELD METHODS AND PROCEDURES
A) Sample Collection (including well construction)
B) Disposal of Contaminated Materials
C) Equipment Decontamination
D) Sample Containers
E) Sample Preservation
F) Sample Packaging and Shipment
G) Sample Documentation
H) Quality Control Samples
Section VII - SITE SAFETY PLAN
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SAMPLE PLAN REQUIREMENTS
COVER SHEET (EPA format is REQUIRED)
* The cover sheet is a record of the review and approval of
the Sample Plan. A copy of the required format is included
in Appendix B.
I OBJECTIVE
* State the objectives of the sampling proposal. Discuss why
the sampling is being proposed and how the data will be
used. State the general analytical information needed from
the site. Provide detailed objectives; do not just state
the obvious.
II BACKGROUND
* Give a concise history of contamination at the site. Dis-
cuss activities that resulted in contamination, what is
known about the location and extent of contamination, and
past and on-going site investigations. Include site infor-
mation and data that are relevant to the proposed sampling,
such as hydrogeology, topography, precipitation, wind direc-
tion, surface water, etc.. Summarize significant analytical
results from past investigations, and discuss unusual
analytical parameters or special methods used, if any.
III MAPS
* Maps should contain all sampling points, known and potential
contamination sources, directions of surface water and
groundwater flow, site boundaries, on-site buildings, and
any other relevant information. More than one map is often
needed to illustrate all the required information. Draw
maps to scale, if possible, or include in the background
section a discussion of the size of the site and the size of
any significant on-site features. Include a map showing the
location of the site in a county or state.
IV RATIONALE FOR SAMPLE LOCATIONS. NUMBERS OF SAMPLES.
& ANALYTICAL PARAMETERS
* This section describes in detail how the Sample Plan will
meet the stated objectives. It covers the what, where and
why of the Sample Plan as discussed below.
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Give a general description of where samples will be col-
lected and the types of matrices that will be sampled. Ex-
plain the rationale for each sampling point, the total num-
ber of sampling points, and any statistical approach used to
select these points. Discuss if sampling points were
selected with a random, judgmental, or systematic approach,
or a combination of these. If some possible sampling points
(e.g., specific wells) are excluded, explain why.
Discuss the rationale for the analytical parameters. The
rationale must relate to site history and the objectives of
the Sample Plan. Justify requests for low quantitation
limits. Give an explanation when not all samples from the
same matrix will be analyzed for the same parameters. Iden-
tify site indicator compounds and other parameters of most
interest. Discuss relevant action levels, especially when
low quantitation limits are required.
Discuss the rationale for using a mobile field laboratory or
any other non-CLP laboratory. Describe where samples for
these laboratories will be collected, if possible, or state
the method that will be used in the field to locate these
samples. Explain how screening data will be used, such as
how it will be used to select samples for analysis at a CLP
or other fixed laboratory. Usually a percentage of all
samples for screening analysis should be split with a
fixed/CLP laboratory to verify the accuracy and precision of
field analytical techniques.
Justify fast turnaround time requests for CLP laboratory
analyses.
REQUEST FOR ANALYSES (Tabular and Narrative)
This section provides information necessary for obtaining
analytical services through EPA's Contract Laboratory
Program (CLP) and/or from a non-CLP laboratory.
CLP analyses will be either Routine Analytical Services
(RAS), or Special Analytical Services (SAS), or a combina-
tion of these two analytical services (RAS+SAS).
Under the RAS program, five types of analyses are available
for soil and/or water matrices: volatiles, semivolatiles,
pesticides/PCBs, 2,3,7,8-TCDD (dioxin), metals, and cyanide.
The compounds included in the RAS analyses are on the CLP
Target Compound List (TCL). Appendix C lists all compounds
on the TCL, and the contract required quantitation limits
(CRQLs). The Hazardous Substance List (HSL) and Priority
Pollutant List (PPL) are NOT identical to the TCL compound
list.
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SAS analyses include all non-routine (i.e., non-RAS)
analytical methods, and non-routine sample matrices (air,
wastes, oil, etc.). RAS+SAS analyses are modifications to
the RAS procedures such as fast turnaround times, different
QC requirements, or different sample preparation techniques.
All high concentration samples (>10% contamination) are SAS.
A fixed contract is available for analysis of high con-
centration samples for TCL compounds.
The Sample Plan should distinguish among RAS, RAS+SAS and
SAS analyses; however, these designations may be changed by
the Regional Sample Control Coordinator (RSCC) because of
factors involved in selecting a CLP laboratory.
Narrative Request For Analyses
Begin Section V with a paragraph summarizing all laboratory
analyses to be performed for the project. This paragraph
must include the site CERCLIS identification number, an-
ticipated sampling dates, sample matrices and concentra-
tions, number of samples, and analytical procedures. Con-
cise phrases are recommended (e.g., 6 low concentration
waters for RAS Semivolatiles, RAS Metals, and SAS
Total Dissolved Solids).
A SAS Client Request Form (CRF) must be included for all
chemical analyses except RAS analyses. For each analytical
parameter or group of analytes to be measured by a single
analytical method, a SAS CRF must be submitted following the
format outlined in the Standard Operating Procedure (SOP)
for the Completion of SAS CRFs, 11/12/92. (See Appendix D
for this SOP and example CRFs.) Generally, the SAS CRFs
should be submitted as an appendix to the plan. These SAS
CRFs will be copied directly from the plan and submitted to
the Sample Management Office (SMO) to request lab space.
Each individual CRF must be independent and separable.
The SAS CRFs are required by the SMO for all SAS analyses in
the CLP. The SAS CRF must clearly identify all technical
requirements AND contractual requirements. It will serve as
the statement of work for the analytical service. The lan-
guage and requirements must be explicit. (See Appendix D.)
QAMS has prepared SAS CRFs for the most commonly requested
SAS procedures. A current list of these "Generic" SAS CRFs
is available upon request. Contact QAMS to obtain copies of
the Generic SAS CRFs needed for a sampling event. To limit
the use of outdated SAS CRFs, the CRFs will not be dis-
tributed in compendium form. Always contact QAMS to ensure
a previously used CRF (e.g., for quarterly monitoring) is
still the most recent revision for a particular analysis.
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QAMS will also maintain a file of SAS CRFs written by sample
plan authors for specific sampling events. These specific
CRFs will have been reviewed by QAMS and will be available
as a reference to plan authors with similar analytical
needs.
After obtaining a Generic SAS CRF, review it to make sure
all sections are applicable to your project. Changes to the
Generic SAS CRF are acceptable, but MUST be readily iden-
tifiable (i.e., written in purple felt tip marker). If the
form has been modified, mark the appropriate box in the up-
per right hand corner of the first page of the CRF. Do NOT
retype the text of Generic CRFs to include your changes.
This will significantly increase the review time and may
delay the scheduling of samples with the CLP.
If a Generic SAS CRF is directly applicable, simply complete
the site specific sections (header sections D, E, and F and
analytical sections 2, 3, 4, and 11). These sections should
be handwritten in contrasting ink.
If a Generic SAS CRF is not available for a specific
analysis, a CRF must be prepared and submitted with the plan
for review. The CRF must be in exactly the format described
in the SOP located in Appendix D and must present all infor-
mation to the same degree of complexity demonstrated by the
examples. The "SAS Compendium" format used previously for
SAS requests will no longer be acceptable. Incomplete or
poorly prepared SAS CRFs will not be accepted by SMO and may
delay procurement of lab space and, therefore, the sampling
event.
New SAS CRFs should be clearly labeled "DRAFT" until the
review has been completed. Each page of a CRF must be dated
and numbered.
New SAS CRFs must be submitted well in advance of the sam-
pling event. A minimum of six weeks is required for review
and lab procurement. Complicated or unusual analytical pro-
cedures may take longer.
All chemical measurements made in the field, including pH
and electrical conductivity, must be described using the ap-
plicable information discussed in the SOP for SAS CRFs.
This includes: Matrix; Analytical Procedure; Hold Times;
Calibration Procedures and Criteria; Quality Control Checks,
Control Limits, and Corrective Action; Reporting Units; and
Documentation.
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B. Request For Analyses Table (See Appendix D for an example)
* List all analytical parameters on a sample by sample basis
in a tabular format. Include a separate table for each
matrix.
* List the container types, sample volumes, preservatives,
special handling and analytical holding times for each
parameter.
* List all QC samples (blanks, backgrounds, duplicates, lab QC
samples and splits). If extra volume is needed for lab QC
samples this must be included. (See Section VI - H.)
* Include at least a weekly sampling schedule, and total the
number of samples and analyses on a weekly basis. Include
duplicates and blanks in the totals.
* Our table format (see Appendix D) does not fit all sampling
schemes and is for guidance. Your modified version must in-
clude all of the information requested on our form. Call
the RSCC for a copy of the Lotus file containing our table.
VI FIELD METHODS AND PROCEDURES
Standard Operating Procedures for Field Methods
* Some information required in Section VI includes routine
procedures that usually vary little from site to site. To
streamline Sample Plan writing and to standardize these
routine practices, contractors are encouraged to develop
Standard Operating Procedures (SOPs) for some of these pro-
cedures .
* SOPs should be concise and focused. They should be specific
to one type of task and protocol. For example, an SOP can
be developed for sampling wells with a bailer, but one SOP
should not describe all methods of well sampling.
* The SOP must be included in the Sample Plan, preferably in-
corporated directly into the text of the appropriate sec-
tion. The SOP must be directly applicable, as written, to
the Sample Plan; if not, modifications to the SOP must be
discussed.
* SOPs are recommended for the most common sampling tech-
niques, equipment decontamination, sample packaging, sample
shipping, and field documentation.
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Sample Collection
Describe how sampling points will be selected in the field
(not required for existing wells), and how sampling points
will be documented and marked for future reference. If a
grid will be used, describe how the grid will be set up.
Outline sequentially or step-by-step the procedure for col-
lecting a sample for each matrix and each different sampling
technique (including samples for mobile-lab or screening
analyses). Include well purging, housekeeping/cleanliness
techniques, field measurements, sample preservation and type
of sample equipment (including material equipment is con-
structed of). The procedures described must ensure that a
representative sample is collected, and that sample handling
does not result in cross contamination or unnecessary loss
of contaminants. Special care in sample handling required
for volatile organic samples must be addressed.
Describe the procedures for collecting mobile-lab/screening
samples separately if the procedures differ from those for
collecting CLP/fixed laboratory samples.
When wells are being constructed for sample collection,
describe the design and construction details. Include a
discussion on well development. This information may be in-
cluded as an Appendix to the Sample Plan, or in a separate
document, which must be referenced in the sample plan and
provided for QAMS to review.
To expedite well construction, the portions of the Sample
Plan describing the rationale for well locations, the
details of well construction, and relevant objectives, back-
ground information, and maps may be approved prior to ap-
proval of the entire Sample Plan. Alternatively, this in-
formation may be provided for QAMS review in a separate
document, such as a work plan or QAPP, prior to preparation
of the sample plan.
For all new and existing wells to be sampled, provide a
table of well specifications that includes at least the well
depths, casing diameters, screened intervals, and, if avail-
able, the last water level measurements. If possible, es-
timate the purge volume from existing data.
Where possible, identify those sampling points which will be
collected in duplicate or as lab QC samples.
Check to make sure that appropriate numbers of blank, back-
ground, duplicate and lab QC samples are included for each
sample matrix.
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Disposal of Contaminated Materials
Describe how contaminated cuttings, well development and
purge water, disposable equipment, decontamination water,
and any other contaminated materials will be stored or dis-
posed of.
Discuss any analyses (CLP and non-CLP) that may be required
for waste disposal purposes.
Drummed wastes should have a label listing sources of the
waste to insure appropriate disposal.
Equipment Decontamination
The following is an EPA Region 9 recommended generic proce-
dure for decontamination of sampling equipment:
1) Wash with non-phosphate detergent
2) Tap-water rinse
3) 0.1N nitric acid rinse (when cross contamination from
metals is a concern)
4) Deionized/distilled water rinse
5) Pesticide grade solvent rinse (when semivolatile and
non-volatile organic contamination may be present)
6) Deionized/distilled water rinse (twice)
7) Organic free water rinse (HPLC grade)
A different procedure may be used. Give the rationale for
your approach.
Do not use a TCL volatile compound, such as acetone, for the
solvent rinse when volatile organic analyses are required.
Describe how drilling equipment will be cleaned.
Whenever possible, obtain sets of sampling tools so that
decontamination can be done in batches, preferably just once
a day at the start or end of a sampling day. This will min-
imize the number of blanks needed.
Sampling equipment must never be reused without first being
decontaminated.
Sample Containers
Describe the type, size and source of containers used for
each analytical parameter. The request for analysis table,
if complete, can be referenced for most of this information.
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Appendix E identifies the containers and volumes which are
required for CLP RAS analyses. Containers provided by the
CLP should not be rinsed before sampling.
For SAS analyses, collect at least twice the minimum volume
required by the analytical method (see Appendix F). In some
cases, a special type of container is required for SAS
analyses. If soil samples will be collected and shipped in
metal sleeves, please contact QAMS for information regarding
the necessary sample volume. A separate sleeve may be re-
quired for each analysis.
If containers are obtained from outside the CLP bottle con-
tract (e.g., metal sleeves for soil sampling), describe how
the containers will be cleaned.
Sample Preservation
Describe the preservation methods that will be used. See
Appendix F for some common preservation requirements.
The preservatives used must be indicated on the sample con-
tainer and on the paperwork.
Region 9 requires acidification of low and medium concentra-
tion water samples for volatile organic analyses, including
analyses such as EPA Method 601. (See Appendix F.)
Sample Packaging and Shipment
Describe how samples will be packaged and shipped. Include
the method of shipment and the shipping schedule. Do not
ship samples as baggage on passenger planes. It is against
Department of Transportation (DOT) regulations.
If medium (>10ppm) or high (>10%) concentration samples will
be shipped, special packaging and DOT labeling requirements
must be described. IT IS THE CONTRACTOR'S RESPONSIBILITY TO
MEET DOT SHIPPING REGULATIONS. EPA staff are generally not
familiar with DOT regulations.
All sample shipments must be reported to the RSCC within one
day after shipment. Friday shipments of samples must be
coordinated with the RSCC by noon on Friday to arrange for
Saturday delivery at the laboratory.
Appendix G includes analytical and CLP contract holding
times for RAS and common SAS parameters. These holding
times should be considered when developing sampling and
shipping schedules. For SAS analyses, the contract holding
time will usually be two days less than the analytical hold-
ing time.
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Sample Documentation
Discuss the use of all paperwork, including field notebooks,
record logs, photographs, CLP sample paperwork, Field QC
Summary Forms, and Chain of Custody forms and seals.
Describe the entries that should be made to the field
notebook.
Include a copy of Appendix G, CLP Paperwork Instructions, as
an appendix to your Sample Plan.
Describe how sample bottles will be labeled. At a minimum,
each bottle must include the CLP sample number, CLP Case
and/or SAS number, station location, analytical parameters,
date sampled, and any preservative added to the sample.
Quality Control Samples
Duplicates (including splits)
Duplicates are a check on laboratory and field procedures.
Collect duplicates at a frequency of 1 sample per week or
10% of all field samples, whichever is greater, for all
parameters and matrices. Duplicates should be from sampling
points which are known or suspected to be contaminated.
Identify the sampling points for duplicates, if known, or
explain how a location will be selected for duplicate
samples.
For large projects, duplicates should be spread out over the
entire site and collected at regular intervals. For ex-
ample, duplicates should usually not be collected from just
one soil boring.
Duplicates are collected, numbered, packaged, and sealed in
the same manner as other samples; a duplicate sample pair is
assigned two separate CLP sample numbers and station loca-
tion numbers, and submitted blind to the laboratory.
Describe how duplicates will be collected. The collection
procedure must insure that duplicates are as similar as pos-
sible.
When sampling soil with sleeves, duplicates should be col-
lected as collocated sleeves by selecting two adjoining
sleeves from the same split spoon. Alternatively, when
volatiles are not a concern, the sample can be homogenized
in a container and then split into separate bottles.
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A discussion of splits must be included when a PRP may re-
quest samples, or when it is necessary to determine the
precision and/or accuracy of field analytical methods by
splitting a percentage of samples with a fixed laboratory.
The sample collection procedures should be identical to col-
lecting duplicates.
Blank Samples
Blank samples are required for water and air sampling. Col-
lect at least one blank per day for each parameter.
Blank samples are a check for cross-contamination during
sample collection and shipment, and in the laboratory. Use
analytically-certified organic-free (HPLC-grade) water for
organic parameters. Use metal-free (deionized-distilled)
water for inorganic parameters.
Blanks are collected, numbered, packaged, and sealed in the
same manner as other samples, and submitted blind to the
laboratory.
Describe how and when blank samples will be collected.
Only one type of blank need be collected. Blanks are listed
below in order of collection preference.
a. Equipment Blank
An equipment blank should be collected when sampling equip-
ment is decontaminated and reused in the field or when a
sample collection vessel (e.g., a bailer or beaker) will be
used. Use the appropriate "blank" water identified above to
fill or rinse the sampling equipment after the equipment has
been decontaminated, and pour or collect this water in the
sample containers.
b. Field Bottle Blank
Collect this type of blank when equipment decontamination is
not necessary and when a sample collection vessel will not
be used (e.g., with dedicated pumps). The field bottle
blank should be poured at a sampling point. Use the ap-
propriate "blank" water identified above to fill the sample
bottles.
c. VOA Travel Blank
Collect a VOA travel blank when there is no other type of
blank for volatiles. All of the VOA vials should be shipped
in the same cooler as the VOA travel blank.
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3. Background Samples (air, soil & surface water)
* Background samples should be analyzed for the complete set
of parameters for each matrix; treat sediments, surface
soils and subsurface soils as separate matrices. Background
samples are collected, numbered, packaged, and sealed in the
same manner as other samples.
* For long term and/or especially large projects, it is recom-
mended that 10% of samples collected be from background
locations.
4. Lab QC Samples
* Select one field sample per week or 1 per 20 samples
(including blanks and duplicates), whichever is greater, and
designate this sample as the "lab QC sample". The lab QC
sample is not an additional sample; it is a special designa-
tion for an existing sample. The laboratory will use this
sample for lab duplicate and matrix spike analyses.
* Lab QC samples should be selected from sampling points which
are suspected to be moderately contaminated.
* Label the bottles and all copies of the paperwork as "lab QC
sample"; the laboratory must know that this sample is for
their QC analyses.
* The first lab QC sample of the sampling effort should be
part of the first or second day's shipment. Subsequent lab
QC samples should be spread out over the entire sampling ef-
fort.
* For water matrices, the lab QC sample must be a double
volume sample; i.e., twice as many bottles as a normal
sample. See Section VI - D for normal sample volume re-
quirements. Additional volume is not necessary for soil
samples.
VII SITE SAFETY PLAN
* Must be approved by the Health & Safety Officer of the or-
ganization doing the field work. It does not have to follow
EPA Region 9 format.
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Bibliography of useful references for preparing a Sample Plan.
A Compendium of Superfund Field Operation Methods. EPA 540/P-
87/001a & 001b, August 1987.
Data Quality Objectives for Remedial Response Activities, two
volumes, EPA 540/G-87/003 and 1004, March 1987.
Field Screening Methods Catalog User's Guide. EPA Office of Emer-
gency and Remedial Response, EPA/540/2-88/005, September 1988.
Handbook for Sampling and Sample Preservation of Water and Was-
tewater . EPA—600/4-82—029, September 1982.
Methods for Chemical Analysis of Water and Wastes. US EPA EMSL
Cincinnati, EPA-600/4-79-020, March 1983.
Practical Guide for Ground-Water Sampling. EPA 600/2-85/104, Sep-
tember 1985.
Preparation of Soil Sampling Protocol: Techniques and
Strategies. EPA 600/4-83-020, August 1983.
A Rationale for the Assessment of Errors in the Sampling of
Soils. US EPA EMSL Las Vegas, EPA/600/4-90/013, May 1990.
RCRA Ground-Water Monitoring Technical Enforcement Guidance Docu-
ment. U.S. EPA Office of Waste Programs Enforcement, September
1986.
Soil Sampling Quality Assurance User's Guide. EPA 600/4-84-043,
May 1984.
Standard Methods for the Examination of Water and Wastewater.
American Public Health Association, 17th Edition, 1989.
Test Methods for Evaluating Solid Waste. Physical and Chemical
Methods Manual. SW-846. two volumes, 3rd Edition, U.S. EPA Office
of Solid Waste and Emergency Response, November 1986.
User/s Guide to the Contract Laboratory Program. U.S. EPA Office
of Emergency and Remedial Response, December 1988.
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APPENDIX A
Environmental Services Branch
Referral List
and
Field Investigation Flow Chart
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ESB REFERRAL LIST
December 1992
Environmental Services Branch (ESB) P-3
(415) 744-1523
i Qhoratory Support Section (LSS) P-3-1
(415)744-1491
lity Assurance Management Section (QAMS) P-3-2
(415)744-1492
SUBJECT
CONTACT
PRIMARY CONTACT LISTED FIRST
TELEPHONE
4 Air Methods
James Whittaker/Steve Remaley
(702)798-2155/744-1527
~ Alternate Test Procedures (ATP)
Tina Diebold/Robbie Hedeen
744-1528/1535
* Asbestos
Kent Kitchingman
744-1492
4 Atomic Absorption (AA)
Hedy Ficklin/Pat Mack
744-1497/(702)798-2117
Tina Diebold
744-1528
* Bkmsays/Toxicity Tests
Peter Husby/Clarice Olson/Hedy Ficklin
744-1488/1489/1497
Marine Toxicity Tests:
Amy Wagner/Peter Husby
744-1495/1488
4 Bioassessments/Ecoassessments
Peter Husby/ Stewart Simpson/Amy Wagner
744-1488/1487/1495
4 Contract Laboratory Program (CLP)
General Information:
Steve Remaley
744-1527
Scheduling Analyses:
Roseanne Sakamoto
744-1536
Special Analytical Services(SAS) Requests
Hedy Ficklin
744-1497
4 Data Quality Objectives (DQO)
Hedy Ficklin/Kira Lynch
744-1497/1496
Non-$F
Rose Fong
744-1534
4 Data Review/Va]idation Procedures
Steve Remaley/Tina Diebold/Hedy Ficklin/Kira Lynch
744-1527/1528/1497/1496
* Data Review Project Status
Roseanne Sakamoto
744-1536
* Detection Limits
Tina Diebold/Steve Remaley
744-1528/1527
* Dioxin
Jim Johnson/Steve Remaley
744-1494/1527
* DMR-QA PE Studies
Tina Diebold/Roseanne Sakamoto
744-1528/1536
* DMR-QA Toxicity
Amy Wagner
744-1495
* DMR-QA Follow-up Inspections
Peter Husby
744-1488
4 Drinking Water Methods
Jim Johnson/Rose Fong
744-1494/1534
* Drinking Water Labs
Pat Mack/Clarice Olson
(702)798-2117/744-1489
~-Environmental Monitoring Methods Index (EMMI)
Jim Johnson/Hedy Ficklin
744-1494/1497
|P Lab
Brenda Bettencourt
744-1491
id Audits/QA
Robbie Hedeen/Kira Lynch
744-1535/1496
4 Field Sampling Plan (FSP) Preparation
Robbie Hedeen/Hedy Ficklin/Kira Lynch
744-1535/1497/1496
4 Fuels Analyses
Hedy Ficklin
744-1497
* Gas Chromatography/Mass Spectrometry (GC/MS)
Steve Remaley/Jim Johnson
744-1527/1494
~GIS
Kathy Baylor/Roseanne Sakamoto
744-1490/1536
* Global Positioning System
Kathy Baylor
744-1490
~ HRS - Site Assessment
Kira Lynch
744-1496
4 Inductively Coupled Plasma (ICP)
Tina Diebold/Jim Johnson
744-1528/1494
4 Inorganic Methods
Pat Mack/Tina Diebold/Hedy Ficklin
(702)798-2117/744-1528/1497
4 Ion Chromatography (IC)
Jim Johnson/Tina Diebold
744-1494/1528
4 Laboratory Audits
Steve Remaley
744-1527
4 Laboratory Certification - Chemistry
Jim Johnson/Pat Mack
744-1494/(702)798-2117
4 Laboratory Certification - Microbiology
Clarice Olson/Jim Johnson/Pat Mack
744-1489/1494/(702)798-2117
~ Management System Reviews (MSR)
Kent Kitchingman/Rose Fong
744-1492/1534
4 Metals
Tina Diebold/Hedy Ficklin/Pat Mack
744-1528/1497/(702)798-2117
4 Mobile Lab Services
Brenda Bettencourt
744-1491
4 Microbiology
Pat Mack/Ctarice Olson/Hedy Ficklin
(702)798-2117/744-1489/1497
4 Non-Superfund Analytical Services
Stewart Simpson
744-1487
4 Organic Methods
Steve Remaley/Jim Johnson/Hedy Ficklin
744-1527/1494/1497
4 Pesticides
Steve Remaley/Jim Johnson/James Whittaker
744-1527/1494/(702)798-2117
4 PCBs
Jim Johnson/Steve Remaley
744-1494/1527 '
4jtnd10nuclides
Jim Johnson/Steve Remaley
744-1494/1527
[ty Assurance
Kent Kitchingman/Hedy Ficklin/Kira Lynch
744-1492/1497/1496
Project Plan (QAPjP) $F Preparation
Hedy Ficklin/Kira Lynch
744-1497/1496
Non-$F
Rose Fong
744-1534
* Quick Turnaround Method (QTM)
Hedy Ficklin
744-1497
4 Sample Holding Times/Preservation/Containers
QAMS Staff
744-1523
-------
SUBJECT
* Sampling: Drinking Water
Soil/Sediment
Groundwater
Surface Water
NPDES/Sludge
Fish
Waste (Solid)
Microbiology/Virology
* Total Quality Management (TQM)
• Toxicity Charateristic Leaching Procedure (TCLP)
~ Water Pollution PE Studies (WP)
~ Water Supply PE Studies (WS)
CONTACT
PRIMARY CONTACT LISTED FIRST
Clarice Olson/Kira Lynch
Stewart Simpson/Kathy Baylor/Kira Lynch
Robbie Hedeen/Kathy Baylor/Kira Lynch
Peter Husby/Stewart Simpson/Kathy Baylor
Peter Husby/Stewart Simpson
Stewart Simpson/Peter Husby
Tina Diebold/Stewart Simpson
Clarice Olson
Kent Kitchingman
Steve Remaley/Hedy Ficklin/Stewart Simpson
Roseanne Sakamoto/Tina Diebold
Roseanne Sakamoto/Tina Diebold
TELEPHONE
744-1489/1496
744-1487/1490/1496
744-1535/1490/1496
744-1488/1487/1490
744-1488/1487
744-1487/1488
744-1528/1487
744-1489
744-1492
744-1527/1497/1487
744-1536/1528
744-1536/1528
ADDITIONAL REFERENCES:
Region 9 Public Inquiry Response Line
Region 9 Library Reference Desk
Region 9 RCRA Information Hotline
(415)744-1500
(415)744-1510
(415) 744-2074
Methods Information Communication Exchange (MICE)
RCRA/Superfund Hotline
(703) 821-4789
(800) 424-9346
EMSL-CI main receptionist
EMSL-CI Chemistry Research Div.
EMSL-CI QA Research Div.
EMSL-LV main receptionist
EMSL-LV QA Research Div.
(513) 569-7301
(513) 569-7586
(513)569-7325
(702) 798-2100
(702)798-2103
Inspector General's Whistleblower Hotline
(800) 424-4000
Government Printing Office (GPO)
National Technical Information Service (NTIS)
EPA Documents (CERI)
Federal Register articles (available for fee)
(202) 783-3238
(800) 553-NTIS
(513) 569-7562
(202) 523-5240
Federal Express
(800)238-5355
American Samoa EPA
(684)633-2304
AZ Dept. of Environmental Quality
AZ Dept. of Health Services
<
(602) 207-2300
(602)542-1000
CA Dept. of Health Services
CA Air Resources Board
CA State Water Resources Control Board
(916)445-4171
(800) 242-4450
(916) 657-2390
Guam EPA
(671) 646-8863
HI Dept. of Health Services (personnel)
HI Environmental Planning Office
(808) 548-6588
(808) 543-8335
NV Dept. of Health Services
NV Division of Environmental Protection
(702)687-4740
(702) 687-4670
Northern Mariana Islands Env. Quality Division
(670)234-6984
-------
FIELD INVESTIGATION FLOW CHART
Sample Plan Author-
J
revision required
A
Remedial Project Manager (RPM)
I
Quality Assurance Management Section (QAMS)
Sample Plan Approved
Regional Sampling Control Center (RSCC)
CLP Labs Contracted
Sampling Begins
jiii i
Lab Analyses
I
Data Validation
Allow 14 days *
for review of
each draft
7 days for RAS
21 days for SAS
35 days *
25 days
* Turnaround times indicated are routine.
Fast turnaround is also available for special cases.
Fast turnaround must be justified and approved.
NOTE: Sample plans should be submitted two months prior
to anticipated sampling date. This allows adequate
time for review, revision, and scheduling lab space
for most routine sampling events.
-------
(11/92)
APPENDIX B
Sample Plan Cover Sheet
-------
(11/92)
U.S. ENVIRONMENTAL PROTECTION AGENCY REGION 9
Sample Plan Title:
Site Name:
Site Location:
City/State/Zip:
Site EPA ID #:
Anticipated Sampling Dates:
Prepared by:
Date
Agency or Firm:
Address:
City/State/Zip:
Telephone: _( )
EPA Project Manager: Section:
Phone #
QAPjP Approval Date:
S (for EPA use) S
U U
P P
E Received by Superfund Remedial Project Manager: E
R Date R
F Reviewed by: F
U Date U
N APPROVED / NOT APPROVED N
D D
Expedited Review? Yes/No
Received by Quality Assurance Management Section:
Q Date Q
A Reviewed by: A
M Date M
S S
APPROVED:
Chief, Quality Assurance Date
Management Section
Environmental Services Branch, OPM
-------
APPENDIX C
CLP Target Compound List
and
Quantitation Limits
-------
TARGET COMPOUND LIST (TCL) AND CONTRACT REQUIRED QUANTITATION LIMITS (CRQL)
Volatiles
1. Chloromethane
2. Bromoraethane
3. Vinyl Chloride
4. Chloroethane
5. Methylene Chloride
6. Acetone
7. Carbon Disulfide
•8. 1,1-Dichloroethene
9- 1,1-Dichloroethane
10. 1,2-Dichloroethene (total)
Quantitation Limits*
Low Med.
Water Soil Soil
CAS Number ug/L ug/Kg uq/Kg
74-87-3
10
10
1200
74-83-9
10
10
1200
75-01-4
10
10
1200
75-00-3
10
10
1200
75-09-2
10
10
1200
67-64-1
10
10
1200
75-15-0
10
10
1200
75-35-4
10
10
1200
75-34-3
10
10
1200
540-59-0
10
10
1200
11. Chloroform
12. 1,2-Dichloroethane
13. 2-Butanone
14. 1,1,1-Trichloroethane
15. Carbon Tetrachloride
67-66-3
10
10
1200
107-06-2
10
10
1200
78-93-3
10
10
1200
71-55-6
10
10
1200
56-23-5
10
10
1200
16. Bromodichloromethane
75-27-4
10
10
1200
17. 1,2-Dichloropropane
78-87-5
10
10
1200
18. cis-1,3-Dichloropropene
10061-01-5
10
10
1200
19. Trichloroethene
79-01-6
10
10
1200
20. Dibromochloromethane
124-48-1
10
10
1200
21. 1,1,2-Trichloroethane
79-00-5
10
10
1200
22. Benzene
71-43-2
10
10
1200
23. trans-1,3-Dichloropropene
10061-02-6
10
10
1200
24. Bromoform
75-25-2
10
10
1200
25. 4-Methyl-2-pentanone
108-10-1
10
10
1200
26. 2-Hexanone
591-78-6
10
10
1200
27. Tetrachloroethene
127-18-4
10
10
1200
28. Toluene
108-88-3
10
10
1200
29. 1,1,2,2-Tetrachloroethane
79-34-5
10
10
1200
30. Chlorobenzene
108-90-7
10
10
1200
31. Ethyl Benzene
100-41-4
10
10
1200
32. Styrene
100-42-5
10
10
1200
33. Xylenes (Total)
1330-20-7
10
10
1200
* Quantitation limits listed for soil/sedimenc arc based on wet weight. The
quantitation limine oalculated by the laboratory for soil/s&ciiment,
calculated on dry weight basis as required by the contract, will be higher.
-------
Target Compound List (TCL) and
Contract Required Quantitation Limits (CRQL)*
Quantitation Limits**
Semlvdlatlles
CAS Number
Water
ug/L
Low Soil/Sedimentb
ur/Kr
35.
Phenol
108-95-2
10
330
36.
bi6(2-Chloroethyl) ether
111-44-4
10
330
37.
2-Chlorophenol
95-57-8
10
330
38.
1,3-Dichlorobenzene
541-73-1
10
330
39.
1,4-Dichlorobenzene
106-46-7
10
330
40.
Benzyl alcohol
100-51-6
10
330
41.
1,2-Dichlorobenzene
95-50-1
10
330
42.
2-Methylphenol
95-48-7
10
330
43.
bls(2-Chloroisopropyl)
ether
108-60-1
10
330
44.
4-Methylphenol
106-44-5
10
330
45.
N-Nitroso-di-n-
dipropylamine
621-64-7
10
330
46.
Hexachloroethane
67-72-1
10
330
47.
Nitrobenzene
98-95-3
10
330
48.
Isophorone
78-59-1
10
330
49.
2-Nitrophenol
88-75-5
10
330
50.
2,4-Dimethylphenol
105-67-9
10
330
51.
Benzoic add
65-85-0
50
1600
52.
bis(2-Chloroe thoxy)
methane
111-91-1
10
330
53
2,4-Di chlorophenol
120-83-2
10
330
54.
1,2,4-Trichlorobenzene
120-82-1
10
330
55.
Naphthalene
91-20-3
10
330
56.
4-Chloroaniline
106-47-8
10
330
57.
Hexachlorobutadlene
87-68-3
10
330
58.
4-Chloro-3-me thylphenol
(para-chloro-meta-cresol)
59-50-7
10
330
59.
2-Methylnaphthalene
91-57-6
10
330
60.
Hexachlorocyclopentadlene
77-47-4
10
330
61.
2,4,6-Trichlorophenol
88-06-2
10
330
62.
2,4,5-Tri chlorophenol
95-95-4
50
1600
63.
2-Ch 1 or onaph tha le ne
91-58-7
10
330
64.
2-Nitroaniline
88-74-4
50
1600
(continued)
-------
Quantitation Limits**
Semlvolatlles
CAS Number
Water
«g/L
Low Soli/Sedliaent^"
65. Dlaethylphthalate
66. Acenaphthylene
67. 2,6-Dlaltrotoluene
68. 3-Nitroanillne
69. Aceupbtliene
70. 2,4-Dlnltrophenol
71. 4-Nitrophenol
72. Dlbenzofuran
73. 2,4-Dlnltrotoluene
74. Diethylphthalate
75. 4-Chlorophenyl-phenyl
ether
76. Fluorene
77._4-Nitroaniline
78. 4,6-Dinltro-2-methylphenol
79. N-nltrosodlphenylaalne
80. 4-Bromophenyl-phenylether
61. Hexachlorobenzene
82. Pentachlorophenol
83. Phenanthrene
84. Anthracene
131-11-3
208-96-8
606-20-2
99-09-2
83-32-9
51-28-5
100-02-7
132-64-9
121-14-2
84-66-2
7005-72-3
86-73-7
100-01-6
534-52-1
86-30-6
101-55-3
118-74-1
87-86-5
85-01-8
120-12-7
10
10
10
50
10
50
50
10
10
10
10
10
50
50
10
10
10
50
10
10
330
330
330
1600
330
1600
1600
330
330
330
330
330
1600
1600
330
330
330
1600
330
330
85. Di-n-butylphthaiate 84-74-2
86. Fluoranthene 206-44-0
87. Pyrene 129-00-0
88. Butylbenzylphchalate 85-68-7
89. 3,3'-Dlchlorobenzldlne 91-94-1
90. Benzo(a)anthracene 56-55-3
91. Chrysene 218-01-9
92. bis(2-Ethylhexyl)phthalate 117-81-7
93. Di-n-octylphthalate 117-84-0
94. Benzo(b)fluoranthene 205-99-2
10
10
10
10
20
10
10
10
10
10
330
330
330
330
660
330
330
330
330
330
(continued)
-------
Quantitation Limits**
Semlvolatlles
CAS Number
Water
"g/L
Low Soll/Sedlment'**
95. Benzo(k)fluoranthene
96. Benzo(0>pyrene
207-08-9
50-32-8
193-39-5
53-70-3
191-24-2
10
10
10
10
10
330
330
330
330
330
97. Indeno(l,2,3-cd)pyrene
98. 01benz(ath)anthracene
99. Beozo(g,h,l)perylene
^Medium Soll/Sedlment Contract Required Quantitation Limits (CRQL) for Seml-
Volatlle TCL Compounds are 60 times the Individual Low Soll/Sedlment CRQL.
~Specific quantitation limits are highly matrix dependent. The quantitation
limits listed herein are provided for guidance and may not always be achievable.
~~Quantitation limits listed for soll/sedlment are based on vet weight. The
quantitation limits calculated by the laboratory for soll/sedlment, calculated
on dry weight basis as required by the contract, will be higher.
-------
Target Compound List (TCL) and
Contract Required Quantitation Limits (CRQL)*
Quantitation Limits**
Water Low Soll/SediaentC
Pesticides/PCBs
CAS Number
uk/L
u*/K*
100. alpha-BHC
319-84-6
0.05
8.0
101. beta-BHC
319-85-7
0.05
8.0
10Z. delta-BHC
319-86-8
0.05
8.0
103. gamma-BHC (Lindane)
58-89-9
0.05
8.0
10&. Heptachlor
76-44-8
0.05
8.0
105. Aldrin
309-00-2
0.05
8.0
106. Heptachlor epoxide
1024-57-3
0.05
8.0
107. Endosulfan I
959-98-8
0.05
8.0
108. Dieldrin
60-57-1
0.10
16.0
109. 4,4'-DDE
72-55-9
0.10
16.0
110. Endrln
72-20-8
0.10
16.0
111. Endosulfan 11
33213-65-9
0.10
16.0
112. 4,4 *-DDD
72-54-8
0.10
16.0
113. Endosulfan sulfate
1031-07-8
0.10
16.0
114. 4,4'-DDT
50-29-3
0.10
16.0
115. Methoxychlor
72-43-5
0.5
80.0
116. Endrln ketone
53494-70-5
0.10
16.0
117. alpha-Chlordane
5103-71-9
0.5
80.0
118. gamma-Chiordane
5103-74-2
0.5
80.0
119. Toxaphene
8001-35-2
1.0
160.0
120. Aroclor-1016
12674-11-2
0.5
80.0
121. Aroclor-1221
11104-28-2
0.5
80.0
122. Aroclor-1232
11141-16-5
0.5
80.0
123. Aroclor-1242
53469-21-9
0.5
80.0
124. Aroclor-1248
12672-29-6
0.5
80.0
125. Aroclor-1254
11097-69-1
1.0
160.0
126. Aroclor-1260
11096-82-5
1.0
160.0
cMedium Soil/Sediment Contract Required Quantitation Limits (CRQL) for Pesticide/PCB
TCL compounds are IS time6 the individual Low Soil/Sediment CRQL.
•Specific quantitation limits are highly matrix dependent. The quantitation
limits listed herein are provided for guidance and may not always be
achievable.
••Quantitation limits listed for soil/sediment are based on wee weight. The quan-
titation Limits calculated by the laboratory for soll/sedlaent, calculated on dry
weight basis as required by the contract, will be higher.
-------
INORGANIC TARGET ANALYTE LIST^(TAL)
Contract Required
Detection Limit
Analyte (ug/L)
Aluminum
200
Antimony
60
Arsenic
10
Barium
200
Beryllium
5
Cadmium
5
Calcium
5000
Chromium
10
Cobalt
50
Copper
25
Iron
100
Lead
5
Magnesium
5000
Manganese
15
Mercury
0.2
Nickel
40
Potassium
5000
Selenium
5
Silver
10
Sodium
5000
Thallium
10
Vanadium
50
Zinc
20
Cyanide
10
(1) Subject Co the restrictions specified in the first page of Part G,
Section IV of Exhibit D (Alternate Methods - Catastrophic Failure) any
analytical method specified in SOU Exhibit D may be utilized as long as
the documented instrument or method detection limits meet the Contract
Required Detection Limit (CRDL) requirements. Higher detection limits
may only be used in the following circumstance:
If the sample concentration exceeds five times the detection limit of
the instrument or method in use, the value may be reported even though
the instrument or method detection limit may not equal the Contract
Required Detection Limit. This is Illustrated in the example below:
For lead:
Method in use — ICP
Instrument Detection Limit (IDL) — 40
Sample concentration — 220
Contract Required Detection Limit (CRDL)> — 5
-------
The value of 220 may be reported even though instrument detection limit
is greater than CRDL. The instrument or method detection limit must be
documented as described in Exhibit E.
(2) The CRDL are the instrument detection limits obtained in pure vater
that must be met using the procedure in Exhibit E. The detection
limits for camples may be considerably higher depending on Che sample
aatrix.
DIOXIN
Compound Quantitation Limits
2,3,7,8-TCDD The CLP does not have set
Quantitation Limits for dioxin.
-------
(11/92)
APPENDIX D
Standard Operating Procedure for the Completion of
Special Analytical Services Client Request Forms
and
Request for Analysis Example Tables
-------
Revision 2
Date H/12/92
Page 1 of 11
STANDARD OPERATION PROCEDURE (SOP)
FOR THE COMPLETION OF
SPECIAL ANALYTICAL SERVICES CLIENT REQUEST FORMS (SAS CRF)
AND PREPARATION OF LABORATORY QC SUMMARY REPORT FORMS
1 INTRODUCTION
1.1 The purpose of this document is to provide guidance to Region 9
clients in the preparation of Special Analytical Services (SAS)
Client Request Forms (CRFs) and Laboratory QC Summary Report
Forms. The objective of SAS is to provide high quality,
non-standard analytical services which are outside the scope of
Contract Laboratory Program (CLP) Routine Analytical Service (RAS)
Statement of Work (SOW) protocols. This document provides
guidance for completing pre-written "generic" SAS CRFs, and for
writing SAS CRFs and Laboratory QC Summary Report Forms when
"generic" forms are not available.
1.2 Background
1.2.1 Viar & Co. solicits, awards and administers regionally
prepared SAS requests as individual subcontracts on Viar's
USEPA contract for the operation of the Sample Management
Office (SMO) . The SAS CRF, when awarded, becomes the
statement of work for that specific, non-routine analytical
service contract.
1.2.2 In order to be eligible to bid on SAS contracts, the
laboratories must have previously met all the requirements
of the SAS Basic Ordering Agreement (BOA). The objectives
of the BOA are:
1.2.2.1 To provide a contract vehicle that establishes
the basic organizational and administrative
requirements for a laboratory's participation in
the SAS program.
1.2.2.2 To provide a contract agreement that contains
explicit language and requirements prior to the
performance of any SAS work.
Thus, the SAS contract consists of two parts: the
administrative and contract requirements developed by VIAR
and the technical requirements developed by the Region.
SASINSTR.SOP
-------
Revision 2
Date 11/12/92
Page 2 of 11
1.3 SAS Types - SAS requests are separated into two basic categories:
"all SAS" and "RAS + SAS".
1.3.1 An "all SAS" includes analytical parameters, detection
limits, matrices, and/or methods beyond the scope of the RAS
contracts. -These contracts may require specialized
instrumentation or analytical protocols.
1.3.2 A "RAS + SAS" request is based upon the RAS protocol, but
includes minor modifications. These are limited to:
a. faster turnaround
b. RAS methods with different QC requirements
c. modifications to portions of the RAS methods, such as
different sample preparation techniques
1.4 SAS Preparation
1.4.1 SASs need to be prepared from several different perspectives
which are described below.
1.4.2 The SAS should be capable of meeting required Data Quality
Objectives (DQOs) specified in the site's Quality Assurance
Project Plan (QAPjP).
1.4.3 The SAS should reflect the appropriateness of analytical
methodologies and data deliverables from both a technical
and contractual point of view. Data deliverables must be
specific and include all items required to perform data
validation and, if necessary, to be legally defensible.
1.4.4 Prior to preparing a SAS CRF, the client should determine if
there are pre-written "generic" SASs available which may
meet the client's current data requirements. The Region 9
Quality Assurance Management Section should be contacted for
further information on the availability of "generic" SAS
CRFs.
1.4.4.1 Clients using the "generic" SAS CRFs should
personalize them for their individual sampling
event and return the completed form(s) to QAMS
as part of the FSP. A lead time of 6 weeks is
required for the review and approval of the FSP
(3 weeks) and for th'e scheduling of laboratory
space (3 weeks).
SASIHSTR.SOP
-------
Revision 2
Date 11/12/92
Page 3 of 11
1.4.4.2 Clients using "generic" SAS CRFs must complete
Header sections D, E and F and Analytical
sections 2, 3, 4 and 11. Changes to the pre-
written portions are allowed, but must be done
in such a fashion that the changes are readily
apparent to facilitate the review process.
1.4.5 If a "generic" SAS CRF is not available, the client is
responsible for providing a complete SAS CRF. These "non-
generic" SAS CRF are to be included in the FSP and must be
approved by the Region 9 Technical Project Officer (TPO)
before the scheduling of laboratory space can begin.
Clients should allow sufficient lead time for the review and
approval process. A minimum of 8 weeks is recommended.
1.5 Scheduling
1.5.1 SASs used to support Superfund sites must be part of an
approved Field Sampling Plan (FSP) before the Regional
Sample Control Center (RSCC) coordinator can forward the
request to the SMO. The RSCC coordinator will review the
SAS CRFs in the FSP for technical clarity, quality control
requirements, and completeness and then forward them to SMO.
1.5.2 Since the SAS is a custom-made contract, it is necessary
that sufficient lead time be provided by the client in order
to secure the required analytical services. One month or
more may be required to complete the solicitation and award
of the SAS to contractor laboratories (see Sections 1.4.3.1
and 1.4.4).
2 INSTRUCTIONS FOR COMPLETING SAS CLIENT REQUEST FORMS - GENERAL
2.1 The SAS consists of the standard client request form (see
Attachment 1) and any additional attachments required to
supplement the information on the form. The SAS cannot reference
other QAPjP or FSP sections since it must be a "stand alone"
document. Supplemental information is especially important if
non-EPA methods are being requested.
2.2 All language in the SAS CRF will use the words "shall" or "must"
for directions that the contractor is required to follow. Words
such as "should" implies that the direction is not required and
may be viewed by the contractor laboratory as optional.
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2.3 Where appropriate, the SAS should include acceptable options and
alternatives. For instance, if two analytical methods will
produce the same results and are equally acceptable, include both
methods, thus allowing the contractor a choice of methods.
INSTRUCTIONS FOR COMPLETING THE HEADER PORTION, SECTIONS A - F
3.1 SECTION A - EPA Region/Client: This is always Region 9. On pre-
written "generic" SASs this section is already filled in.
3.2 SECTION B - Region Contact: ESAT RSCC Coordinator, ESAT/ICF,
(415) 882-3069. On pre-written "generic" SASs this section is
already filled in.
3.3 SECTION C - Date of Request: Leave this blank. It will be
completed by the ESAT RSCC coordinator when the request is
forwarded to SMO.
3.4 SECTION D - Site Name: Enter the complete Superfund site name.
3.5 SECTION E - City/State: Enter the city and state where the site
is located.
3.6 SECTION F - 2 Digit Superfund Site Identifier: Enter the 2 digit
Superfund site ID code.
INSTRUCTIONS FOR COMPLETING THE ANALYTICAL PORTION, SECTIONS 1-14
4.1 SECTION 1 - General description of analytical service requested:
4.1.1 Describe in one or two sentences the target parameter(s),
matrix type, general description of detection limits (e.g.,
mg/L, /ig/L, mg/Kg, etc.) and method(s) of analysis.
4.1.2 If the target parameters constitute a large number of
individual analytes, they can be described as a general
category (i.e. volatile organics) and reference made to a
table of analytes (e.g., Table 1) for the full list.
4.1.3 Justification for all fast turnaround requests must be
included here, as well as in the FSP.
¦ SOP
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4.2 SECTION 2 - Definition and number of work units ... :
4.2.1 Define the total number of field samples, including
field/trip blanks and field duplicates. Do not Include
laboratory quality control (QC) samples, such as matrix
spike/spike duplicates and laboratory method blanks. (These
will be added in later by SMO.) It is essential that an
accurate number of work units be specified since the total
will be considered the maximum allowed under this SAS
award. (Laboratories are not obligated to accept more than
the specified number of work units.)
4.2.2 The expected range of concentrations should be included, if
known. List any known or suspected contaminants and the
concentration levels at which they may be found in the
samples. Include contaminants that are not part of the
target analytes requested for this analysis. This is
critical for both laboratory safety and proper analysis of
the samples.
4.2.3 If samples are to be composited by the laboratory, this must
be stated and necessary instructions included.
4.2.4 If more than one matrix is involved, break down the totals
by matrix.
4.3 SECTION 3 - Purpose of analysis... :
4.3.1 Specify the program (i.e. Superfund, RCRA, etc.) that the
site is under.
4.3.2 Specify the phase of remediation, such as Remedial
Investigation/Feasibility Study (RI/FS), Remedial Design
(RD), etc.
4.4 SECTION 4 - Estimated date(s) of collection:
4.4.1 List the dates that the sampling is expected to cover. For
a sampling lasting more than a few days, include a schedule
listing the dates on which sampling will take place and the
number of samples to be collected and shipped on each
sampling date.
4.4.2 The shipping dates, once set at the time of contract award,
limits the obligation of the laboratory. Laboratories are
not required to accept samples after the set shipping dates.
Minor delays or adjustments to the schedulfe are usually
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acceptable to the receiving laboratory, however, major
changes may require a resolicitation of the SAS.
4.5 SECTION 5 - Estimated date(s) and method of shipment:
4.5.1 The method of shipment is usually overnight express carrier.
The name of the carrier should be included, if known.
4.5.2 The date(s) of shipment is usually the same day as
collection for delivery on the next working day. If
Saturday deliveries are expected, it must be noted here.
4.6 SECTION 6 - Number of days analysis and data required... :
4.6.1 Specify the contract required analysis holding time from the
date of sample receipt by the laboratory. This is usually a
few days less than the technical holding time.
4.6.2 Specify the time frame in which data packages and all other
deliverables are required.
4.6.2.1 For large numbers of samples or for samples
shipped over the course of several weeks, it is
convenient to group samples by Sample Delivery
Groups (SDGs). A SDG is defined as all samples
received within a 14 day period or 20 samples,
whichever is reached first.
4.6.2.2 Unless otherwise specified, the turnaround time
for data packages will be the number of days
specified after receipt of the last sample.
4.7 SECTION 7 - Analytical protocol required ... :
4.7.1 Reference the method number and source of the protocol.
Include a copy of the method as an attachment, if the method
is not well known or readily available.
4.7.2 Include other methods that are acceptable options, i.e.
Nitrate/Nitrite by EPA Methods 353.2 or 353.3.
4.7.3 State methods which should not be exercised as options.
This is to guard against inadequate protocols which may be
suggested by laboratories during the SAS solicitation
period.
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4.8 SECTION 8 - Special technical instructions ... :
4.8.1 Any modifications or additions to the protocols listed in
Section 7 should be referenced in this section. This
section consists of at least two subsections:
a. Calibration Procedure and Criteria
b. Internal Quality Control Checks, Control Limits and
Corrective Actions
4.8.1.1 Many standard methods, such as SW846 methods,
list the QC checks to be performed, but do not
specify the frequency of QC checks, compounds to
be used for surrogates and matrix spikes or the
control limits. Also, individual laboratories
may interpret QC requirements differently. For
these reasons, QC requirements must be specified
explicitly in the SAS CRF. A reference to the
method, or its QC requirements, is not
sufficient.
4.8.2 If the laboratory is required to supply sampling material
(i.e. tenax cartridges for air sampling), all requirements
must be stated. Chain-of-custody must be included from the
laboratory to the remedial contractor.
4.9 SECTION 9 - Analytical results required ... :
4.9.1 Data Calculations and Reporting Units: Specify how the data
are to be calculated and reported.
4.9.2 Documentation and Deliverables: Specify all deliverables
required to validate the data. Deliverables should include
all items necessary to document and recreate the analyses on
paper. This would include, but not be limited to:
a.
sample tracking reports, e.g. chain-of-custody forms
b.
a copy of the SAS CRF
c.
telephone logs
d.
a case narrative
e.
sample results
f.
QA/QC summaries
g-
raw sample data
h.
sample preparation logs
i.
example calculations
j.
calibration data
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4.10 SECTION 10 - Other ... :
4.10.1 Reference and include as an attachment any additional
information or instructions necessary to perform the
analyses.
4.10.2 This section must include the requirement for the
laboratory to complete the "Laboratory QC Summary
Form" (see example SAS CRF).
4.11 SECTION 11 - Name of sampling/shipping contact, etc.: State the
name (with affiliation) and phone number of the person(s)
responsible for field sampling and shipping samples from the site.
This is the person(s) who will be contacted (by the Region) should
questions or problems arise during the sampling event.
4.12 SECTION 12 - Data Requirements: List all target compounds or
analytes, the required detection limits and/or contract required
quantitation limits (CRQLs) for each and the desired precision.
If the SAS includes more than one matrix, list all concentration
units. Desired precision may be expressed as + X or as a
concentration. If a large number of target compounds or analytes
are requested, reference and Include them as Table 1.
4.13 SECTION 13 - QC Requirements: List all laboratory QC
requirements, including frequency and required control limits.
These requirements will have been described previously in Section
7 and/or Section 8.
4.13.1 Typical requirements would include, but not be limited
to: laboratory method blanks, laboratory duplicates,
surrogate spikes, laboratory control samples, and
matrix spike/spike duplicate analyses.
4.13.2 Frequency should be expressed as either a time period
(i.e. daily) or as per a specified number of samples
(i.e. per SDG).
4.13.3 Limits should be expressed as X recovery, relative
percent difference or concentration.
4.14 SECTION 14 - Action required ... : List the action(s) to be taken
if the control limits are exceeded. Typically this requires
reanalysis, or repreparation and reanalysis, of the samples.
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5 INSTRUCTIONS FOR PREPARING THE "LABORATORY QC SUMMARY REPORT" FORM
5.1 A Laboratory QC Summary Report (QSR) Form to accompany the SAS CRF
must be prepared by the author of the SAS CRF for submission to
the laboratory with the SAS CRF. The laboratory will complete the
form and submit it as part of the data package.
5.2 The QSR form should include specific questions relating to the
analysis method outlined in the SAS CRF. The SAS CRF should be
used for guidance in preparing the QSR form. Please refer to the
attached example of a QSR form.
5.3 QSR Header
5.3.1 The header of the QSR form should include specific
information pertaining to a given Sample Delivery Group
(SDG).
5.3.2 The header should provide space for the following
information:
(a) Name of the laboratory
(b) Name and title of the person preparing the data
package
(c) Method of analysis
(d) SAS number
(e) Matrix and number of samples in the SDG
(f) Date
5.4 QC Summary Table
5.4.1 The purpose of the QC Summary Table is to provide a list of
the minimum QC requirements for the analysis specified in
the SAS CRF.
5.4.1.1 All QC parameters for which QC limits have been
set should be included in this table.
5.4.2 The QC parameters included in this summary table will be
specific for each analysis to be performed.
5.4.3 All boxes in the QC Summary Table should be filled in by the
author of the SAS CRF prior to submission to the laboratory.
5.5 The basic questions in the QSR form should be phrased so the
response is either "YES" or "NO". All'"YES" answers should
indicate compliance with SAS CRF QC requirements: A "NO" is
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indicative of non-compliance, a laboratory or sample analysis
problem, or of the existence of an event that requires further
information.
5.5.1 For each "NO" answer, a supplementary question should be
asked explaining why the QC requirement was not met.
5.5.2 Supplementary questions should be phrased so they can be
completed with short answers.
Questions concerning the following method requirements should be
addressed in the QSR form:
5.6.1 Holding Times
5.6.1.1 Were the contract and technical holding times
met both for extraction/preparation and
analysis?
5.6.1.2 Was the data package sent within the specified
time period?
5.6.2 Method of Analysis and Detection Limits
5.6.2.1 Was the appropriate analysis method used?
5.6.2.2 Were the detection limits listed in the SAS CRF
achieved?
5.6.3 Calibrations
5.6.3.1 Were the calibration requirements of parameters
such as percent Relative Standard Deviation
(ZRSD), percent Difference (ZD), minimum
Relative Response Factor (RRF), correlation
coefficient and/or percent Recovery (XR) met?
5.6.3.2 Were calibrations performed at the frequency
specified in the method?
5.6.4 Blanks
5.6.4.1
5.6.4.2
Was blank contamination a problem?
Were blanks analyzed at the frequency specified
in the method?
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5.6.5 Sample QC
5.6.5.1
5.6.5.2
5.6.6 Other
5.6.6.1
Vere the QC requirements met for percent
Recovery (XR) and/or Relative Percent Difference
(RPD) for the following?
(1) Matrix Spikes/Matrix Spike Duplicates
(MS/MSD)
(2) Laboratory Control Samples (LCS)
(3) Laboratory duplicates
(4) Surrogate spikes
Were all required sample QC analyses performed
at the frequency specified in the method?
Questions addressing other method-specific
requirements may be necessary.
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D. S. ENVIRONMENTAL PROTECTION AGENCY
CLP Sample Management Office SAS Number
P. 0. Box 818 - Alexandria, Virginia 22313
Phone: 703/557-2490; FTS/557-2490
SPECIAL ANALYTICAL SERVICES
Client Request
Regional Transmittal Telephone Request
D.
E.
A. EPA Region/Client: Region 9
B. Region Contact: Jane Anderson, ESAT, (415) 882-3069
C. Date of Request:
Site Name: " J~'o % ) Q_ "b o vv\ p
City/State: .2. vw*-Y\ \j\ \V e 3 & lA
F. 2 Digit Superfund Site Identifier: ^
Please provide below a description of your request for Special Analytical
Services under the Contract Laboratory Program. In order to most efficiently
obtain laboratory capability for your request, please address all applicable
questions. Incomplete or erroneous information may result in a delay in the
processing of your request. If you need to provide additional information not
addressed by the questions, please attach additional sheets of paper.
1. General description of analytical service requested:
The analysis of low concentration water and soil samples for chlorinated
herbicides by SW846 Method 8150.
2. Definition and number of work units Involved (specify whether whole
samples or fraction; whether organics or inorganics; whether aqueous or
soil and sediments; and whether low, medium or high concentration):
3. Purpose of analysis (specify whether Superfund [enforcement or remedial
action], RCRA, NPDES, etc.):
SAS8150.CRF
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¦»> 4. Estimated date(s) of collection (provide a sampling schedule):
XTo,r>e /£", /??z
5. Estimated date(s) and method of shipment:
Federal Express - shipped same day as collection for next day delivery.
6. Number of days analysis and data required after laboratory receipt of
samples:
Contract required holding time Is five (5) days for extraction of water
samples, ten (10) days for the extraction of soil samples and forty (40)
days for analysis from the date of sample receipt by the laboratory.
Data packages and all other deliverables are required within 35 days
from receipt of last sample in each Sample Delivery Group (SDG). A SDG
is defined as all samples received within a 14 day period or 20 samples,
whichever is reached first.
7. Analytical protocol required (attach copy If other than a protocol
currently used in this program):
Follow SW846 Method 8150 for extraction and analyses. Contract required
quantitation limits (CRQL) are as per Table 1 in SW846 Method 8150.
a. Dlazomethane Is a carcinogen and can explode under certain
conditions. Refer to Section 7.3.1 of Method 8150 for
precautions.
b. Capillary columns may be used for this analysis, as long as the
laboratory demonstrates that the analysis meets all the
performance and QA/QC criteria specified in Method 8150 and in
this contract.
8. Special technical instructions (if outside protocol requirements,
specify compound names, CAS numbers, detection limits, etc.):
a. Calibration Procedure and Criteria:
Calibrate according to Sections 5.11 and 7.5 of SW846 Method 8150
and Sections 7.4.2 and 7.5 of SW846 Method 8000, with the
following specifications:
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1. Five-point initial calibration curve with a low standard at
the concentrations of the CRQL or lower is required. The
average Response Factor (RF) from the initial calibration is
to be used to quantitate sample results.
The low concentration standard must have a signal-to-noise
ratio of 5:1 or greater for all analytes of interest. If
this requirement cannot be met, the laboratory must submit a
Method Detection Limit (MDL) study as part of the data
package, in order to validate its ability to achieve the
contract required detection limits. The MDL £s defined as
the minimum concentration of a substance that can be
measured and reported with 99X confidence that the value is
above zero.
2. A continuing calibration at the midpoint concentration for
each analyte is to be analyzed at the beginning of each day
and after each group of 10 samples. This standard is to be
used to verify instrument performance.
3. Less than 20X relative standard deviation (ZRSD) in
calibration factors (CF) for the initial calibration
standards and less than a +15X difference (XD) in CF for the
daily continuing calibrations is required.
b. Internal Quality Control Checks. Control Limits and Corrective
Actions:
1. Analyze method blanks at a frequency of one per group of 20
or fewer samples. The method blanks must contain less than
or equal to the CRQL of the herbicide compounds listed in
Table 1. If a method blank exceeds these criteria, the
laboratory must consider the analytical system to be out of
control. The source of the contamination must be
investigated and appropriate corrective measures must be
taken and documented before further sample analysis
proceeds. All samples processed with a method blank that is
out of control must be re-extracted and re-analyzed at no
additional cost to the Agency. The Laboratory Manager, or
his designee, must address problems and solutions in the SDG
narrative.
2. A herbicide surrogate (e.g., a herbicide or chemically
similar compound that is not expected to be present in the
samples) must be spiked into the standards, samples, method
blanks and QC samples (see Section 5.13 and 8.3 of Method
8150). The amount of surrogate added must be at least 10
times the instrument detection limit. Recoveries of 65-125*
are required, unless documentation (such as control charts)
are available to support a different range of recoveries.
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Laboratory must submit, as part of the data package, all
supporting documentation.
3. Second column confirmation is required for all positive
results reported.
4. Sample extracts containing one or more analytes at
concentrations above the initial calibration range are to be
diluted and re-analyzed. If dilution is necessary, the
dilution must be adjusted so that the highest concentration
analyte is determined at a concentration in the upper half
of the calibration range. The laboratory must report the
results and document both analyses.
5. Analyze matrix spikes and matrix spike duplicates (MS/MSD)
at the frequency of one per group of 20 or fewer samples.
Concentration of matrix spike solution should be such that
the final extracts contain amounts at the mid-range of the
calibration curve. The matrix spiking solution should
contain a minimum of three herbicides chosen from the
analyte list in Table 1. Recoveries of 75-125Z for waters
and 65-135X for soils are required.
6. If the above control limits are exceeded, take appropriate
actions to correct the problem and re-analyze the affected
samples.
Analytical results required (if known, specify format for data sheets,
QA/QC reports, Chain-of-Custody documentation, etc.) If not completed,
format of results will be left to program discretion.
a. Data Calculations and Reporting Units:
1. Calculate the CF and the concentration of individual
analytes using the equations in Sections 7.4.2 and 7.8.1 of
SW846 Method 8000. The sample results are to be reported in
the concentration units of micrograms per liter (ug/L) for
water samples and micrograms per kilogram (ug/Kg) on a dry
weight basis for soil samples.
2. All records of analysis, dilutions and calculations must be
legible and sufficient to recalculate all sample
concentrations and QC results. Include an example of the
calculations in the data package.
.CRF
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b. Documentation and Deliverables:
Deliverables (In the form of a purge file - i.e., original
documents) for each Sample Delivery Group shall include all
deliverables required by the IFB, including, but not limited to:
1. All Sample Tracking Reports (i.e., signed SAS Packing
Lists/Chain-of-Custody forms).
2. A copy of the SAS, as provided by SMO (so that any SMO
changes will be known). Only the technical portion of the
SAS is required.
3. Any telephone logs referring to the samples.
4. A Case Narrative, signed by the laboratory manager or his or
her designee', certifying the accuracy and validity of all
data reported and describing any problems encountered during
the analyses and documenting their resolution(s).
5. Tabulated sample results on a modified CLP Form 1 with
units, percent solids, and sample weights or volumes clearly
specified.
6. Surrogate result summaries on a modified CLP Form II with
calculated percent recovery (XR) values.
7. Matrix Spike/Matrix Spike Duplicate (MS/MSD) result
summaries on a modified CLP Form III with calculated percent
recovery (XR) and relative percent difference (RPD) values.
8. Blank data on a modified CLP Form IV with tabulated results
specifying which samples were analyzed with each blank.
9. Raw Sample data, Including
a. Tabulated results
b. All sample data system printouts
c. Manual worksheets
10. Standards data, including:
a. Standards summaries on modified CLP Forms VI and VII
with calibration factors and percent relative standard
deviation (XRSD) values or percent difference (XD)
values.
b. All standard data system printouts with all compounds
clearly identified.
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11. Raw QC data, including:
a. Blank data, in chronological order:
1. Tabulated results
2. All blank data system printouts.
b. MS/MSD data, in chronological order:
1. Tabulated results
2. All MS/MSD data system printouts.
«.
12. All computer printouts with integrated areas,~peak heights,
and calibration factors.
13. Bench sheets for sample preparation, indicating dates,
times, methods of sample extraction/preparation, spiking
solution identification and volumes/amounts added,
instrument run time/date, etc.
14. A formula (including definitions) showing how the results
were calculated, with an example of an actual calculation.
15. A form describing the source and traceability of the
standards and listing the concentration of the standards
used, the quantitation area for the standards, the response
factor for the standard, the calculated ZRSD for the initial
calibration and the ZD for the continuing calibrations.
16. Extraction logs, dilution logs and percent solids for all
samples.
10. Other (use additional sheets or attach supplementary information, as
needed):
Attached is a copy of the "U. S. EPA Region 9 Laboratory QC Summary
Report" form. This form is to be completed by the Laboratory Manager or
his/her designee and submitted with each data package. The form is to
reflect the conditions contained within the data package with which it
is submitted. Laboratories may make additional copies of this form as
needed. ¦
11. Name of sampling/shipping contact: &r-fc.
l
Phone: ( Y/g) /g? 3 - 5*
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12.
Data Requirements:
Parameter
Detection Limit
8150 - water or soil
See Table 1
13. PC Requirements:
PC Required
Frequency of PC
Limits (X or Conc.^
Matrix Spike/
1 per SDG (not more
75 - 125 XR water
65 - 135 XR soil
<±30* RPD
Matrix Spike Duplicate than 20 samples per SDG)
Method Blanks
1 per SDG
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TABLE 1
CHLORINATED HERBICIDES
Compound Detection Limits
Water (ug/L) Soil (ug/Kg)
2,4-D
12
240
2,4-DB
9.1
180
2.4,5-T
2.0
40
2,4,5-TP (Silvex)
1.7
34
Dalapon
58
1200
Dicamba
2.7
54
Dichloroprop
6.5
130
Dinoseb
0.7
14
MCPA
2500
50,000
MCPP
1900
38,000
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U. s. EPA REGION 9
INSTRUCTIONS
1. A separate form is Co be completed and attached to the Regional copy
(original) of each data package submitted. This form is to be placed
directly behind the case narrative.
2. The Laboratory QC Summary Report form is to be completed by the
Laboratory Manager, or his/her designee.
3. This form will be used to identify areas of non-compliance with the
required QC limits that may result in resampling or reduction in
payment.
4. Answers to questions are designed so that a YES answer indicates
compliance and requires no further explanation. A NO answer indicates
non-compliance and requires a short explanation. If a lengthy
explanation is required (or desired) , write See Case Narrative in the
blank space and include the explanation in the case narrative.
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U. S. EPA REGION 9
LABORATORY QC SUMMARY REPORT
LABORATORY: SAS
SUBMITTED BY: # SAMPLES:
TITLE: MATRIX:
ANALYSIS: HERBICIDES bv EPA METHOD 8150 DATE:
QC SUMMARY TABLE
QC PARAMETER
QC LIMITS
FREQUENCY
Laboratory Blank
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2. Were all samples extracted within the technical
holding times of 7 days (water) or
14 days (soil) from sample collection?
YES
HO
a. If no, list the samples that were extracted outside of the holding
time.
b. How many days outside of the holding time were these samples
extracted?
3. Were all samples received intact and in good YES NO
condition?
4. Were all samples analyzed within 40 days of receipt? YES NO
a. If no, list the samples that were analyzed outside of the holding
time.
b. How many days outside of the holding time were these samples
analyzed?
5. Was the data package sent within 35 days YES NO
from the receipt of the last samples in the SDG?
a. If no, how many days late was the data package sent?
6. Was EPA Method 8150 used to analyze these samples? YES NO
a. If no, specify which method was used.
b. ^ If no, why was this method used? Who authorized its use?
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7. Was a 5-point Initial Calibration Curve run? YES NO
a. If yes, when?
b. If no, why not? ;
8. Did the Initial Calibration curve meet the QC YES NO
requirement -of <20Z RSD for all analytes?
a. If no, specify the analyte(s) and RSD(s) that were outside of the
QC limits.
9. Was a Continuing Calibration standard run at
the beginning of each day? YES NO
After every 10 samples? YES NO
a. If no, why not?
10. Did the Continuing Calibration standards meet
the QC requirement of <+15X D for all analytes? YES NO
a. If no, specify the analyte(s) and RSD(s) that were outside of the
QC limits.
11. Was the minimum response factor of 5:1 signal
to noise ratio met for all analytes in the
Initial and Continuing Calibrations? YES NO
12. Were laboratory blanks extracted and analyzed
at a minimum frequency of 1 per SDG? YES NO
a. If no, at what frequency were blanks performed.
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13. Was blank contamination, if any,
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18. Did che MS/MSD meet the QC requirement of
<+30X RPD for all spike compounds? YES NO
a. If no, specify the analyte(s) and XRPD(s) that were outside of the
QC limits.
19. Vere the CRDLs met for all analytes? YES NO
a. If no, why not?
8150 SUM.RPT
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U. S. ENVIRONMENTAL PROTECTION AGENCY
CLP Sample Management Office SAS Number
P. 0. Box 818 - Alexandria, Virginia 22313
Phone: 703/557-2490; FTS/557-2490
SPECIAL ANALYTICAL SERVICES
Client Request
Regional Transmittal Telephone Request
A. EPA Region/Client: Region 9
B. Region Contact: Jane Anderson, ESAT, (415) 882-3069
C. Date of Request:
D. Site Name: I 3 < b U» IndwsrtrflS
E. City/State: Ghost C4
F. 2 Digit Superfund Site Identifier:
Please provide below a description of your request for Special Analytical
Services under the Contract Laboratory Program. In order to most efficiently
obtain laboratory capability for your request, please address all applicable
questions. Incomplete or erroneous information may result in a delay in the
processing of your request. If you need to provide additional information not
addressed by the questions, please attach additional sheets of paper.
1. General description of analytical service requested:
The analysis of low concentration water for Hexavalent chromium (Cr*6)
by EPA Method 218.4. Laboratories bidding on this analysis must be
located within 3 hours drive of the site.
2. Definition and number of work units Involved (specify whether whole
samples or fraction; whether organics or inorganics; whether aqueous or
soil and sediments; and whether low, medium or high concentration):
JL3 lou> o->«uV<.rs
3. Purpose of analysis (specify whether Superfund [enforcement or remedial
action], RCRA, NPDES, etc.):
$F Ri/FS
X0
SAS218 4.CBF
Page 1 of 5
Revision 6/92
Approved
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4. Estimated date(s) of collection (provide a sampling schedule):
PebrUAtry g _ , ftfqj
5. Estimated date(s) and method of shipment:
By car to arrive at laboratory within 12 hours of sample collection.
6. Number of days analysis and data required after laboratory receipt of
samples:
Contract required analysis holding time is twelve (12) hours from the
time of sample receipt by the laboratory.
Data packages and all other deliverables are required within 35 days
from receipt of last sample in each Sample Delivery Group (SDG). A SDG
is defined as all samples received within a 14 day period or 20 samples,
whichever is reached first.
7. Analytical protocol required (attach copy if other than a protocol
currently used in this program):
a. Follow EFA Method 218.4 for analysis of Cr+6 by atomic absorption,
chelation-extraction.
b. Samples are to be transported and stored at 4°C until analysis and
validation of results are complete.
c. Domestic and industrial waste samples are to be filtered prior to
the determination of hexavalent chromium.
8. Special technical instructions (if outside protocol requirements,
specify compound names, CAS numbers, detection limits, etc.):
a. Calibration Procedure and Criteria:
1. Use at least five calibration standards (not including a
zero standard) to obtain a standard calibration curve. The
analytical working range must not exceed 10 to 250 ug of
chromium per liter. The XRSD is not to exceed 10Z for any
analyte.
2. Calibration verification standards at the mid-point
concentration are to be analyzed at a frequency of one per
group of 10 or fewer samples and at the end of the analysis
of a sample delivery group. Percent variances of ±102 from
the expected result are required. Results of the
SAS218_*.CRF Page 2 of 5 Revision 6/92
Approved .
-------
calibration verification standards must fall within the
control limits of 90 - 110X of the expected value.
b. Internal Quality Control Checks. Control T.fmft-a and Corrective
Actions:
1. Analyze laboratory blanks at a frequency of one per group of
20 or fewer samples. Laboratory blanks must contain less
than 10 ug/L Cr4*. Otherwise, all samples associated with
the blank must be prepared again and reanalyzed.
2. Analyze laboratory duplicates at a frequency of one per
group of 20 or fewer samples. Relative percent difference
(RPD) of less than +20X is required.
3. Analyze matrix spikes at a frequency of one per group of 20
or fewer samples. Matrix spike concentration is to be 150
ug/L. Recoveries of 75 - 125Z are required.
4. Samples containing hexavalent chromium concentrations above
the calibration range are to be diluted and re-analyzed.
Report the results and documentation for both analyses.
5. If the above control limits are exceeded, take appropriate
actions to correct the problem and re-analyze the affected
samples.
9. Analytical results required (if known, specify format for data sheets,
QA/QC reports. Chain-of-Custody documentation, etc.) If not completed,
format of results will be left to program discretion.
a. Data Calculations and Reporting Units:
Calculate the sample results according to Section 8 of EPA Method
218.4. Sample results are to be reported to the nearest ug/L for
concentrations less than 10 ug/L Cr*6 and to 2 significant figures
for concentrations exceeding 10 ug/L Cr**. All records of
analysis and standard curve must be legible and sufficient to
recheck all sample concentrations and QC results.
b. Documentation and Deliverables:
Deliverables (in the form of a purge file - i.e., original
documents) for each Sample Delivery Group shall include all
deliverables required by the IFB, Including, but not limited to:
1. All Sample Tracking Reports (i.e., signed SAS Packing
Lists/Chain-of-Custody forms).
SAS218_*.CRF Page 3 of 5 Revision 6/92
Approved
-------
2. - A copy of the SAS, as provided by SHO (so that any SMO
changes will be known). Only the technical portion of the
SAS Is required.
3. Any telephone logs referring Co the samples.
4. A Case Narrative, signed by the laboratory manager or his or
her designee, certifying the accuracy and validity of all
data reported and describing any problems encountered during
the analyses and documenting their resolutlon(s).
5. Tabulated sample results on a modified CLP Form I, with
units, percent solids, and sample weights or volumes clearly
specified.
6. Initial and continuing calibration verifications (ICV and
CCV) on a modified CLP Form II, with calculated percent
recovery (XR).
7. Blank data on a modified CLP Form III specifying which
samples go with each blank.
8. Matrix spike result summary on a modified CLP Form V with
calculated percent recovery (XR).
9. Duplicate results on a modified CLP Form VI with calculated
percent difference (XD).
10. Preparation and chelation extraction logs on modified CLP
Form XIII.
11. Analysis run logs on modified CLP Forms XIV.
12. Raw sample, standard and QC data, including:
a. instrument output
b. bench sheets and worksheets
c. tabulated results
13. Bench sheets for sample preparation, QC spikes.
14. Traceability forms for all standards used for calibration
and spiking.
Other (use additional sheets or attach supplementary information, as
needed):
Attached is a copy of the "U. S. EPA Region 9 Laboratory QC Summary
Report" form. This form is to be completed by the Laboratory Manager or
his/her designee and submitted with each data package. The form is to
>.crf Page 4 of 5 Raviaioo 6/92
Approved
-------
reflect the conditions contained within the data package with which it
is submitted. Laboratories nay make additional copies of this form as
needed.
11. Name of sampling/shipping contact: D.6. Cooper
Phone: <
12. Data Requirements:
Parameter
Hexavalent Chromium
Detect*^ T.lmit-
10 ug/L
13. PC Requirements:
PC Required
Laboratory Blanks
Laboratory Duplicates
Matrix Spikes
Frequency of PC
1 per 20 samples
1 per 20 samples
1 per 20 samples
Limits (X or Cone.)
< 10 ug/L
RPD <±20X
75 - 125X
14. Action required if limits are exceeded:
If above control limits are exceeded, take appropriate actions to
identify the problem by re-analyzing the affected samples. Corrective
action should be taken before additional samples are analyzed.
SASZie VCRP
Page 5 of 5
Revision
Approved
6/92
-------
D. S. EPA REGION 9
INSTRUCTIONS
1. A separate form is to be completed and attached to the Regional copy
(original) of each data package submitted. This form is to be placed
directly behind the case narrative.
2. The Laboratory QC Summary Report form is to be completed by the
Laboratory Manager, or his/her designee.
3. This form will be used to identify areas of non-compliance with the
required QC limits that may result in resampling or reduction in
payment.
4. Answers to questions are designed so that a YES answer indicates
compliance and requires no further explanation. A NO answer indicates
non-compliance and requires a short explanation. If a lengthy
explanation is required (or desired), write See Case Narrative in the
blank space and include the explanation in the case narrative.
-------
U. S. EPA REGION 9
LABORATORY QC SUMMARY REPORT
LABORATORY:
SUBMITTED BY:
TITLE:
ANALYSIS: HEXAVALENT CHROMIUM bv EPA METHOD 300.3
DATE:
SAS #:
§ SAMPLES:
MATRIX: _
QC SUMMARY TABLE
| QC PARAMETER
QC LIMITS
FREQUENCY
1 Laboratory Blank
-------
2. Were all samples analyzed within the technical
holding time of 24 hours from sample collection? YES NO
a. If no, how many samples were analyzed outside of the holding time?
b. How many days outside of the holding time were these samples
analyzed?
3. Were all samples received intact and in good YES NO
condition?
4. Was the data package sent within 35 days YES NO
from the receipt of the last samples in the SDG?
a. If no, how many days late was the data package sent?
5. Was EPA Method 218.4 used to analyze
these samples? YES NO
a. If no, specify which method was used.
b. If no, why was this method used? Who authorized its use?
6. Was a 5-point Initial Calibration Curve run? YES NO
a. If yes, when?
b. If no, why not?
300 SIW.RPT
Page 2 of 4
Revision 6/92
Approved
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7. Did Che Initial Calibration curve meet the QC YES NO
requirement of <101 RSD?
a. If no, specify RSD.
8. Was a Continuing Calibration standard run at
the beginning of each day? YES NO
After every 10 samples? YES NO
a. If no," why not?
9. Did the Continuing Calibration standards meet
the QC requirement of <+10X D? YES NO
a. If no, specify ZD.
10. Were laboratory blanks analyzed at a
minimum frequency of 1 per 20 samples? YES NO
a. If no, at what frequency were blanks performed?
11. Was blank contamination, if any, less than
the CRDL for all analytes? YES NO
a. If no, at what levels was the contamination present?
12. Were Matrix Spike analyses performed at a minimum
frequency of 1 per SDG? YES NO
a. If no, why not?
300_SUM.RPT Page 3 of 4 Revision 6/92
Approved
-------
13. Did the Matrix Spike meet the QC requirement of
751 - 125% R? YES NO
a. If no, specify recovery.
14. Vere Laboratory Duplicate analyses performed at a minimum
frequency of 1 per SDG? YES NO
a. If no, why not?
15. Did the Laboratroy Duplicate meet the QC
requirement of <+2OX RPD? YES • NO
a. If no, specify the relative percent difference.
16. Was the CRDL met? YES NO
a. If no, why not?
300_SUM.RFT Page 4 of 4 Revision 6/92
Approved
-------
ANALYSES REQUESTED
CLP ANALYSES REQUESTE
RAS+SAS
ROUTINE ANALYTICAL SERVICES (RAS)
SPECIAL ANALYTICAL 1
SERVICES (SAS) |
CHEMISTRY TYPE
ORGANICS
INORGANICS
ANALYSES REQUESTED
PRESERVATIVES
ANALYTICAL
HOLDING TIKE (s)
CONTRACT
HOLDING TIME (S)
SAMPLE x SAMPLE
NO. OF
BOTTLES
PER
ANALYSIS
NO. OF
BOTTLES
PER
ANALYSIS
NO. OF
BOTTLES
PER
ANALYSIS
NO. OF
BOTTLES
PER
ANALYSIS
NO. OF
BOTTLES
PER
ANALYSIS
NO. OF
BOTTLES
PER
ANALYSIS
NO. OF
BOTTLES
PER
ANALYSIS
NO. OF
BOTTLES
PER
ANALYSIS
SAMPLE
LOCATION
SAMPLING
SCHEDULE
TOTALS III | III
-------
ualtiii uoutnio mi ¦ uoua tutu
at iui wiitio
imcial analttical mvicti (u*>
lourut analytical tuvicti cut) |
annum r m
M6ANIC1
IHORCANtCt
cmanici
IWMMIC* |
imcimc AJUiTstt itautmo
MITKSO
601
MilHGD
602
MA JO*
AMI0MI
1 TCl
1CL 1 SCNI VOAl
VOA'I | (low cone)
TCl I MITICIDIt
•INI V0A| t Mil
(Md cone) | low cone)
MITICI01I
I Kit
(Md cone)
TCL ' j Ttt 1 CTAN10I 1
MITALt (tat)lMTALI (tot)l 1
(low cone) | (md cone) | (Md cone) |
MtttivAiivu
Add 2 drops
111 MCI
Chill u(C
Add 2 drop* I
111 NCI
Chill to * C |
Add 1 drop* IChill 10 4 C
111 NCI
Chill to 4 C
Chill to 4 C
Chill to 4 C
Chill to 4 C
Chill to 4 ClChlll to 4 ClChlll to 4 C,|
add MMOl add MXOJ add NaON to
to pN <2 | to p* <2 |pN>12 |
/unman memo tiw (•>
Mold <14
din
Mold
Hold <10
diy*
Mold
14 day*
* uwii
KO. OF
I0T11II
Ml
ANAITIIS
*0. or
IOITLII
HI
ANALYSIS
no. or
IOITLII
Kl
ANALTIII
ho. or
lOTIltt
PU
ANALTIII
no. or
IOITLII
Ml
ANALTIII
no. or
IOITLII
Ml
ANALTIII
no, or
IOITLII
HI
ANALTIII
NO. or
IOITLII
Pll
ANALTIII
no. or
lomt*
PCI
ANALTIII
no. or
lOTTLtt
Ml
ANALTIII
10. or
•omit
Ml
ANALTIII
TOTAL
no. or
101 TUt
Ml UtLl
!
lomt
i*»tn
twu
LOCATION
uwiins
ICMDIJU
GCNCtNTIAIION
10U | MO.
llitll
lllll
vllt
2 i (0 •!
• lit!
vial
1 I t tltir
polyttliyltM
bottl*
t 1 40 al
•till
vial
2 x t (Itor
Mtir gilt*
bottlto
I I 12 01
Midi BOUth
glut )ir
1 i 1 11t«r
ufcor
elttt bettlt
1 I J2 ot
Mid* aouth
Slut Jar
1 I 1 titer
poly*thyl«n*
bottl*
liMtl
Mid* MUth
tint ]*r
llttN
Nidi aouth
|Um )tr
r
|
1
| |
10TAU Ion Cent
! ! ! ! ! i i i i i i i i
I I I I I I I I I I
-------
RgggEST- FOft AHAliYS;I'S-
WWillXs- QROttMRUM^
HEHISTRY TYPE
qfc&fVKtCS
IMOSGANICS
I
I
I **S I
| TOC ft |
I COD |
1 RAS ~ SAS | IAS
SPCCinC ANALYSES REQUESTED j VOA'S I SEMI VOAs
| Low CRQLs |
I
RAS
METALS
(total)
I
|Cl,W02/W03.
|S04,ALK.TDS
1-
¦I-
¦ I
|H2SO& to |
|pH<2** |
|chiii |
RESER VAT IVES
|Add 2 drops |CMll to 4 C |
| 1:1 MCI j |
(Chill to 4 C j |
Add HN03 | Chill
to pH <2 | to 4 C
I
\
|Hold <14
ANALYTICAL MOLDING TIME (a)|days
I
I
|Hold <28 1
I |
I I
I
(Hold <7 days |Nold to <6 |Hold to <7
| to extract Ion] Months 128 | days
|then 40 days |days for Kg]|
1
|Hold <10
(days
I
•I"
¦I"
I-
I-
CONTRACT MOLDING TIME (*>
(Hold * |
I
I
I
SAMPLE |
LOCATION| SAMPLING
NUMBER | SCHEDULE
| |3 x 40 ¦!
|CONCEH|glass
I IvJal
| L/H I «>•
|2 x 1 liter (1 x 1 liter I 1x500*1
|a* j C1/2>* | <1/2>*
I
P-3D ( 1/8/90
Lsb QC |
I
I
I
I
I
I
I L I
I
P-3S ( 1/8/90
I
I «• I
I I
) i
P-1B ( 1/8/90 | L
I t
E-1D | |
(dtp of | 1/8/90 | L
P-1D) | j
1 I
E-2D | 1/8/90 | L
(blank) j |
GRAND TOTALS
I 5 (
18
12
* * ainlnn vol me needed when full recovery of a well purged dry exceeds 3 hours
-------
ANALYSES REQUESTED MATRIX = LOU CONCENTRATION WATERS
CLP ANALYSES REQUESTE
RAS+SAS
ROUTINE ANALYTICAL SERVICES (RAS)
SPECIAL ANALYTICAL 1
SERVICES (SAS) |
CHEMISTRY TYPE
ORGANICS
INORGANICS
ANALYSES REQUESTED
RAS+SAS
VOA's
RAS
VOA's
RAS
SEMI VOAs
RAS
PEST & PCBs
RAS
METALS
(total)
RAS
CYANIDE
SAS
TRITIUM
SAS
Gross alpha&
beta, gamma
PRESERVATIVES
Add 2 drops
1:1 HCl
Chill to 4
Add 2 drops
1:1 HCl
Chill to 4
Chi 11 to 4 C
Chill to 4 C
add HN03
to pH <2
Chill to 4
add NaOH to
pH>12
none
none
in
field
ANALYTICAL
HOLDING TIME (s)
Hold <14
days
Hold <14
days
Hold <7 days
prior to
extraction,
40 days after
extraction
Hold <7 days
prior to
extraction,
40 days after
extraction
Hold to <6
months
[26 days
for Hg]
<14 days
Hold to <6
months
Hold to <6
months
CONTRACT
HOLDING TIME (S>
Hold <10
days
Hold <10
days
Hold <5 days
prior to
extraction,
40 days after
extraction
Hold <5 days
prior to
extraction,
40 days after
extraction
Hold to <6
months
[26 days
for Hg]
<12 days
Hold to <6
months
Hold to <6
months
SAMPLE x SAMPLE
NO. OF
BOTTLES
PER
ANALYSIS
NO. OF
BOTTLES
PER
ANALYSIS
NO. OF
BOTTLES
PER
ANALYSIS
NO. OF
BOTTLES
PER
ANALYSIS
NO. OF
BOTTLES
PER
ANALYSIS
NO. OF
BOTTLES
PER
ANALYSIS
NO. OF
BOTTLES
PER
ANALYSIS
NO. OF
BOTTLES
PER
ANALYSIS
SAMPLE
LOCATION
SAMPLING
SCHEDULE
3 x 40 ml
glass
vial
2 x 40 ml
glass
vial
2 x 1 liter
amber
glass bottle
2 x 1 liter
amber
glass bottle
1 x 1 liter
poly
bottle
1x1 liter
poly
bottle
1 x 8 oz
amber
glass bottle
4x1 liter
poly
bottle
MU-109
2/25-2/28
2
1
1
4
HU-112
2/25-2/28
2
1
1
1
4
¦
MU-147
2/25-2/28
3
1
1
4
MW-206
LAB QC
2/25-2/28
4
4
4
2
2
2
8
GU-210
blank near
MU-206
2/25-2/28
3
2
2
1
1
1
4
MU-219
2/25-2/28
2
1
1
4
GU-220
dup of
MU-219
2/25-2/28
2
1
1
4
HW-251
2/25-2/28
3
1
1
4
TOTALS | 9 | 12 | 6 | 6 | 9 | 3 | 9 I 36
-------
APPENDIX E
Sample Container Requirements
for
CLP Analyses
-------
ORGANIC SAMPLE COLLECTION
REQUIREMENTS
WATER SAMPLES
REQUIRED
VOLUME
CONTAINER TYPE
EXTRACTABLE ANALYSIS 1 GALLON
-(LOW LEVEL)
EXTRACTABLE ANALYSIS 1 GALLON
(MEDIUM LEVEL*)
VOLATILE ANALYSIS 80 ML
(LOW OR MEDIUM LEVEL*)
0000 -
00QD4
DC
•LITER AMBER
GLASS BOTTLES
x 32-OZ. WIDE-MOUTH
GLASS JARS
2 x 40-ML GLASS VIALS
SOIL/SEDIMENT SAMPLES
REQUIRED
VOLUME
CONTAINER TYPE
EXTRACTABLE ANALYSIS
(LOW OR MEDIUM LEVEL*)
6 OZ.
D
on
1 X 8-OZ. WIDE-MOUTH
GLASS JAR
OR
2 x 4-OZ. WIDE-MOUTH
GLASS JARS
VOLATILE ANALYSIS
(LOW OR MEDIUM LEVEL*)
240 ML
SB
2 x 120 ML WIDE-MOUTH
GLASS VIALS
•ALL MEDIUM LEVEL SAMPLES TO BE SEALED IN METAL PAINT CAN FOR SHIPMENT ^
I >>
-------
INORGANIC SAMPLE COLLECTION
REQUIREMENTS
WATER SAMPLES
REQUIRED
VOLUME
CONTAINER TYPE
METALS ANALYSIS
(LOW LEVEL)
METALS ANALYSIS
(MEDIUM LEVEL*)
CYANIDE ICN'I ANALYSIS
(LOW LEVELI
CYANIDE (CN~| ANALYSIS
(MEDIUM LEVEL*)
1 LITER
16 OZ.
1 LITER
16 OZ.
U
1 x 1 •UTTER
POLYETHYLENE BOTTLE
1 x 16-OZ. WIDE-MOUTH
GLASS JAR
1 x 1-LITER
POLYETHYLENE BOTTLE
1 x 16-OZ. WIDE-MOUTH
GLASS JAR
SOIL/SEDIMENT SAMPLES
METALS "AND CYANIDE (CN")
ANALYSIS
(LOW OR MEDIUM LEVEL*)
REQUIRED
VOLUME
6 OZ.
0
on
CONTAINER TYPE
1 x 8-OZ. WIDE-MOUTH
GLASS JAR
OR
2 x 4-OZ. WIDE-MOUTH
GLASS JARS
•ALL MEDIUM LEVEL SAMPLES TO BE SEALED IN METAL PAINT CAN FOR SHIPMENT
<
%
-------
DIOXIN SAMPLE COLLECTION
REQUIREMENTS
WATER SAMPLES
REQUIRED
VDUIME
CONTAINER TYPE
2,3.7,8-TCOD
ANALYSIS
(MUIX1 • CONCENTRATION)
2 LITERS ^
III * * 1-LITER AM8ER
GLASS BOTTLES
SOIL /SEDIMENT SAMPLES
REQUIRED
VOLUME
CONTAINER TYPE
2.3.7.8-TCDD
ANALYSIS
IMULTI -CONCENTRATION I
4 OZ.
M 1 x 4-02. WIDE-MOUTH
U GLASS JAR
n 0R
1 x 8-0Z. WIDE-MOUTH
»—' GLASS JAR
HIGH HAZARD SAMPLE COLLECTION
REQUIREMENTS
REQUIRED
LIQUID OR SOLID SAMPLES VOLUME CONTAINER TYPE
ORGANIC AND INORGANIC
6 OZ.
\ 1 x 8-OZ. WIDE-MOUTH
ANALYSIS
1 GLASS JAR
•ALL MEDIUM LEVEL SAMPLES TO BE SEALED IN METAL PAINT CAN FOR SHIPMENT
>
-------
(11/92)
APPENDIX F
Sample Holding Times, Treatment and Preservation
for
RAS and Common SAS Analyses
-------
(11/92)
Preservation Requirementa for RAS Analyses
WATER SAMPLES
Parameter Concentrat ion Preservat ion
Volatiles Low/Medium Acidify to pH < 2 with HC1.
Add 2 drops 1:1 HC1 per vial before sample
collection. This is generally sufficient to
obtain pH < 2, but depends upon the buf-
fering capability of each aquifer and upon
the particular eyedropper used. During purg-
ing, conduct a pH test on at least one vial
at each site for each aquifer. The tested
vial must be discarded. If the pH is >2,
additional HC1 should be added to sample
vials. Another vial should be pH tested to
ensure pH is now <2. Discard the test vial.
If the sample is suspected of containing
residual chlorine or is to be analyzed for
disinfection by-products such as trihaio-
methanes, other preservation techniques
employing reducing agents such as ascorbic
acid may be required.
Chill collected samples to 4° C. Samples
must be filled with zero headspace and
checked for air bubbles by inverting and rap-
ping sharply against palm. If a pea-size or
larger bubble appears, another sample must be
collected. If acidification causes bubbling,
collect non-acidified samples and notify the
RSCC.
Semivolatiles
Pesticides/PCBs
Low/Medium
Low/Medium
Chill to 4 C
Chill to 4 C
Dissolved Metals Low/Medium
Filter Sample through 0.45 micron filter
immediately after sample collection or with
in-line filtration when possible. Acidify to
pH < 2 with HNO^ after filtration.
Total MetalB
Low/Medium Includes suspended sediments and
particulates. Acidify to pH < 2 with HNO^.
-------
(11/92)
Preservation Reoulrementa for RAS Analyses
WATER SAMPLES
Parameter ConcentratIon Preservation
Cyanides Low/Medium Preserve all samples with 2 ml of 10 N NaOH
per liter of sample to pH > 12. Chill to 4°
C.
Treatment for chlorine or other known oxidiz-
ing agents may be necessary. Test a drop of
the sample with potassium lodlde-starch test
paper (K-I starch test paper). A blue color
Indicates the need for treatment. Add ascor-
bic acid, a few crystals at a time, until a
drop of sample produces no color on the In-
dicator paper. Then add an additional 0.6 g
of ascorbic acid for each liter of sample
volume.
Preservation Requirements for RAS Analyses
SOIL SAMPLES
Parameter
Organlcs
Metals
Cyanide
ConcentratIon Preservation
Low/Medium Chill to 4° C
Low/Medium None
Low/Medium Chill to 4° C
-------
(11/92)
Analytical and Contractual Holding Times for RAS Analyses
Matrix:
Hater
Soil
Analysis
Analytical *
Holding Times
Contractual* *
Holding Times
Analytical*
Holding Times
Contractual**
Holding TlmeB
VOA
14
days
10
days
14
days
10
days
B/N/A
7
days
5
days
14
days
10
days
Pest./PCB
7
days
5
days
14
days
10
days
Mercury
28
days
26
days
28
days
26
days
Cyanide
14
days
12
days
14
days
12
days
Metals
6
months
35
days
6
months
35
days
* The Analytical Holding Time is the amount of time a sample or extract may
be held from sample collection to sample extraction and analysis without the
results being qualified due to potential chemical degradation, analyte losses,
or other changes.
** The Contractual Holding Time is the amount of time a sample or extract may
be held from sample receipt at the laboratory to sample extraction and
analysis according to the contract with the laboratory. Contractual Holding
Times are generally a few days shorter than Analytical Holding Times to allow
for sample shipment to the laboratory.
-------
SAMPLE PRESERVATION
Complete and unequivocal preservation of samples, either domestic sewage, industrial wastes, or
natural waters, is a practical impossibility. Regardless of the nature of the sample, complete stability
for ever) constituent can never be achieved. At best, preservation techniques can only retard the
chemical and biological changes that inevitably continue after the sample is removed from the pare:
source. The changes that take place in a sample are either chemical or biological. In the former case,
certain changes occur in the chemical structure of the constituents that are a function of physical
conditions. Metal cations may precipitate as hydroxides or form complexes with other constituent;,
cations or anions may change valence states under certain reducing or oxidizing conditions; otlici
constituents may dissolve or volatilize with the passage of time. Metal cations may also adsorb on'i
surfaces (glass, plastic, quartz, etc.), such as, iron and lead. Biological changes taking place in n
sample ma> change the valence of an element or a radical to a different valence. Soluble constituents
may be converted to organically bound materials in cell structures, or cell lysis may result in release
of cellular material into solution. The well known nitrogen and phosphorus cycles are example* nt
biological influence on sample composition. Therefore, as a general rule, it is best to analyse the
samples as soon as possible after collection. This is especially true when the analyte concentration is
expccied to be in the low i/g/l range.
Meihods of preservation are relatively limited and are intended generally to (1) retard biol *•«.»'
action. (2) retard hydrolysis of chemical compounds and complexes, (3) reduce volatilit)
constituents, and (4) reduce absorption effects. Preservation methods are generally limited to pH
control, chemical addition, refrigeration, and freezing.
The recommended preservative for various constituents is given in Table 1. These choices are based
on the accompanying references and on information supplied by various Qualitx Assurance
Coordinators As more data become available, these recommended holding times will be adjust-j 1 -
reflect new information. Other information provided in the table is an estimation of the volume
sample required for the analysis, the suggested type of container, and the maximum recommended
holding times for samples properly preserved.
-------
TABLE 1
RECOMMENDATION FOR SAMPLING AND PRESERVATION
OF SAMPLES ACCORDING TO MEASUREMENT"
Measurement
Vol.
Req.
(ml)
Container2 Preservative®*4
Holding
Time5
100 Physical Properties
Color 50 P.G
Conductance 100 PtG
Hardness 100 P,0
Odor
PH
Residue
Filterable
Non-
Filterable
Total
Volatile
Settleable Matter
Temperature
Turbidity
200 Metals
Dissolved
Suspended
Total
200
2S
100
100
100
100
1000
1000
100
*00
200
100
G only
P.G
P.G
P.G
P.G
P.G
P.G
P.G
P.G
P.G
P.G
Cool. 4*C
Cool, 4*C
HNO, to pH<2
Cool. 4'C
None Rrq.
Cool, 4*C
Cool. 4*C
Cool. 4*C
Cool 4*C
Cool. 4°C
None R'eq.
Cool, 4*C
Filter on site
HNO, to pH <2
Filter on site
HNOj to pH<2
48 Hrs
26 D.i\«
6 Mos
24 Hrs
Anah/r
Imnicdi.iii K
7 Days
7 Days
7 Days
7 Days
48 Hiv
Aiulwr
Imimtli.tnlx
48 Hrs.
6 Mos.
6 Mos
6 Mos
<•>
-------
TABLE 1 (COND
Measurement
Dissolved Oxygen
Probe
Winkler
Phosphorus
Ortho-
phosphate.
Dissolved
Hydrolyzable
Total
Total.
Dissolved
Silica
Sulfate
Sulfide
Sulfite
40U Organics
BOD
COD
Oil & Crease
Organic carbon
Phenolics
Vol.
Req.
(ml)
300
300
SO
SO
SO
50
50
50
500
50
1000
50
1000
25
500
Container8 Preservative3,4
(i ImiiiIi' ami lop None Rrq.
G bottle and top Fix on site
atul Mon-
ti! diiik
Filter on site
Cool. 4.*C
Cool. 4*C
H,S04 to pH<2
Cool. 4*C
HjS04 to pH<2
Filler on site
Cool. 4*C
H]SO« to pH<2
Cool, 4*C
Cool. 4'C
Cool. 4°C
add 2 ml run
aci'tati' plus NaOH
to pH >9
None Req.
P.G
P.G
P.G
P.G
P only
P.G
P.G
P.G
P.G
P.G
G only
P.G
G only
Cool. 4*C
Cool. 4°c:
H,S04 to pH<2
Cool. 4*C
H,S04 to pH<2
Coot 4'C
H3SO4 or HQ to pH<2
Cool. 4°C
HjSO, to pH <2
Holding
Time6
Anal\ic
Immrdi.itrh
8 Hours
48 His-
• •
28 D.tx*
28 Da\N
24 Hrs
28 D.i\ s
28 Dj\s
7 Da\«>
Analyze
Immediateh
4R His
28
28 1)j\s
28 Djss
28 Days
-------
TABLE 1 (CONT)
Measurement
Chromium*
Mercury
Dissolved
Total
Vol.
Req.
(ml)
200
100
100
Container8 Preservative'"4
300 Inorganics. Non-MeUllics
Acidity 100
Alkalinity 100
Bromide 100
Chloride 90
Chlorine 200
Cyanides 500
Fluoride
Iodide
Nitrogen
Ammonia
Kjeldahl. Total
P.C
P.G
P.G
P.G
P.G
P.G
P.G
P.G
P.G
300 P.G
100 P.G
400 P.G
300 P.G
Nitrate plus Nitrite 100 P.G
Nitrate*
Nitrite
100
90
P.G
P.G
Cool. 4 °C
Kilter
HNO, to pH<2
HNO,-to -pH<2
Cool.4°C:
Cool. 4*C
Nonr Req.
None Req.
Nonr Req
Cool. 4'C
NaOH to pH >12
0 6^ aworbir arid'
None Req.
Cool. 4*C
Cool,4*C
HjS04 to pH<2
Cool, rc
HjSOt to pH <2
Cool «*C-
H}SO« to pH<2
Cool, rc
Cool, rc
Holding
Time8
24 Hrs.
28 Days
28 Days
14 Da\s
MDjxs
28 Da\ «•
28 Da> s
Analwr
Immrdi.iifh
14 Da\sT
28 Da\s
24 Hrs
28 Da\$
28 Daxs
28 Da\ s
48 Hrs
48 Hrs
-------
TABLE 1 (CONT)
Vol.
Measurement
Req.
(ml) Coniainci2 Preservative3'4
Holding
Time8
MBAS
250 P.G
Cool. 4*C
«Hiv
NT A
50 P.G
Cool. 4*C
24 His
1. More specific instructions for preservation and sampling are found with taeh procedure as
detailed in this manual. A general discussion on sampling water and industrial wastewater may
be found in ASTM. Part 31. p. 72-82 (1976) Method D-3370.
2. Plastic (P) or Glass (G). For metals, polyethylene with a polypropylene cap (no liner) is
preferred
M. S.implc piescnation should 1m- performed immediately ujxm sample collection. F01
< omposite samples e.ic h .iticjuoi should Ik- preserved at the time of col lei 11011. When usi'ol
.111 .uiiom.ued samplei makes it imjx>ssiblc to preserve each aliquot, then samples ma\ lx-
pi('scr\('(l l>> maintaining ai 1°(. until compositing and sample splitting is c-ompleirit
I Win n ,im s.implc is 10 be ship|xad by common carriei or sent through ilir I'niied Sun »
Mails. 11 intisi compl) with tin- Department of Transposition H.i/jidous Materials
Regulations (-19 CKR Part 172) The person offering such materia) for transportation is
lesponsible foi ensuring sue h compliance. For the preservation requirements of Table I.
1 In- Office of Hazardous Materials. Materials Transportation Bureau. Department of
1'iansportation has deiei mined thai the Hazardous Materials Regulations do not appl\ 10
tht folio* ing materials. Hydrochloric acid (HCI) in water solutions at concentrations of
0.01% l>> Mcighi or IcssfpH about 1.9601 greater); Nitricacid(HN'Oa)in water solutions at
c oik enti .uions of 0.15% b> weight or less (pH alx>ut 1.62 or greater); Sulfuric acid (HaSO*1
in watei solutions at concentrations of 0.35% b\ weight or less(pH about 1.15 or greatei 1.
Sodium hwlrovide (NaOH) in water solutions at concentrations of 0.080% b\ weight «»i
less (pH dbom 12.30 or less).
.*>. Samples should be analyzed as soon as possible after collection. The times listed are tht
maximum times that samples ma> be held before analysis and still considered valid
Samples ma\ be held foi longei periods only if the |x'i mi nee. or monitoiing lalx>iaitii\.
has data on file to show that the specific types of sample undei studs are stable (or tht
longer time, and has received a variance from the Regional Administiaioi. Some samples
max not be stable foi the maximum lime |>eiiocl given in the (able. A |*ci miller. 01
monitoring laboratory, is obligated to hold the sample for a shorter time if knouled^
exists 10 show this is necessary to maintain sample stability.
6. Should only be used in the presence of residual chlorine.
-------
7. Maximum holdui); litui- is 21 hours when sulfide is pu'seut. Optionally, all dimples m.i\
lie lesied with lead a< elate pa|x i Ix-foir ihe pi I adjustment in oidei Ic* tlcierinin«* if sullide
is picscni. II sulfide is picscni. ii can l»e removed by ihe addition of cadmium nitrate
|M»wdn until a negative spot lest is obtained. Tin- sample it filtered and ihen NaOH is
added lo pi! 12.
8. Si vim pies fiom iton-t hloi inated dunking watei supplies cone. HjSO* should beaddrd
lo lowei sample pi! lo liv» than 2. The sample should Ix- analyzed before 14 days.
-------
APPENDIX G
U.S. EPA Region 9
CLP Paperwork Instructions
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Revision: 4
Date: 11/4/92
Page: 1 of 13
0. S. EPA REGION 9
CLP PAPERWORK INSTRUCTIONS
1 ORGANIC and INORGANIC TRAFFIC REPORT/CHAIN-OF-CUSTODY RECORD
1.1 CASE DOCUMENTATION
Complete these forms when collecting RAS or RAS+SAS samples.
Enter the SAS number (for RAS+SAS analysis only) and/or Case
number at the top right of the form. Case numbers have the format
"xxxxx" (i.e. 18123) and SAS numbers have the format "xxxx-Y-xx"
(i.e 6123-Y-Ol).
NOTE: Do not use these numbers as sample numbers. Use the RAS
sample numbers provided on the printed labels.
Complete the boxes in the header, as follows:
1.1.1 Box 1 - PROJECT CODE/SITE INFORMATION
Enter the Project Code (i.e $F), Site Name, City, State,
Site Spill ID. (Note: the information entered here does not
go through to the laboratory's copies.)
If sampling is not under the Superfund program, enter the
Account code (account to be billed), any Regional
Information and the name of the program, i.e. RCRA, in the
box titled "Non-Superfund program."
1.1.2 Box 2 - REGIONAL INFORMATION
Enter the Region number, the name of your sampling company,
and your name and signature in the designated spaces.
1.1.3 Box 3 - TYPE OF ACTIVITY
Check the Funding Level of sampling. Next, check the code
which describes the task of the sampling mission.
Fundlne Level
SF - Superfund
PRP - Potential Responsible Party
ST - State
FED - Federal
CLPPAPER.SOP
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Date: U/V93
Page: 2 of 13
Pre-Remedial
PA - Preliminary Assessment
SSI - Screening Site Investigation
LSI - Listing Site Investigation
Remedial
RIFS - Remedial Investigation Feasibility Study
RD — Remedial Design
O&M — Operations and Maintenance
NPLD - National Priorities List
Removal
CLEM — Classic Emergency
REMA — Removal Assessment
REM — Removal
OIL — Oil Response
UST — Underground Storage Tank Response
1.1.4 Box 4 - SHIPPING INFORMATION
Enter the date shipped, the carrier (i.e. Federal Express)
and the air bill number in the appropriate spaces.
1.1.5 Box 5 - SHIP TO
Enter the name of the laboratory contact (i.e. Sample
Custodian), laboratory name and full address.
1.1.6 Box 6 - PRESERVATIVE
This box provides a list of commonly used preservatives.
Enter the appropriate preservative in Column D. If you
enter "5" on the Organic Traffic Report or "7" on the
Inorganic Traffic Report indicating "Other", specify the
preservative used at the bottom of the "Sample
Documentation" area.
If you are using more than one type of preservative, you may
either note the preservatives in the box specifically under
the requested analyses (i.e. in the Cyanide box enter "2")
or list them, separated by commas, in the same order as the
checked sample analyses. (Atlernatiyely, the analysis may
be listed on separate lines.)
CLPPAFER.SOP
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Date: 11/4/92
Page: 3 of 13
1.1.7 Box 7 - SAMPLE DESCRIPTION
This box provides a list of the description/matrices of the
samples that are collected. Enter the appropriate
description in Column A.
1.2 SAMPLE DOCUMENTATION
1.2.1 SAMPLE NUMBERS
Carefully transcribe the RAS sample numbers from the printed
labels onto the Organic or Inorganic Traffic Report/Chain-
of-Custody in the column labeled "CLP Sample Numbers."
Each RAS sample is assigned a unique sample number. A RAS
sample is comprised of one matrix from one station location
for one analytical program going to one laboratory.
For example, if RAS water samples are collected from the
same location for both volatile and pesticide analysis and
are sent to the same laboratory, they are given the same
sample number. However, if these samples are sent to
different laboratories, they must be given different RAS
sample numbers.
RAS sample numbers have the following formats: YX123 for
organic and MYX123 for inorganic samples. Use RAS sample
numbers for RAS+SAS analysis.
1.2.2 Column A - SAMPLE DESCRIPTION
Enter the appropriate sample description code from Box 7.
NOTE: Describe water blanks as "Leachate" (#3) and soil
blanks as "Rinsate" (#4).
Note: Item #6 "Oil" and Item #7 "Waste" are for RAS+SAS
projects only. Do not ship oily samples or waste samples
without making prior arrangements with the RSCC coordinator
and SMO.
1.2.3 Column B - CONCENTRATION
Enter "L" for low and "M" for medium concentration samples.
(Prior arrangements must have been made with the RSCC
coordinator, SMO and the laboratories accepting the samples
before shipping medium concentration samples. At this time,
CLPPAPER.SOP
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Date: 11/4/92
Page: 4 of 13
high concentration samples must be scheduled through the SAS
system.)
NOTE: Medium concentration samples must be shipped in metal
cans.
1.2.4 Column C - SAMPLE TYPE COMPOSITE/GRAB
Enter the type of sample you collected. A composite is a
sample composed of more than one discrete sample. A grab is
a discrete sample.
1.2.5 Column D - PRESERVATIVE USED
Enter the preservative used from Box 6.
1.2.6 Column E - RAS ANALYSIS
Check the analytical fractions requested for each sample,
for example, VOAs, BNAs and Pesticides/PCBs are for
low/medium concentration organics. Total metals and cyanide
are for low/medium concentration inorganics.
NOTE: Both total and dissolved metals can be requested for
each individual inorganic sample, however, they must be
assigned different sample numbers. If cyanide is also
requested, it is given the same sample number(s) as the
total metals sample(s).
Note: ARO/TOX analyses can only be requested for high
concentration samples.
1.2.7 Column F - REGIONAL SPECIFIC TRACKING NUMBERS OR TAG NUMBERS
Region 9 does not issue tracking numbers or tag numbers.
Samplers may use this column for sampler specific tracking
numbers or for "Special Instructions". If you choose to use
this as "Special Instructions", be sure to note, at the
bottom of the "Sample Documentation" area, what the special
handling is. The number and type of containers could be
entered here. (i.e. 3-40 mL, 6-1L)
1.2.8 Column G - STATION LOCATION NUMBER
Enter the station location in the space provided.
Cl.PPAFER.SOP
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Revision: 4
Date: 11/&/9?
Page: 5 of 13
1.2.9 Column H - MO/DAY/YEAR/TIME OF SAMPLE COLLECTION
Record the month, day, year and time (use military time,
i.e. 1600 - 4:00 pm) of sample collection.
1.2.lOColumn I - SAMPLER INITIALS
Enter your initials.
1.2. llColumn J - CORRESPONDING CLP ORGANIC/INORGANIC SAMPLE NUMBER
Enter the corresponding CLP sample number for organic or
Inorganic analysis.
1.2.12Column K - DESIGNATED FIELD QC
Enter the appropriate qualifier for "Blind" Field QC samples
in this column. (NOTE: All samples must have a qualifier.)
Not a QC Sample
Note: Information entered here is not reproduced onto the
laboratories' copies.
"B" - These are blanks and Include trip blanks (T), field
blanks (F) and equipment blanks (E). Blanks may be
further Identified by the letter in parenthesis. For
example, B(T) indicates that the sample is a trip
blank.
"D" •" These are field duplicates, but do not include samples
designated as laboratory duplicates. The primary
sample is identified with and the duplicate is
give "D" in column K. In addition, the station
locations should also identify the primary and
duplicate samples. For example, MW-1 is the primary
sample and MW-1B is the duplicate sample.
"S" - These are spiked field samples and are generated by
field personnel
Blind Field PC
Qualifier
Blind Blanks
Blind Field Duplicates
Blind Field Spikes
Blind PE Samples
B
D
S
PE
CLPPAFER.SOP
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Revision: 4
Date: 11/4/93
Page: 6 of 13
"PE" - These are performance evaluation samples. They are
spiked samples but are not field samples. They are
usually prepared by other than field personnel.
- all other samples not designated as field QC samples
1.3 -SHIPMENT FOR CASE COMPLETE (Y/N>"
This should reflect the status of the samples scheduled to be
shipped to a laboratory for a specific case. Only when All.
samples scheduled/collected for shipment to a laboratory for a
specific case have been shipped is the case complete.
1.4 "PAGE 1 OF "
This is usually 1. Each cooler is to be accompanied by one or
more Traffic Report/Chain-of-Custody Record form(s) . The form(s)
accompanying each cooler must list only those samples contained in
that cooler.
1.5 "SAMPLE USED FOR SPIKE AND/OR DUPLICATE"
Enter the sample number of the sample designated for spike and/or
duplicate analysis. This is also known as the Laboratory QC
sample. This sample should be included in the first shipment to
the laboratory and In the first shipment for each subsequent
sample delivery group (SDG).
1.6 "ADDITIONAL SAMPLER SIGNATURES"
Record additional sampler signatures that are different from that
in Box 2.
1.7 "CHAIN OF CUSTODY SEAL NUMBER"
Enter the Chain of Custody Seal Number used to seal the cooler, if
applicable.
1.8 "SPLIT SAMPLES ACCEPTED/DECLINED"
The sampler should ask the sight owner, PRP, etc. whether they
want split samples taken. The split samples are either accepted
or declined. Record their signature and check the appropriate
box.
1.9 Instructions summarizing CLP sample volumes, packaging and
shipment reporting requirements are printed on the back of the
Traffic Reports.
CLPPAFER.SOP
-------
A
^ A United Starts Environmental ProtectionAoency OrQ&fliC TrdfflC RODOrt
PA « Chain of Custody Record
1 ' * 703-557-2490 FTS 557-2490 (for Oroanic CLP Analysis)
SASNo.
(it applicable)
Case N0.1
/zsys1
1. Project Code
Account Code
2. Region No.
9
Sampling Co.
ACS
4. Date Shipped Carrier .
q-jLhi/ £/
6. Preser-
vative
tCnter In
Column D)
1. HQ
2.HN03
3. NaHS04
4. H2SO4
5. Other
(Spedfy)
6. ice only
N. Not
preserved
7. Sample
Description
(Enter
in Column A)
1. Surface Water
2. Ground Water
3. Leachate
4. Rlnaate
5. Soil/Sediment
6. Oil (High only)
7. Waste (High only)
8. Other
(Specify)
Regional Information
Sampler (NameJ •> f.
AlrblN Number
fZ3 7??0
Non-Superfund Program
Sampler Signature
OJbuJu
5.ShipTo^ jttfptoL- &e*£F)
y/boo?
A
(s>
j ,
/j^
/
r^/oS
093d
%r
mYMD
y/hcx>9
¦2
A
6
U
t
•
?
k/tl/4/ /£>CO
w
mvi3i
—.
YA0/O
A
L
a
L
i
•
Mbd-I
i/xbi //co
4r
mx/dx
•—
Shipment (or Case
complete? (Yflflp
Page 1 of '
Sample used for a spike and/or duplicate Additional Sampler Signatured
VA OO / J\
Relinquished by: ((Signature)
Date / Time
Received by: (Signature)
Relinquished by: (Signature)
Date/Time
Received by: (Signature)
Relinquished by: (Signature)
Date / Time
1
Received by: (Signature)
Relinquished by: (Signature)
Date/Tims
Received for Laboratory by:
(Signature)
Date/Time Remarks la custody seal Intact? Y/N/none
1
EPA Form 9110-2
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Revision: A
Date: 11/4/92
Page: 7 of 13
2 SAS PACKING LIST/CHAIN-OF-CUSTODY FORM
2.1 CASE DOCUMENTATION
Complete this form when collecting SAS samples.
Enter the SAS number at the top right of the form. SAS numbers
have the format "xxxx-Y-xx" (i.e 6123-Y-01).
NOTE: Do not use this number for sample numbers. Use the SAS
sample numbers provided on the printed labels.
Complete the boxes in the header, as follows:
2.1.1 Box 1 - PROJECT CODE/SITE INFORMATION
Enter the Project Code (i.e $F), Site Name, City, State,
Site Spill ID. (Note: the information entered here is not
reproduced onto the laboratory's copies.)
If sampling is not under the Superfund program, enter the
Account code (account to be billed) , any Regional
Information and the name of the program, i.e. RCRA, in the
box titled "Non-Superfund program."
2.1.2 Box 2 - REGIONAL INFORMATION
Enter the Region number, the name of your sampling company,
and your name and signature in the designated spaces.
2.1.3 Box 3 - TYPE OF ACTIVITY
Check the Funding Level of sampling. Next, check the code
which describes the task of the sampling mission.
Funding Level
SF - Superfund
PRP — Potential Responsible Party
ST - State
FED - Federal
Pre-Remedial
PA — Preliminary Assessment
SSI - Screening Site Investigation
LSI - Listing Site Investigation
CLFPAPER.SOP
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Date: 11/4/92
Page: 8 of 13
Remedial
RIFS - Remedial Investigation Feasibility Study
RD - Remedial Design
O&M - Operations and Maintenance
NPLD - National Priorities List
Removal
CLEM - Classic Emergency
REMA - Removal Assessment
REM - Removal
OIL — Oil Response
UST - Underground Storage Tank Response
2.1.4 Box 4 - SHIPPING INFORMATION
Enter the date shipped, the carrier (i.e. Federal Express)
and the air bill number in the appropriate spaces.
2.1.5 Box 5 - SHIP TO
Enter the name of the laboratory contact (i.e. Sample
Custodian), laboratory name, and full address.
2.1.6 Box 6 - SAMPLE DESCRIPTION
This box provides a list of the description/matrices of the
samples that are collected. Enter the appropriate
description In Column A.
2.1.7 Box 7 - PRESERVATIVE
This box provides a list of commonly used preservatives.
Enter the appropriate preservative in Column C. If you
enter "6" indicating "Other", specify the preservative used
at the bottom of the "Sample Documentation" area.
2.2 SAMPLE DOCUMENTATION
2.2.1 SAMPLE NUMBERS
Carefully transcribe the SAS sample numbers from the printed
sample labels onto the SAS/COC in the space provided.
Each SAS sample is assigned a unique .sample number. A SAS sample
consists on one matrix from one station location for one analysis
going to one laboratory.
CLPFAPER SOP
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Revision: 4
Date: 11/4/92
Page: 9 of 13
For example, if SAS water samples are collected from the same
location for both herbicide and anion analysis and are sent to the
same laboratory, they are given the same SAS sample number.
However, if these samples are sent to different laboratories, they
must be given different SAS sample numbers.
SAS sample numbers have the format SYxxxx (i.e. SY1234).
2.2.2 Column A - SAMPLE DESCRIPTION
Enter the appropriate sample description code from Box 6.
2.2.3 Column B - CONCENTRATION
Enter "L* for low concentration, "M" for medium
concentration and "H" for high concentration.
NOTE: Medium and high concentration samples must be shipped
in metal cans.
2.2.4 Column C - PRESERVATIVE USED
Enter the preservative used from Box 7.
If more than one type of preservative is used for a sample,
separate the preservative reference numbers with commas.
The sequence of the reference numbers must follow the
sequence of the requested "SAS Analysis" parameters that are
recorded in Column D.
2.2.5 p - ANALYSIS
Enter the analysis requested.
2.2.6 Column E - REGIONAL SPECIFIC TRACKING NUMBERS OR TAG NUMBERS
Region 9 does not issue tracking numbers or tag numbers.
Samplers may use this column for sampler specific tracking
numbers or for "Special Instructions". If you choose to use
this as "Special Instructions", be sure to note, at the
bottom of the "Sample Documentation" area, what the special
handling is. The number and type of containers could be
entered here (i.e. 6-1L).
2.2.7 Column F - Station Location Number
Enter the station location in the space provided.
CLPPAPER.SOP
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Date: 11/4/92
Page: 10 of 13
2.2.8 Column G - Mo/Day/Year/TLme of Sample Collection
Record the month, day, year and time (use military time,
I.e. 1600 - 4:00 pm) of sample collection.
2.2.9 Column H - Sampler Initials
Enter your initials.
2 .2. lOColuunn I - Designated Field QC
Enter the appropriate qualifier for "Blind" Field QC samples
in this column. (NOTE: All samples must have a qualifier.)
Blind Field PC Qualifier
Blind Blanks B
Blind Field Duplicates D
Blind Field Spikes S
Blind PE Samples PE
Not a QC Sample
Note: Information entered here is not reproduced onto the
laboratories' copies.
"B" - These are blanks and include trip blanks (T), field
blanks (F) and equipment blanks (E). Blanks may be
further identified by the letter in parenthesis. For
example, B(T) indicates that the sample is a trip
blank.
"D" - These are field duplicates, but d.o iriot Include samples
designated as laboratory duplicates. The primary
sample is identified with and the duplicate is
give "D" in column K. In addition, the station
locations should also identify the primary and
duplicate samples. For example, Mtf-1 is the primary
sample and Mff-IB is the duplicate sample.
"S" - These are spiked field samples and are generated by
field personnel
"PE" - These are performance evaluation samples. They are
spiked samples but are not field samples. They are
usually prepared by other than field personnel.
- all other samples not designated as field QC samples
CLPPAPER.SOP
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Revision: 4
Date: 11/4/92
Page: 11 of 13
2.3 "SHIPMENT FOR CASE COMPLETE (Y/N)"
This should reflect the status of the samples scheduled to be
shipped to a laboratory for a specific case. Only when ALL
samples scheduled/collected for shipment to a laboratory for a
specific case have been shipped is the case complete.
2.4 "PAGE 1 OF "
This is usually 1. Each cooler is to be accompanied by one or
more Packing List/Chain-of-Custody form(s). The form(s)
accompanying each cooler must list only those samples contained in
that cooler.
2.5 "SAMPLE USED FOR SPIKE AND/OR DUPLICATE"
Enter the sample number of the sample designated for spike and/or
duplicate analysis. This is also known as the Laboratory QC
sample. This sample should be Included in the first shipment to
the laboratory and in the first shipment for each subsequent
sample delivery group (SDG).
2.6 "ADDITIONAL SAMPLER SIGNATURES"
Record additional sampler signatures that are different from that
in Box 2.
2.7 "CHAIN OF CUSTODY SEAL NUMBER"
Enter the Chain of Custody Seal Number used to seal the coolers,
if applicable.
2.8 "SPLIT SAMPLES ACCEPTED/DECLINED"
The sampler should ask the sight owner, PRP, etc. whether they
want split samples taken. The split samples are either accepted
or declined. Record their signature and check the appropriate
box.
2.9 Instructions summarizing CLP sample volumes, packaging and
shipment reporting requirements are printed on the back of the
Traffic Reports.
CLPPAPER.SOP
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JSL D A c«!2X^tf%Z&ZS£®S5a». „jcial Analytical Service
\#l_r r\ P«*ln9Ua/Ctaol Custody
SAS No.
6/#3-y-a/
1. Project Code
4?
Account Code
2. Region Nc
9
>. Sampling Co.
Ate
4. Date Shipped Carrier
9'At-Qt F&i
6. Sample
Description
(Enter
in Column A)
1. Surface Water
2. Ground Water
3. leachate
4. Rinsate
5. Soil/Sediment
6. Oil
7. Waste
8. Other
(Specify)
7. Preservative
(Enter In Column C)
1.HCI
2. HN03
3. NAHSO4
4. H9SO4
5. NAOH
6. Other
(Specify)
7. Ice only
N. Not preserved
Regional Information
Sampler (Name)
£lark Merit
Airbill Number
t&3 e
Site Name
"Tex/C tOa.S'te
3. Type of Activity Ramditi rmdmi
ifi Pr»- R1FS mCLEM|—I
SF IS FU™dW RD REMA
prpPIpai Ira ~ rem Z
ST ~SSQOiM OIL _
fedlZjlsOnplo_ ust lI
City, State Site Spill ID
Srnaliwlle (LA £&
Sample
Numbers
A
Matnx
Enter
from
Box 6
B
Cone
Low
Med
High
C
Preserv-
ative
Used
from
Box 7
0
Analysis
RegionalSpedflc^
Trackjajfflumber
>dag Number
F
Station
Location
Identifier
0
Mo/Oay/
Year/Time
Sample
Collection
H
Sampler
Initials
1
Designated
Field QC
1. svo too
A
L
7
Merb/djde
9/&U/ 6766
.—.
*.£Y0/Ol
#
A
7
/Jerbj&Je /hvM
/MO
9/aift/ 0730
at
3 SVO 102
A
A
7
/J Grb *<*;//*>
JWlU-3
—
4SY0/03
a
A
7
A/erb/C.t4<°
MlO*3&
0tOD
«• SYd/Oi
A
A
7
Merbtpjde
/>/h/dZ
ft "
* SV6/06
cS
3
A
A
*
7
//erbt&tctf . A/vcn
lLaT /&%J/
M/oV
4/zifof CfdO
at
* sit) to? .
2
A
f
/4erb/&d<°
M/OS"
a?3o
® 5V0/0f
a
A
f
//er4>/ii/de s #/>*&>
/MhJ'i
Wto /boo
at
io syo/of
£
A
fi/Arblh
Date / Time
9/%fe; | /%»
Received by: (Signature)
/33?S&7SPf
Relinquished by: (Signature)
Date / Time
1
Received by: (Signature)
Relinquished by: (Signature)
Date/Time
Received by: (Signature)
Relinquished by: (Signature)
Date / Time
Received by: (Signature)
Relinquished by: (Signature)
Date / Time
Received (or Laboratory by:
(Signature)
Date / "Time
Remarks Is custody seal Intact? Y/N/none
EPA Form: 91104(7/91}
DISTRIBUTION: White • Region Copy Yallow • 8MO Copy Oold • Lab Copy lor Return to flaglon
Pink- Lab copy tor Returnto8IIO
Sn Reverse Side far Additional Standard Inetructlonfe
Split Samples Q Accepted (Signature)
1 lOedlned
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Revision: 4
Date: U/VP2
Page: 12 of 13
3 FIELD OA/OC SUMMARY FORM
3.1 Complete one form per laboratory per matrix for each sampling
event. For long term projects, complete a form(s) after each
month of sampling. Complete the header portion even if no QA/QC
samples were provided.
3.2 Complete all applicable entries. Please use the appropriate
sample numbers for each laboratory, (i.e. For the laboratory
performing the RAS organics, use the CLP organic sample numbers,
YX123, etc. For the laboratory performing the SAS analyses, use
the SAS sample numbers, SY0123, etc.) Please do not use station
locations. If a laboratory is performing more than one type of
analyses, list all applicable sample numbers. (For example, if a
laboratory is doing both RAS organics and SAS organics, list both
numbers separated by-a backslash, YX123/SY0123 or list the two
sample number on-separate lines.)
3.3 This form is very important for validation purposes. The
validators will compare the results of duplicates and assess the
quality of blanks, if they know which samples they are. The lack
of this information will delay the completion of the validation.
4 SAMPLE BOTTLES
4.1 Sample bottles be labeled with the following Information:
a.
Case or SAS number
b.
Date/Time of collection
c.
Matrix/Concentration
d.
Station Location
e.
Sample number (from the pre-printed labels)
f.
Analysis
g-
Preservative
4.2 Pre-printed, self-adhesive labels are provided for RAS Organic,
RAS Inorganic and SAS samples. See Sections 1.2.1 and 2.2.1 for
the proper assignment of sample numbers.
4.2.1 Transcribe the appropriate sample number onto the
corresponding bottle label and/or affix the sample number
label onto the bottle.
4.2.2 Destroy all unused labels or return them to the RSCC
coordinator. DO NOT use them on future samplings. New
sample number will be assigned..
CLPPAPER.SOP
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FIELD OVQC SIMtfJOf PCFH
Instruction: Ccn^lete ooe fooa per laboratory and per natrix for each sanpling event.
rute. 9/fri/<7/ Site: ~7c*'C
Savler;_^r^_^J2t. Case/SAS I» -/-0 /
Office: Laboratory: /&/?Azt -.
Fhone I; (f7
Matrix: X'Groundwater Surface Soil Air
(check one) Surface Water Subsurface Soil Other
I. BLAMCS
Sample I
yfK>o7
SIO/fiL
SV6/67
II. BACKGROUND SAMPLES
Type (circle one)
Equip / Field / t^yel)
Equip /^flel^)/ Travel
Equip // Travel
Equip /(field)/ Travel
Equip /^Fiehj)/ Travel
Equip / Field / Travel
Equip / Field / Travel
Equip / Field / Travel
Equip / Field / Travel
Equip / Field / Travel
Etjuip / Field / Travel
Equip / Field / Travel
Date Collected
Wz/Zf/
t/zi/?/ '
Sample I
Date Collected
III. foB OC SAMPLES
Sample I
Vd-6o/
SY6/0/
Date Collected
¦?/&/?/
IV. DUPLICATES
Sample f Matches Sample ( Date Collected Type (circle one)
£>¥ Woa 3 ?•£//?/
a XS/c/6
a « composite split
sva/A? Sva/cZ
*#£/ c/d
b * consecutive
a / b / c / d
c e colocated
a / b / c / d
d * consecutive
a / b / c / d
soil sleeves
a/b/c/d
'• Checklist of Field Problems Encountered
_^°e Sample I / Date(s) of'Occurrence / Corm>ents
Pimping Equipment Problems
Sanple Filtering Problems
Less Than Required Sample \blune
Lev Flcv/fcecharye Rates
Preservation Prcblea
_^jSaaples Nat Shipped in 24hrs.
Federal Express Delay
-------
Revision: 4
Date: 11/4/92
Page: 13 of 13
DISTRIBUTION OF COPIES
5.1 ORGANIC TRAFFIC REPORT/CHAIN-OF-CUSTODY FORM
a. Blue (original) copy to QAMS, Region 9
b. Pink (second) copy to SMO
c. White (third) and Yellow (fourth) copies accompany samples
to laboratory
d. Photocopy for sampler's files
5.2 INORGANIC TRAFFIC REPORT/CHAIN-OF-CUSTODY FORM
a. Green (original) copy to QAMS, Region 9
b. Pink (second) copy to SMO
c. White (third) and Yellow (fourth) copies accompany samples
to laboratory
d. Photocopy for sampler's files
5.3 SAS PACKING LIST/CHAIN-OF-CUSTODY FORM
a. White (original) copy to QAMS, Region 9
b. Yellow (second) copy to SMO
c. Pink (third) and Gold (fourth) copies accompany samples to
the laboratory
d. Photocopy for sampler's file
5.4 FIELD QA/QC SUMMARY FORM
5.5
a.
b.
Original to QAMS, Region 9
Photocopy for sampler's files
When all paperwork has been completed by the sampler and samples
are ready to be shipped, place the laboratories' copies in a
plastic bag and tape it to the inside of the lid of the cooler(s).
SMO's copies must be submitted within 5 days of sampling. The
Region's copies may be submitted at that time or at the end of the
sampling event. If the sampling event covers an extended length
of time, the Region's copies must be submitted monthly. (Note:
The RSCC will not forward SMO's copies. They will be returned to
the sampler.)
QAMS address:
U.S. EPA Region 9
Quality Assurance Management
Section (P-3-2)
75 Hawthorne Street
San Francisco, CA 94105
Attn: RSCC Coordinator
SMO address:
Sample Management Office
P. 0. Box 818
Alexandria, VA 22313
Attn: Region 9
Coordinator
CLPPAFER.SOP
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