Preparation of a
U.S. EPA Region 9 Field Sample Plan
for
EPA-Lead Superfund Projects
Quality Assurance Management Section
U.S. EPA, Region 9
August, 1993
(Document Control No. 9QA-05-93}
REVISED APPENDIX G
October, 1994
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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
rA\ REGION IX
XSS£ I 75 Hawthorne Street
li-Ht^ Smn Franclsco» CA 9410S
MEMORANDUM
DATE:
SUBJECT:
FROM:
THROUGH:
TO:
December 16, 1992
Revised Region 9 guidance for preparation of
>ling plans for EPA-lead Superfund projects
1 Scientist
it Section, P-3-2
Section, P-3-2
ny Environmen
Quality. Assurance Manag
Kent Kitchingman, Ch
Quality Assurance Manag
Superfund Remedial Proj'ectyManagers, H-6-1, H-6-2,
H-5-3, H-6-4, H-7-1, H-7-2
Superfund Site Assessment Managers, H-8-1
Superfund Project Officers, H-8-2
The following is a summary of the changes in the Region 9 sampling
plan guidance revised in November 1992.
The roost significant change in the guidance is the new SAS
procedure. other significant changes involve the preservation
protocol for volatile organic samples and the required inclusion of
the CERCLIS identification number in the Request for Analysis
section.
Please ensure that your contractors (EPA-lead sites, anyone using
the CLP) are aware of this revised field sampling plan guidance.
Sample Plan Training will be conducted in the near future. Contact
Robbie Hedeen at 415/744-1535 to request this training or for any
questions concerning the sample plan guidance.
1. New SAS Request
Section V: Request for Analysis
A: The entire Narrative Request for Analysis section
has been revised to reflect the preparation of new
Special Analytical Services (SAS) Client Request
Forms (CRFs) , the procedures for obtaining and
using ^generic" SAS CFRs, and the requirements for
inclusion of SAS CRFs in sampling plans.
Appendix D: Contains the SOP for completing or creating a
new SAS CRF.
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y revisions^
introduction: Paragraph 7 clarifies the required sections of an
amendment to an existing sample plan. The
requirements include an entire Request for-
Ana-lysis section complete with all SAS CRFs.
Section V: Request for Analyses
Paragraph 4 provides updated examples of RAS+SAS
analyses? Low quantitation limit (25 ml purge)
volatile analysis and RAS analyses with
additional compounds are no longer considered
RAS+SAS. They have been redefined by SMO as SAS
analyses.
Section V.A: Marrative Request for Analyses
Paragraph 1 requires that the Site CERCLIS ID is
included in the paragraph summarizing the lab
analyses to be performed.
Section VI. D: Field Methods and Procedures
Sample Containiers
A notice regarding the collection of soil samples
in metal sleeves has been added.
Bibliography: The bibliography has been expanded.
Appendix A: Contains an expanded ESB Referral List.
Revised Field Investigation Flow Chart.
Appendix B: Revised Sampling Plan Cover Sheet format.
* *
Appendix C: Contains an updated Target Compound List.
Appendix D: Contains the SAS CRF SOP, including examples.
Appendix F: Revised VOA preservation procedure.
Contractual and Analytical Holding Times are
defined.
Appendix G: Current CLP Paperwork instructions.
Superseded by '"Instructions for Sample Shipping and
Documentation" (October, 1994)
cc: Super fund Section Chiefs (except H-7-4)
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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
6) Sample Documentation 11
H) Quality Control Samples 11
Section VII - Health and Safety Plan 13
Bibliography 14
APPENDICES
Appendix A. Environmental Services Branch Referral List
Field Investigation Flow Chart
Appendix B. Sample Plan Cover Sheet
Appendix C. CLP Target Compound List and Quantitation Limits
Appendix D. SAS Client Request Form SOP and Examples
Request for Analysis Example Table
Appendix E. Sample Container Requirements for CLP Analyses
Appendix F. 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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TKTRODnCTIOH
* The purpose of the Field 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 As-
surance Management Staff to contract for laboratory
analyses.
This guidance document describes the requirements for con-
tractors and EPA staff preparing Field 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 Field 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 Field Sample Plan
preparation are listed below.
* The Field Sample Plan is a "stand alone" document. DO NOT
INCLUDE IT AS PART OF ANY OTHER DOCUMENT!!i
* The Regional guidelines for preparing Field Sample Plans and
QA Project Plans (QAPjPs) are designed to minimize overlap
between the two documents. As a result, some QAPjP elements
which are also required in the Field Sample Plan may be ad-
dressed in the QAPjP by reference to the Field Sample Plan.
The Field Sample Plan, however, may not reference field pro-
cedures in the QAPjP or any other document, except as back-
ground information.
Separate Field Sample Plans must be prepared for every sam-
pling episode. An exception may be granted to Field Sample
Plans for periodic monitoring, such as quarterly groundwater
monitoring, or when a new sampling proposal involves the
same techniques as a previous Field Sample Plan. In both
cases, an amendment to an existing Field Sample Plan is re-
quired. 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 re-
^HSc*c°^?nalysis section including the narrative, table,
and SAS Client Request Forms. Call QAMS to determine if a
new Field Sample Plan is required or for more information on
the requirements of a Field Sample Plan amendment.
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The Field Sample Plan is reviewed and approved by QAMS and
the EPA Remedial Project Manager. She normal turnaround
times for Field 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.
OAKS 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 QAPP. Alloy
,
review and time f^ »»v revisions. (Also see Sec-
tion VI.)
See page 14 for a bibliography of useful references for
preparing a Field Sample Plan.
REQUIRED FIELD SAMPLE PLAN SECTIONS
COVER SHEET (EPA format required)
Section I - OBJECTIVE
Section II - BACKGROUND
Section III - MAPS
Section IV - RATIONALE FOR SAMPLE LOCATIONS, NUMBERS OF
SAMPLES, AND ANALYTICAL PARAMETERS
Section V - 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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COVER SHEET (EPA format is REQUIRED!
The cover sheet is a record of the review and approval of
the Field Sample Plan. A copy of the required format is in-
cluded in Appendix B.
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.
Ill 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 SAMPIE LOCATIONS. NUMBERS OF SAMPUiS.
& ANALYTICAL PARAMETERS '
* This section describes in detail how the Field Sample Plan
will meet the stated objectives. It covers the what, where
and why of the Field Sample Plan as discussed below.
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c
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 veils) are excluded, explain why.
Discuss the rationale for the analytical parameters. The
rationale must relate to site history and the objectives of
the Field Sample Plan. Justify requests for low guantita-
tion limits. Give an explanation when not all samples from
the same matrix will be analyzed for the same parameters.
Identify site indicator compounds and other parameters of
most interest. Discuss relevant action levels, especially
when low guantitation 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 PAS 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. F
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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 Field 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. .
A. 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
?VfV? outdated SAS CRFs, the CRFs will not be dis-
tributed in compendium form. Always contact QAMS to ensure
JtmVJS'iL?S'd ^ (e'?-< f°r «"«*«*ly monitoring) s
still the most recent revision for a particular analysis.
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OAKS will also maintain a file of SAS CRTs 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 CRT, review it to make sure
all sections are applicable to your project. Changes to the
Generic SAS CRT 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 CRT. 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 CRT 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 nay 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 Field Sample Plan writing and to standardize
these routine practices, contractors are encouraged to
develop standard Operating Procedures (SOPs) for some of
these procedures.
* 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 Field Sample Plan,
preferably incorporated directly into the text of the ap-
propriate section. The SOP must be directly applicable, as
written, to the Field 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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A. 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 narked 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 Field 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 Field
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 Field Sample Plan. Alternatively, this
information may be provided for QAMS review in a separate
document, such as a work plan or QAPP, prior to preparation
of the Field 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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B. 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.
c. 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.
D. 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.
E. Sample Preservation
* Describe sample preservation methods in step by step detail.
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.)
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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6. sample Documentation
* Discuss the use of all paperwork, including field notebooks,
record logs, photographs, CLP sanple 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 Field 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.
H. Quality Control Samples
1. 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
yolatiles 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-
milst Mmnles. or when it is necessary to determine the
Secision*«nd/o? accuracy of field analytical methods by
Slittina a percentage of samples with a fixed laboratory.
Se saSle cSJlectioS procedures should be identical to col-
lecting duplicates.
2. 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. ^
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.
* Por 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 PIAN
* 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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«* uaeftii references for preparing a
iM«id operation Methods, EPA 540/P-
87/OOla & OOlb, August 1987
p.*. o«»litv Qh^etives fnr Remedial FeSPQnse AgtJVitJes, two
volumes" EPA 540/G-87/003 and 1004, March 1987.
yiald screening Methods e^loa Pser^s Guide. EPA Office of Emer-
gency and Remedial Response, EPV54 0/2-88/005, September 1988.
Handhooie for sairoiina and sample Preservation of Water anfl Was-
tewater. EPA-600/4-82-029, September 1982.
Methods for ghenieal 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 Protocols 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/ 6 00/4 -9 0/0 13, 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 Wastevater.
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.
14
-------
APPENDIX A
Environmental Services Branch
Referral List
and
Field Investigation Flow Chart
(08/93)
-------
ENVIRONMENTAL SERVICES BRANCH REFERRAL LIST
May 1994
onmental Services Branch (ESB) P-3
(415) 744-1523
412-2311
ratory Section (LS) P-3-1
ty Assurance Management Section (QAMS)"P^2
510]
744-1492
CONTACT
TELEPHONE
JECT
PRIMARY CONTACT LISTED FIRST
Jim Whittaker/Kira Lynch
Methods
HedyFiddin/Rich Bauer
(510) 412-2319/744-1496
imate Test Procedures (ATP)
744-1492/1499
>estos
Km Lynch
744-1496
HedyRckfin/KenHendrix
744-14927(510) 412-2321
mic Absorption (AA)
assays/Toxicity Tests
Peter Husby/Clance OteonVHedy FickBn
(510)412-2331/2330/744-1492
arine Toxidty Tests:
Amy Wagner/Peter Husfay
(510)412-2329/2331
assessments/Ecoassessments
Peter Husby/ Stewart Sanpson
(510)412-2331/2333
itract Laboratory Program (CLP)
eneral Information/Laboratory Audits
Steve Remaley
744-1527
ihedulmg Analyses:
Rich Bauer
744-1499
Dedal Analytical Services(SAS) Requests
IHedyFJckBn
744-1492
a Quality Objectives (DQO)
Hedy Rckfin/Kira Lynch
744-1492/1496
a Review/Validation Procedures
Rich Bauer/Bill KessJer
744-1499/1528
:a Review Project Status
Rich Bauer
744-1499
:ection Limits
(Rich Bauer/Jim Johnson
744-14997(510) 412-2336
ion
R-QA PE Studies
Jam Johnson/Steve Remaley
[510) 412-2336/744-1527
Stewart Simpson
[510)412-2333
R-QAToxicity
Amy Wagner
(510)412-2329
R-QA Follow-up Inspections
:ument Review
Jm Johnson/Peter Husby
[510) 412-2336/2331
HedyRckfin
744-1492
iking Water Methods
Jim Johnson/Rose Fong
(510)412-2336/744-1534
iking Water Labs
/ironmental Monitoring Methods Index (EMMI)
Jim Johnson/Clarice Olson
[510)412-2336/2330
Hedy Hcldin/Jim Johnson
744-1492/(510) 412-2336
SPLab
Stewart Simpson
[510)412-2333
Id Audits, Request For
Id Audits Quality Assurance
Stewart Simpson
[510) 412-2333
Kira Lynch
744-1496
Id Sampling Plans (FSPs)
tedy Rckfin/Kira Lynch
'44-1492/1496
3ls Analyse
4edy Fiddin/Rich Bauer
744-1492/1499
Chromatography/Mass Spectrometry (GC/MS
Steve Remaley/Jim Johnson
744-1527/(510) 412-2336
^graphic Information System (GIS)
sitioning System (GPS)
foseanne Sakamoto
744-1535
Stewart Simpson
510)412-2333
jsessment
actively Coupled Plasma (1CP)
ratory Audits/Oversight
DES Laboratory Audits
joratory Certification - Chemistry
moratory Certification - Microbiology
nagement System Reviews (MSR)
tals L
bile Lab Services
:ro biology
tody Rcklin/Pat Mack
Jim Whittaker
BfllKessler
r44-1492ffS10T412-2312
510)412-2319
Stewart Simpson
'44-1528
8m Johnson/Pat Mack
aarice Olson/Jim Johnson/Pat Mack
HedyHcklin "
510) 412-2333
510)412-2336/2312
510) 412-2330/2336/2312
Hedy FickBn/Ken Henditt
744-1492
n-Superfund Analytical Services
ganic Methods
'eterHusby/Stewart;
>at Mack/Clarice Oteon/Hedv Fickfm
sticides
Bs
trenda Bettencourt
Jim Johnson/Steve Remaiev"
HedyRckfin
im Johnson/James Whittaker
'44-14927(510) 412-2321
510)412-2331/2333
12-2312/2330/744-1492
ality Assurance
> Project Plans (QAPjPsV
ion-$F
Hedy Fiddin/Kiia Lynch
ick Turnaround Method (Q
(510)412-23360319
'10)412-2336
'44-1492/1496
r44-1492/1496"
r44-1534/1496
'44-1492
-------
BJECT
adionudides
CRA Issues
ample Containers
ample Holding Times/Preservation/Containers
ampling: Drin ting Water
Fish
Groundwater
Microbiology/Virology
NPOES
Soil/Sediment
Surface Water
Waste (Solid)
Dial Quality Management i TQM)
oxidty Cnarateristic Leaching Procedure (TCLP)
'ater Pollution PE Studies (WP)
'ater Supply PE Studies (WS)
CONTACT
PRIMARY CONTACT USTEORRST
Jim Johnson
Rich Bauer/Stewart Simpson
Roseanne Sakamoto
Roseanne Sakamoto/Rich Bauer
Stewart Simpson
Stewart Sim son/Peter Husby
Kire Lynch/Roseanne Sakamoto
Clarice Olson
Stewart Simpson/Peter Husby
Stewart Simpson
Kira Lynch
Stewart Simpson/Peter Husby
Stewart Simpson
HedyFickBn
Rich Bauer/Stewart Simpson
Stewart Simpson
Stewart Simpson
TELEPHONE
(510)412-2336
744-14997(510)412-2333
744-1535
744*1535/1499
(510)412-2333
(510) 412-2333/2331
744-1496/1535
(510) 412-2330
(510) 412-2333/2331
(510) 412-2333
744-1496
(510) 412-2333/2331
(510) 412-2333
744-1492
744-1499/(5lO) 412-2333
510) 412-2333
510) 412-2333
OPTIONAL REFERENCES AS SHOWN ON MAY 1993 REFERRAL LIST:
ENVIRONMENTAL SERVICES BRANCH
T. Stumph, Chief
STAFF
EllaMcGefaee, Branch Secretary
Susan Lee (SIS)
RonMerida(SIS)
SAN FRANCISCO
RICHMOND
UALITY ASSURANCE
IANAGEMENT SECTION
Ficklin, Chief (acting)
LABORATORY SECTION
B. Bettencourt Chief
UNCTIONS
sgional Quality Assurance
xbnical Assistance
ocument Review
ontract Management
iboratory Oversight
udits-Ub. Field. MSR
not Review
ata Quality Assessment
raining
SAT Task Coordination
TAFF
-Bauer
-Fong
.Kessler
-Lynch
Remaley
-Sakamoto
FUNCTIONS
Health, Safety and Envin
Purcfaasing(Lab)
Perfonnanoe Evaluation Sfridiq
tialComplu
STAFF
P.Bdanger
J.Mam
J. Rcdwioc
C.Tambwekar(SEE)
C.Hemrich(SEE)
IFffiLD SERVICES TEAM
FUNCTIONS
Sample Collection/Field Work
Field Audits
Field Equipment Management (EMFAC)
Lab Evaluations
Training
ESAT Task Coordination
STAFF
Stewart Simpson (TI.)
J.Johnson
B. dark (SEE)
R. Roberson (SEE)
IBIOLOGYTEAM | [CHEMISTRY TEAM
FUNCTIONS '
Biotogictl Analyses
Training
ESAT Task Coortmation
SIAfE
P.Hasby(TJ-)
COtoon
A.Wi
FUNCTIONS
Chemical Analyses
Quality Assorance
ESAT Task Coordination
STAFF
P. Mack (T.L.)
(LHendnx
J.Wmn*ker
-------
FIELD INVESTIGATION FLOW CHART
Sample Plan Author-^-
revision required
EPA Project Manager (RPM, SAM), ^
for review of
each draft
Quality Assurance Management Section (QAMS)
Sample Plan Approved
Regional Sampling Control Center (RSCC)
CLP Labs Contracted
Sampling Begins
Lab Analyses 35
Data Validation 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.
-------
(08/93)
APPENDIX B
Field Sample Plan Cover Sheet
-------
(08/93)
U.S. ENVIRONMENTAL PROTECTION AGENCY REGION 9
Sample Plan Titles
Site Name:
Site Location!
City/State/Zip*
Site EPA ID ft
Anticipated Sampling Datest
Prepared by* __»^^_
Date
Agency or Firm: _^__^_^____^__^_____^^___^^___
Address:
City/State/Zip:
Telephones ( )
EPA Project Managers Sections
Phone *
QAPjP Approval Date:
s (for EPA use) s
u D
* p
E Received by Superfund Remedial Project Managers _ E
R Date R
F Reviewed by: • _ »- • ' . p
0 Date U
N APPROVED / NOT APPROVED H
D. D
*"**•***•*******•
Expedited Review? Yes/No
Received by Quality Assurance Management Sections
Q
A Reviewed bys _
• ~~ ^~— — —
Date
APPROVED:
Date H
Chief, Quality Assurance Date
Management Section
Environmental Services Branch, OPM
-------
APPENDIX C
CLP Target Compound List
and
Quantitation Limits
(08/93)
-------
TARGET COMPOUND LIST (TCL) AND CONTRACT REQUIRED QUANTITATION LIMITS (CRQL)
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
23.
24.
25.
26.
27.
28.
29.
30.
31.
32.
33.
Volaciles
Chlorome thane
Bromome thane
Vinyl Chloride
Chloroe thane
Methylene Chloride
Acetone
Carbon Disulfide
1 . 1-Dichloroethene
1, 1-Dichloroe thane
1.2-Dichloroethene (total)
Chloroform
1 , 2 -Dichloroe thane
2-Bucanone
1,1, 1 -Tr ichloroe thane
Carbon Tetrachloride
Bromodichlorome thane
1,2- Dichloropropane
cis-1 . 3-Dichloropropcne
Trichloroethene •""
Dibromoehlorome thane
1.1.2 -Trichloroethane
Benzene
CAS Number
74-87-3
74-83-9
75-01r4
75-00-3
75-09-2
67-64-1
75-15-0
75-35-4
75-34-3
540-59-0
67-66-3
107-06-2
78-93-3
71-55-6
56-23-5
75-27-4
78-87-5
10061-01-5
79-01-6
124-48-1
79-00-5
71-43-2
trans -1.3- Dichloropropene 10061 -02-6
Bromoform . 75-25-2
4-Methyl-2-pentanone
2-Hexanone
Tetrachloroethene
Toluene
1.1,2.2 -Tetrachloroethane
Chlorobenzene
Ethyl Benzene
S tyrene
Xylenes (Total)
108-10-1
591-78-6
127-18-4
108-88-3
79-34-5
108-90-7
100-41-4
100-42-5
1330-20-7
Ouantitation
Lev
Water Soil
tiE/L UE/KE
10.
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
.10
10
10
10
10
10
10
10
10
10
10
. 10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
Limits*
Med.
Soil
UE/KE
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
A fc W W
1200
1200
*4b W W
120T>
1200
1200
1200
1200
.1200
1200-
1200
1200
-------
TARGET COMPOUND LIST (TCL) AND CONTRACT REQUIRED QUANTITATION LIMITS (CRQL)
36.
35.
36.
37.
38.
39.
60.
41.
62.
63.
66.
65.
66.
67.
68.
69.
50
51.
52.
53.
56.
55.
56.
57.
58.
59.
60.
61.
62.
63.
66.
65.
66.
67.
68.
Phenol
bts(2-Chloroethyl) ether
2-Chlorophenol
1 . 3 -Dichlorobenzene
1 ,6-Dichlorobenzene
1 . 2 • Diehlorobenzene
2-Methylphenol
2.2'-oxybis
( 1 • Chloropropane )
6-Mcchylphenol
N-Nitroso-di-n-
propylamine
Hexachloroechane
Nicrobenzene
Isophorone
2--Nitrophenol
2 . 6 - D ime chylphenol
bis(2-Chloroethoxy)-
me chane
2 ,6-Dichlorophenol
1.2.6 -Trichlorobenzene
Naphthalene
6-Chloroaniline
Hexachlorobucadiene
6 -Chloro- 3 -me chylphenol
2 -Me chylnaphchalene
Hexachlorocyclopencadiene
2,6, 6 -Trichlorophenol
2.6, 5 -Trichlorophenol
2 - Chloronaphthalene
2-Nicroaniline
Dimethylphthalate
Acenaphthylene
2.6-Dlnicrocoluene
3-Nitroaniline
Acenaphchene
2.6-Dinitrophenol
6-Nitrophenol
CAS Number
108-95-2
111-44-4
95-57-8
541-73-1*
106-46-7
95-50-1
.95-48-7
108-60-1
106-46-5
621-66-7
67-72-1
98-95-3
78-59-1
88-75-5
105-67-9
111-91-1
120-83-2
120-82-1
91-20-3
106-47-8
87-68-3
59-50-7
91-57-6
77-47-4
88-06-2
95-95-4
91-58-7
88-74-4
131-11-3
208-96-8
606-20-2
99-09-2
83-32-9
51-28-5
100-02-7
Ouantttaeton Limits*
Low Med.
Uacer £eJl Soil .
UB/L utflCe ut«e_
10
10
.10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
25
10
25
10
10
10
25
10
25
25
330
330
330
330
330.
330
330
330
330
330
330
330'
330
330
330
330
330
330
330
330
330
330
330
330
330
800
330
800
330
330
330
800
330
800
800
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
loocto
10000
10000
10000
25000
10000
25000
10000
10000
10000
25000
10000
A WWWW
25000
fc W w W
25000
Previously known by the name bis(2-Chloroisopropyl) ether
-------
Semi vol at lies
69. Dibenzofuran
70. 2,4-Dinierotoluene
71. Diethylphthalate
72. 4-Chlorophenyl-phenyl
echer
73. Fluorene
76. 4-Nitroaniline
75. 4,6-Dinitro-2-methylphenol
76. N-nitrosodiphenylamine
77. 4-Bromophenyl-phenylether
78. Hexachlorobenzene
79. Pencachlorophenol
80 . Phenanthrene
81. Anthracene
82. Carbazole
83. Di-n-butylphthalate
84 . Fluorancherie
85. Pyrene
86 . Bucylbenzylphchalace
87. 3,3'-Dichlorobenzidine
88. fienzo(a)anchracene _
89. Chrysene
90. bis(2-Echylhexyl)phchalace
91. Di-n-octylphthalate
92. Benzo(b)fluoranchene
93. Benzo(k)fluoranthene
94. Benzo(a)pyrene
95. lndeno(l,2,3-cd)pyrene
96. Dibenz(a,h)anchracene
97. Benzo(g.h.i)perylene
CAS Number
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
86-74-8
84-74-2
206-44-0
129-00-0
85-68-7
91-94-1
56-55-3
218-01-9
117-81-7
117-84-0
205-99-2
207-08-9
50-32-8
193-39-5
53-70-3
191-24-2
Quantisation Limits*
Low Hed.
Water Soil Soil
ue/L ue/Ke ue/Ke
10
10
10
10
10
25
25
10
10
10
25
10
10
10
10
10
10
10
10
10.
10
10
10
10
10
10
10
10
10
330
330
330
330
330
•
80*0.
800
330
330
330
800
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
10000
10000
10000
10000
10000
25000
25000
10000
10000
10000
25000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
* W W WW
10000
AW W WW
10000
10000
* Quanticacion limits listed for soil/sedi»ent are based on wet weight The
qu.ncic.eian limits calculated by the laboratory for soil/se£»ent
calculated on dry weight basis as required by the contract, win £e higher
-------
TARGET COMPOUND LIST (TCL) AND CONTRACT .REQUIRED QUANTITATION LIMITS (CRQL)
Otmnft Earion Limits*
Pes tie ides /Aroelors
98. alpha -BHC
99. beca-BHC
100. delta-BHC
101. gamma -BHC (Lindane)
102. Heptachlor
103. Aldrin
104. Hepeaehlor epoxide
105. Endesulfan I
106. Dieldrin
107. 4, 4 '-DDE
108. Endrin
109. Endosulfan II
110. 4. 6*. ODD
111. Endesulfan sulface
112. 4. A'- DDT
113. Methoxychlor
116. Endrin ketone
115. Endrin aldehyde
116. alpha • Chlordane
117. gamma -Chlordane
118. Toxaphene
119. Aroclor-1016
120. Aroclor-1221
121. Aroclor-1232
122. Aroclor-1242
123. Aroclor-1248
124. Aroclor-1254
125. Aroclor-1260
CAS Number
319-84-6
319-85-7
319-86-8
58-89-9
76-44-8
309-00-2
1024-57-3
959-98-8
60-57-1
72-55-9
72*20-8
33213-65-9
72-54-8
1031-07-8
50-29-3
72-43-5
53494-70-5
7421-36-3
5103-71-9
5103-74-2
8001-35-2
12674-11-2
11104.28-2
11141-16-5
53469-21-9
12672-29-6
11097-69-1
11096.82-5
Water
ue/L
0.05
0.05
0.05
0.05
0.05
0.05
0.05
0.05
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.50
0.10
0.10
0.05
0.05
5.0
1.0
2.0
•i.o
1.0
1.0
1.0
1.0
Soil
uc/Ke
1.7
1.7
1.7
1.7
1.7
• 1.7
1,7
1.7
3.3
3.3
3.3
3.3
3.3
3.3
3.3
17/0
3.3
3.3
1.7
1.7
170.0
33.0
67.0
33.0
33.0
33.0
33.0
33.0
* Quantitation limit* listed for soil/sediment are based on wet weight. The
quotation limits calculated by the laboratory for soil/sediment.
calculated on dry weight basis as required by the contract, will be higher.
There is no differentiation between the preparation of low and medium soil
samples in this method for the analysis of Pesticides/Aroclors
-------
INORGANIC TARGET ANALYTE LIST (TAL)
Contract Required
' Detection Unit
Analyte (ug/L)
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Mercury
Nickel
Potassium
Selenium
Silver
Sodium
Thallium
Vanadium
Zinc
Cyanide
200
60
10
200
5
5
5000
io
50
25
100
3
5000
15
0.2
40
5000
- 5
10
5000
10
50
20
10
(1) Subject to the restrictions specified in the first page of Part G
Section IV of Exhibit D (Alternate Methods - Catastrophic Failure) any
analytical method specified in SOW Exhibit D nay 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 linit
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) - 3
-------
(08/93)
APPENDIX D
Standard Operating Procedure for the Completion of
Special Analytical Services Client Request Forms
and
Request for Analysis Example Tables
-------
Revision
Date OB/11/93
Page _1_ of _U
STANDARD OPERATION PROCEDURE (SOP)
FOR THE COHPLETZOH OF
SPECIAL ANALYTICAL SERVICES CLIENT REQUEST FORMS (SAS CRT)
AND PREPARATION OF LABORATORY QC SUMMARY REPORT FORMS
1.0 TMTROPPCTION
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 (SOU) 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
US EPA contract for the operation of the Sample Management
Office (SMO). The SAS CRT, 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.
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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
t
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 CRT, 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 the scheduling of laboratory
space (3 weeks).
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1.4.4.2 Clients using "generic" SAS CRFs oust complete
Header sections 0, E and F and Analytical
sections 2, 3, 4 and 11. Changes to the pre-
written portions are allowed, but oust be done
in such a fashion that the changes are readily
apparent to facilitate the review process.
1.4.5 If a "generic" SAS CRT 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 oust be
approved by the Region 9 Technical Project Officer (TPO)
before the scheduling of laboratory space can begin.
Clients should allow sufficient lead tine 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 CtlERT REQUEST FORMS . CEMCTAT.
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. Vords
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 «here appropriate, the SAS should include acceptable options end
Alternative.. 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.
3.0 Ttisnmcncnui re* COMPIKTTWC THE HEADER PQRTIOW. SECTIPHS-A-^-E
3.1 SBCTIOH A - EPA Region/Client: This U always Region 9. On pre-
written "generic" SASs this section is already filled in.
3.2 SECTIOH 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 SECTIOH D - Site Name: Enter the complete Superfund site name.
3.5 SECTION E - Nearest Major City: Enter the name of the nearest
major city to the site location. This is especially helpful when
the site is located in a small town and a laboratory must be
located within a specified distance.
3.6 SECTION F - City/State: Enter the city and state where the site
is located.
3.7 SECTION G - 2 Digit Superfund Site Identifier: Enter the 2 digit
Superfund site ID code. ^ '
3.8 SECTION H - CERCLIS 0: Enter the 12 digit CERCLIS ID code.
4.0 INSTRUCTIONS FOR CQMfliETIT"? TPE 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, fjg/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
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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 veil as in the FSP.
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
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of
number of samples to bo collected and shipped on each
sampling date. .
4.4.2 The chipping 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 schedule are usually
acceptable to the receiving laboratory, however, major
changes may require a reaolicitation 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. Also include
the technical analysis 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.
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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.
4.8 SECTION 8 • Special technical instructions ... :
4.8.1 Any aodifieations 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 cheeks 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 CRT. 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). aJJ. 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
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e. telephone log*
d. a ease narrative
e. staple results
£. QA/QC summaries
g. raw sample data
h. sample preparation logs
i. example -calculations
j. calibration data
4.10 SECTXOR 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 CRT).
/
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
quantisation 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).
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4.13.3 Units should be expressed as Z recovery, relative
percent difference or concentration.
A. 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.
5.0 jrHSTRUCTIOHS FOR PREPARING THE "LABORATORY PC SUMMARY REPORT" FORM
S.I 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. 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.
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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 CRT prior to submission to the laboratory.
55 The basic questions in the QSR fora should be.phrased so the
* response is either "YES" or "HO". All "YES" answers should
indicate compliance with SAS CRF QC requirements. A "HO" is
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 so the laboratory may explain why the QC requirement
. was not met.
5.5.2 Supplementary questions should be phrased so they can be
completed with short answers.
5.6 Questions concerning the following method requirements should be
addressed in the QSR form:
5.6.1 Holding Times
5.6.1.1 Vere the contract and technical holding times
met both for extraction/preparation and
analysis?
5.6.1.2 Vas the data package sent within the specified
time period?
5.6.2 Method of Analysis and Detection Limits
5.6.2.1 Vas the appropriate analysis method used?
5.6.2.2 Vere the detection limits listed in the SAS CRF
achieved?
5.6.3 Calibrations
5.6.3.1 Vere 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 (ZR) met?
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5.6.3.2 Were calibrations performed at the frequency
specified in the method?
5.6.3.3 Blanks
5.6.3.4. Was blank contamination a problem?
5.6.3.5 Were blanks analyzed at the frequency specified
in the method?
5.6.4 Sample QC
5.6.4.1 Were the QC requirements met for percent
Recovery (ZR) 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
5.6.4.2 Vere all required sample QC analyses performed
at the frequency specified in the method?
5.6.5 Other
5.6.5.1 Questions addressing other method-specific
requirements may be necessary.
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U. S. ENVIRONMENTAL PROTECTION AGENCY
CLP Staple Management Office - SAS Number
P. 0. Box 818 - Alexandria, Virginia 22313 .
Phone: 703/557-2490; FTS/S57-2490 Modified? _ YES XT. NO
SPECIAL ANALYTICAL SERVICES
Client Request
_ Regional Transmittal ___ Telephone Request
EPA Region/Client: Region 9
Region Contact: RSCC Coordinator. ESAT. (415) 882-3069
Date of Request:
Site Name: K^U^-VO Al^TC XlT\dxxSV
Nearest Major City: fWg^TTfcp O hS, CA
City/State/ZIP Code : SV^O. I I V I I \6 , C A
2 Digit Superfund Site Identifier:
CERCLIS #:
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 samples for hexava lent chromium
(Cr* ) by EPA Method 218.4 (Atomic absorption, chelation-extraccion) .
Laboratories bidding on this analysis must be located within a 3 hour
drive from the site of sample collection.
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):
218-SAS-cw Page _L of _7_
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3 Purpose of analysis (sp-clfy Aether Superfund [enforcement or remedial
action], RCHA. HTOES. etc.):
LSI
Estimated date
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8. Special technical instructions (if outside protocol requirements,
specify compound names. CAS numbers, detection limits, etc.):
a.
1. Perform an initial calibration with a calibration blank and
at least five levels of standards. The analytical working
range must include standards at concentrations of 10 pg/L
through 250 pg/L. The correlation coefficient of the
calibration curve must be 0.995 or greater. A curve must be
prepared with each set of samples.
b Internal Quality Control Cheeks. ConcrQl_Llmits_and Corrective
Actions:
1. When calibration standard measurements exceed the quality
control (QC) requirements for the Initial Calibration, the
ICV or the CCVs, analysis must be terminated, the problem
corrected, the instrument recalibrated, and the calibration
reverified. The CCV standard reflects the conditions of ,
analysis of all associated analytical samples (that is. the
preceding analytical samples up to the previous CCV). All
samples associated with an out-of-control CCV must be
reanalyzed.
2. Analyze an Initial Calibration Verification (ICV) standard
at the mid-point concentration after the initial calibration
curve. The ICV standard must be from a different source and
of a different concentration than those used for the initial
calibration standards. Recoveries of 90-1101 of the true
value are required.
3. Analyze an Initial Calibration Blank (ICB) after the ICV
standard. Analyze a Continuing Calibration Blank (CCB)
every 10 samples, after unusually concentrated samples, and
at the end of the analyses.
A. Analyze a Continuing Calibration Verification (CCV) standard
at the mid-point concentration every 10 samples and at the
end of the analyses. The CCV standard must be from a source
different from that used for the Initial Calibration
standards. Recoveries of 90-1101 of the true value are
required.
5. Laboratory Method Blanks must be prepared and analyzed with
each group of samples prepared.
6. If the Cr*« concentration in any of the ICBs, the CCBs, or
the Laboratory Method Blanks is above the CRDL, reanalyze
the blank in question and all associated samples with
results less than 10 times the level of contamination in the
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216 SAS.Otf
associated blank. If the concentration in the blank ctill
exceeds the CRDL. terminate the analysis, correct the
problem, recalibrate the instrument, verify the calibration.
and reanalyze all associated samples with results less than
10 times the level of contamination in the associated blank.
7. Analyze a Contract Required Detection Limit (CRDL) standard
at a frequency of one per sample delivery group. The CRDL
standard must be from a source different from that used for
the Initial Calibration standards. Recoveries of 80-120X of
the true value are required.
8. Analyze Matrix Spikes (MS) at a frequency of one per SDG.
Matrix spike concentration must be equivalent to the
mid-point standard of the calibration curve. Matrix spike
recoveries must be within 75-125X. Matrix spike recoveries
that are outside of this QC criteria should be flagged by
the laboratory.
9. Analyze laboratory duplicates at a frequency of one per SDG.j.
A QC limit of 20Z for relative percent difference (RPD) is
required for original and duplicate sample values greater
than or equal to 5 times the CRDL. A QC limit of ± the CRDL
is required if either the original sample or duplicate
sample values is less than S times the CRDL. Duplicate
results that fail these QC criteria should be flagged by the
laboratory.
10. Analyze Laboratory Control Samples (LCS) at a frequency of
one per sample delivery group. LCS concentration must be
equivalent to the midpoint standard of the calibration
curve. The LCS must be from a source different from that
used for the calibration standards. Recoveries of 80-120Z
of the true value are required.
11. Samples containing Cr** at concentrations above the
calibration range are to be diluted and reanalyzed'within
the calibration range of the Initial Calibration. The
laboratory must submit documentation for the analysis of
both .the diluted and undiluted sample.
12. If the above control limits are exceeded, take appropriate
actions to correct the problem and reanalyze the affected
samples.
13. The QC requirements, listed above are the minimum required.
It is impossible to address all analytical situations that
might be experienced by a laboratory during the analysis of
environmental samples. The laboratory is expected to adhere
to good laboratory practices when analyzing samples. If the
laboratory has questions concerning the analyses of samples
Page A of 7 Bwrisian 08/23/M
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nee addressed in this document, the .Region should be
notified IMMEDIATELY (through the Sample Management Office).
9, Analytical results required (if known, specify format for data sheets.
QA/QC reports. Chain-of-Custody documentation, etc.) If nor completed.
format of results vill be left to program discretion.
_ r>»fm Calculations and Reporting Units!
A. j^^jggj^^^j^^^^^^ff^^^^f^f^i^^
Calculate the sample results according to Section 8 of EPA Method
218.4. Sample results are to be reported to 1 significant figure
for concentrations <10 itg/L and to 2 significant figures for
concentrations fclO pg/L. All records of sample analysis and the
standard curve must be legible and sufficient to recheck all
sample concentrations and QC results. Include an example of the
calculations in the data package.
b. Documentation and DeliverablesI
Deliverables (in the form of a purge file • i.e.. original
documents) for each Sample Delivery Group shall include all
deliverables required by the Information for Bid (IFB), including.
but not limited to:
1. All Sample Tracking Reports (i.e., signed SAS Packing
Lists/Chain-of-Custody forms).
2. Complete SDG File (CSF) inventory on a modified CLP Form
DC-2.
3. Sample log-in information on CLP Form DC-1.
4. 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.
5. Any telephone logs referring to the samples.
6. 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).
7. Tabulated sample results on a modified CLP Form I, with
units and sample volumes dearly specified.
8. Initial and continuing calibration verifications (ICV and
CCV) on a modified CLP Form II (Part 1), with calculated
percent recovery (XR).
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9. Contract Required Detection Limit (CRDL) standard on a
modified CLP Form II (Part 2), with calculated percent
recovery (ZR).
10. Blank data (ICB, CCB and laboratory method blanks) on a
modified CLP Form III.
11. Matrix spike result summary on a modified CLP Form IV (Part
1) with calculated percent recovery (ZR).
12. Laboratory duplicate results on a modified CLP Form VI with
calculated relative percent difference (RFD).
13. Laboratory Control Sample (LCS) results on a modified CLP
Form VII with calculated percent recovery (ZR).
14. Chelation-extraction logs on modified CLP Form VIII.
15. Analysis run logs on modified CLP Forms XIV.
16. Raw sample, standard and QC data, including:
a. instrument output
b. bench sheets and worksheets,
c. tabulated results
17. Bench sheets for sample preparation (including initial pH
information) and QC spikes.
18. Standard preparation logs, including traceable lot numbers,
for all standards used for calibration and spiking.
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: \^.V(X/\C.
Phone: ( 3iO )
2iB_SAS.cnr Page _£_ of 7 Revision os/zs/o
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12. Data Remilrenents t
Hexavalent chromium (Cr**)
Contract Required
Detection Limit fCRPL)
10 fig/L
13. PC Retroirenenca!
DC Required
Laboratory Blanks
Laboratory Duplicates
Matrix Spike
Laboratory Control Sample
Frequency of OC
with each group
of samples prepared
1 per SDG
1 per SDG
1 per SDG
Lta'its (1 or Cone .
S10 pg/L
RFD <20Z
or ±CRDL
75-125Z
80-1202
14. Action required if limits are exceeded:
If above control limits are exceeded, take appropriate actions to identify the
problem by reanalyzing the affected samples. Corrective action should be
caken before additional samples are analyzed.
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U. S. EPA RE6ZOB 9
LABORATORY QC SUMMARY REPORT
XHSTRuCTIONS
1 A separate fora is to be completed and attached to the Regional copy
(original) of each data package submitted. This fora is to be placed
directly behind the case narrative.
2. The Laboratory QC Summary Report fora is to be completed by the
Laboratory Manager, or his/her designee.
3 This farm 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 SM (Use Narrative in the
blank space and include the explanation in the ease narrative.
-------
0. S. EPA HEGXOH 9
LABORATORY QC SUMMARY REPORT
LABORATORY: .
SUBMITTED BY:
TITLE:
ANALYSIS : HHtAYAmTT CHRP**™* TO WATER
SAMPLES BY EPA METHOD 218.4
SAS f: _
t SAMPLES:
MATRIX: .
DATE:
QC SUMMARY TABLE
QC PARAMETER
Laboratory Blank
Initial Calibration
Initial Calibration
Verification (ICV)
Standard
Initial Calibration
Blank (ICB)
Continuing Calibration
Verification (CCV)
Standard
Continuing Calibration
Blank (CCB)
CRDL Standard
Matrix Spike
Laboratory Duplicate
Laboratory Control
Sample (LCS)
'
QC LIMITS
SCRDL
Cerr. Coeff. * 0.99S
ZR - 90-1101
SCRDL
XR - 90-110X
SCRDL
XR - 80-120X
XR - 75-125X
tCRDL or RPD <20X
XR - 80-120X
FREQUENCY |
with each group of I
samples prepared f
..... 1
with each group of
samples prepared
after the Initial
Calibration curve
after the ICV standard
1 per 10 samples and at
the end of the analyses
1 per 10 samples and at
1 per SDG-
' fl
1 per SDG 1
y
1 per SDC |
2ie_*sxs.p5R
Page
of
Ravi»ioi> Ot/09/91
Approved
-------
1 Ware mil sample* analyzed within the contract YES NO
required holding tine of 12 hours froa
sample receipt?
.a. If no, how many samples were analyzed outside of the holding time?
b. How many hours (or days) outside of the holding time were these
samples analyzed?
2. Were all samples analyzed within the technical YES NO
holding time of 24 hours from sample collection?
a. If no, how many samples were analyzed outside of the holding time?
b. How many hours (or days) outside of the holding time were these
samples analyzed?
3. Were all samples received intact and in good YES NO
condition?
4. Urns the data package sent within 35 days YES NO
from the receipt of the last samples in the SDC?
a. If no, how many days late was the data package sent?
5. Vas EPA Method 218.4 used to analyze YES NO
these samples?
a. If no, specify which method was used.
b. Why was this method used? Who authorized its use?
21B_«SAS.oa Page 2 of S Kwriaim e*/0«/»3
-------
6. Vas the initial pH of each sample YES NO
measured and reported?
If no. why not?
7. Was a 5-point Initial Calibration curve YES NO
prepared with each group of sanples?
If no, why not?
8. Did the Correlation Coefficient(s) of the YES NO
Initial Calibration curve(s) meet the QC
requirement of £ 0.995?
a. If no, list the value(s) that did not meet the QC requirement.
9. Were mid-point Initial Calibration Verification YES NO
(ICV) standards and Initial Calibration Blanks
(ICB) run after the Initial Calibration curve?
If no, why not?
10. Were mid-point Continuing Calibration YES NO
Verification (CCV) standards and Continuing
Calibration Blanks (CCB) run every 10 samples?
a. If no, why not?
At the end of the analyses? YES NO
a. If no, why not? .
11. Did the calibration verification (ICV and CCV) YES NO
standard recoveries meet the QC requirement of
90-110X7
a. If no, specify recovery(ies).
21I_4SAS.QSR . «
rae Revision 0«/0»/M
AppX* QVtttf
-------
12. Were laboratory blank, prepared and analyzed YES HO
with each group of samples prepared?
a. If no. at what frequency vere blank* prepared?
13. Vas blank contamination. If any. S the CRDL YES HO
for Cr4* in the laboratory method blank(s)?
In the Initial Calibration Blank(s) (ICB)? YES HO
In the Continuing Calibration Blank(s) (CCB)? YES HO
a. If no, in which blanks was contamination present and at what
levels?
14. Vere matrix spike analyses performed at a minimum YES HO
frequency of 1 per SDC?
If no, why not?
15. Did the matrix spike recovery(ies) meet the YES HO
QC requirement of 75-125X7
a. If no, specify recovery(ies).
16. Were laboratory duplicate analyses performed at a YES HO
minimum frequency of 1 per SDC?
a. If no. why not?
17. Did the laboratory duplicate results meet the YES HO
QC requirement of t the CRDL (for results <5
times the CRDL) or a RPD <20Z (for results
25 times the CRDL)?
a. If no, specify the relative percent difference.
218_4SAS.OSR Page 6 of S . K«*«ioo e*/0»/M
Approved
-------
18. Were Laboratory Control Sample (LCS) YES N0
analyses performed at a minimum frequency
of 1 per SDG?
a. If no, why not?
~19. Old the LCS recovery(ies) meet the QC requirement YES NO
of 80-1201?
a. If no, specify recovery(ies).
20. Were samples with Cr** concentrations exceeding the YES NO
calibration range diluted and reanalyzed
within the calibration range?
If no, why not?
21. Vas the Contract Required Detection Limit (CRDL) YES NO
standard analyzed at a minimum frequency
of 1 per SDC?
If no, why not?
22. Did the CRDL standard recovery (ies) YES NO
meet the QC requirement of 80-1202?
a. If no, specify recovery.
23. Was che CRDL met? YES NO
a. If no, why not? ""
216_«SAS.OSR P»*« S nf *
—2_ 01 3 Revision 0*/0«/«3
Approved
-------
D. S. ENVIRONMENTAL PROTECTION AGENCY
CLP Saaple Management Office SAS Number
p. o. Box 818 - Alexandria. Virginia 22313 *
Phone: 703/557-2490; FTS/S57-2490 Modified? __ YES V NO
SPECIAL ANALYTICAL SERVICES
Client Request
_ Regional Transmittal ' Telephone Request ,
A. EPA Region/Client: Region 9
B. Region Contact: RSCC Coordinator, ESAT. (415) 882-3069
•
C. Date of Request:
D. Site Name: S ^ \\ \\.\\ Sl^QrfajHJi
E. city/state: Co/\c€y~ Corr\Cf } CA
T. 2 Digit Superfund Site Identifier: X0
ID * :
lease provide belov 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 SV846 Method 8150A. Revision 1 (11/90).
2. Definition and number of work units Involved (specify whether whole
samples or fraction; whether organic* or inorganics; whether aqueous or
soil and sediments; and whether low, medium or high concentration):
whether super£und
B1SOASAS.CW
Revision 12/11/92
Approved
-------
^
Estimated date(s) of collection (provide a sampling schedule):
AuQusV 15 - AWC^A^* 2Oj 1^3
Estimated date(s) and method of shipment:
Federal Express • shipped same day as collection for next day delivery.
Bumber 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 JOT 20 samples.
whichever is reached first.
Analytical protocol required (attach copy if other than a protocol
currently used in this program):
Follow SV846 Method 81SOA, Revision 1 (11/90) fer extraction and
analyses. Contract required quantitation limits (CKQL) are as
per Table 1.
a. CAUTION: Diazomethane is 'a carcinogen and can EXPLODE under
certain conditions. Refer to Section 7.4.1 of SV846 Method 8150A.
Revision 1 (11/90) for precautions.
b. Capillary columns may be used for this analysis, ac long as the
laboratory demonstrates that the analysis meets all the
performance and QA/QC criteria specified in SV846 Method 81SOA,
Revision 1 (11/90) and in-this contract.
Special technical instructions (if outside protocol requirements.
' specify compound names. CAS numbers, detection limits, etc.):
a. Calibration Procedure and Criteria:
Calibrate according, to Sections. 5.12 and 7.6 of SV846 Method
8150A, Revision 1 (11/90). end Sections 7.4.2 -and 7.5 of SV846
Method 8000, with the following .specifications:
eiSOASAS.CST PAD* t ~.f
rage _z_ of
-------
1. As per Section S.12 of SV846 Method 81SOA - A minimum of
five calibration standards for each parameter of interest
should be prepared through dilution of the stock standards
with diethyl ether. One of the concentrations should be at
a concentration near, but above, the method detection limit.
The remaining concentrations should correspond to the
expected range of concentrations found in real samples or
should define the working range of the gas chromatograph
(GC). Calibration standards must be replaced after six
months, or sooner if comparison with check standards
indicates a problem.
The low concentration standard must have a slgnal-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 is defined as
the minimum concentration of a substance that can be
measured and reported with 99Z confidence that the value is
above zero.
2. A continuing calibration at the mid-point 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 20Z relative standard deviation (ZRSD) in
calibration factors (CF) for the initial calibration
standards, and less than a *15Z difference (ZD) between the
CF for the daily continuing calibrations and the average CF
from the initial calibration, are required.
b' Tnterpal Qualltr Control Cheek*. Control u*l+.t «n
-------
2. A herbicide surrogate (e.g.. an herbicide or chemically
similar compound that is not expected to be present In the
samples) must be spiked Into the standards, samples.
laboratory blanks and QC samples (see Section 5.14 and 8.3
of SV846 Method 8150A, Revision 1 (11/90)). The amount of
surrogate added must be at least 10 times the instrument
detection limit. Recoveries of 65-1251 are required, unless
documentation (such as control charts) is available to
support a different range of recoveries. The laboratory
must submit, as part of the data package, all supporting
documentation for surrogate recoveries, and historical
surrogate recovery data if necessary.
3. Second column confirmation is required.for all positive
results reported.
4. Sample extracts containing one or more analytes at
concentrations above the ini**** calibration range are to be
diluted and reanalyzed. If dilution is necessary, the
dilution must be adjusted so that the highest concentration
analyte is determined at a concentration in die upper half
of die calibration range. The laboratory must report die
results and document both analyses./
5. Analyze matrix spikes and matrix spike duplicates (MS/KSD)
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 75-1251 for waters
and 65-1351 for soils are required.
6. The QC requirements listed above are the minimum required.
It is impossible to address all analytical situations that
might be experienced by a laboratory during-the analysis of
environmental samples. The laboratory is expected to adhere
to good laboratory practices when analyzing samples. If die
laboratory has questions concerning the analyses of samples
not addressed in this document, die Region should be
notified IMMEDIATELY (through die Sample Management Office).
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 Unitsi
1. Calculate die CF and the concentration of individual
analytes using die equations in Sections 7.4.2 and 7.8.1 of
ur Page JU_ of 8 R~UI«, H/II/M
Approved ^____^
-------
SV8A6 Method 8000. The sample results are to be reported in
the concentration units of micrograms per liter (pg/L) for
water samples and micrograms per kilogram (pg/Kg) on a dry
weight basi* 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.
b. Docwtentation and Deliverablesi
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.
A. 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 I wit*
units percent solids, and sample weights or volumes clearly
specified. • J
6. Surrogate -result summaries on a modified
-------
10. Standards data, including:
a. Standards summaries on modified CLP Forms VI and VII
with calibration factors (CF) and percent relative
standard deviation (ZRSD) values or percent difference
. (ZD) values.
b. All standard data system printouts with all compounds
clearly identified.
11. Raw QC data, including:
a. Blank data, in chronological order:
1. Tabulated results
2. All blank data system printouts.
b. KS/MSD data, in chronological order:
1. Tabulated results
2. All MS/HSD 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
-------
11. Name of sampling/shipping contact: \\OXC\I
Phone: (Jl" ) |23~
dwy>A/En3y
12. . Data Requirements:
Parameter
8150A - water or soil
Contract Required
Ouantitatton Limit fCROL>
See Table 1
13. QC Requirements:
OC Required
Matrix Spike/
Matrix Spike Duplicate
Laboratory blanks
Surrogates
Initial Calibration
Continuing Calibration
Frequency of OC
1 per SDC (not more
than 20 samples per SDC)
1 per SDG
all samples, standards
as needed
Daily
Limits f Z or Cone . >
75 - 125 XR water
65 • 135 ZR soil
<±302 RFD
-------
TABLE 1
Target Compound List • EPA Method 632
Contract Required
Quantitation Units (CRQL)
Compound Water fuy/L> Soil
2.4-D
2.4-DB
2.4.5-T
2.4.5-TP (Silvex)
Dalapon
Dieamba
Diehloroprop
Dinoseb
MCPA
KCPP
12
9;l
2.0
4.7
58
2.7
6.5
0.7
2500
1900
240
180
40
34
1200
54
130
14
50.000
38.000
B1SUSAS.CRF
Page _g_ of
-------
0. S. EPA RJEGIOH 9
LABORATORY QC SUMMARY REPORT
ZRSTRUCTIOMS
1. A separate font is Co be eoopleted and attached to the Regional copy
(original) of each data package submitted. This fora is to be placed
directly behind the case narrative.
2. The Laboratory. QC Suomary Report for* 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 MO 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 ease narrative.
-------
0. S. EPA RECIOH 9
LABORATORY QC SUMMARY REPORT
LABORATORY: .
SUBMITTED BY:
TITLE:
ANALYSIS:
METHOD 81SOA
SAS f:
t SAMPLES:
MATRIX: __
DATE:
QC PARAMETER
QC StBMARY TABLE
QC LIMITS
FREQUENCY
Laboratory Blank
-------
2. Were all camples extracted within the technical
holding tines of 7 days (water) or
14 days (soil) from sample collection?
YES
NO
a. If no, list the samples that were extracted outside of the holding
b. How many days outside of the holding time were these camples
extracted? ^*
3.
Were all samples received intact and in good
condition?
YES
NO
4.
Were all samples analyzed within 40 days of receipt? YES ' H0
were analyzed outside of the holding
a. If no, list the samples that
time.
5.
Was the data package sent within 35 days
from the receipt of the last samples in the SDC?
YES
NO
a.
If no, how many days late was the data package sent*
Was EPA Method 8150A used to analyze these samples? YES
*• If no, specify which method was used.
NO
b' lf
no, why was this method used? Who
authorized its use?
81SOASAS.QSR
of
12/3/M
-------
c.
d.
Was Che approved method followed without
modifications or deviations?
YES
NO
If no, specify what the modifications or deviations were and who
approved them.
8.
7. Vas a 5• point Initial Calibration Curve run?
a. If yes, when? '
b. If no, why not? .
Did the Initial Calibration curve Beet the QC
requirement of <20Z BSD for all analytes?
a.
?f •«
limits.
**
YES
NO
. YES
NO
and RSD(«) that were outside of the
9.
10.
Was a Continuing Calibration standard run at
the beginning of each day?
After every 10 samples?
If no, why not?
YES
YES
NO
NO
a.
Did the Continuing Calibration standards meet
the QC requirement of <±15X D for all analytes?
a.
QC
*"
YES NO
«nd XD(s) that were outside of the
11.
Was the minimum response factor of 5:1 signal
to noise ratio met for «n .nalytes in the
Initial and Continuing Calibrations?
YES
NO
BiaOASAS.QSR
of
-------
12. Were laboratory blanks extracted and analyzed
at a minimus frequency of 1 per SOC?
a. If no, at what frequency were blanks performed.
YES
NO
13. Was blank contamination, if any,
-------
17. Did the MS/MSD meet the QC requirement of
7SZ • 12SZ R (water) or 65Z • 135Z R (soil)
for all spike compounds?
a. If no, specify the analyte(s) and XR(s) that were outside of the
QC limits.
18. Did the MS/MSD meet the QC requirement of
<±30X RED for all spike compounds? YES NO
a. If no, specify the analyte(s) and XRFD(s) that ware outside of the
QC limits.
19. Was the CRQL met for all analytes? YES HO
a. If no, why not? •
20. Vas It possible to analyze all analytes YES NO
within the Initial calibration range?
a. If no, were these samples diluted YES NO
according to the Instructions IB
Seccioo 8.b.4 of the SAS request?
b. List these samples and the associated analytes.
c. If no, explain why not and list those samples.
21. Vas second column confirmation performed on all
saaples with positive results? YES NO
a. If no, why not?
Page _j_ of
I€B M/a/M
-------
ANALYSES REQUESTED
OP ANALYSES REQUESTS
CHEMISTRY TYPE
ANALYSES REQUESTED
PRESERVATIVES
ANALYTICAL
HOLDING TINE (t)
CONTRACT
HOLDING TINE (•)
SAMPLE X SAMPLE
SAMPLE SAMPLING
LOCATION SCHEDULE
RAS+SAS
NO. OF
BOTTLES
PER
ANALYSIS
ROUTINE ANALYTICAL SERVICES (RAS)
ORGANICS
NO. OF
BOTTLES
PER
ANALYSIS
NO. OF
BOTTLES
PER
ANALYSIS
NO. OF
BOTTLES
PER
ANALYSIS
INORGANICS
NO. OF
BOTTLES
PER
ANALYSIS
NO. OF
BOTTLES
PER
ANALYSIS
SPECIAL ANALYTICAL
SERVICES (SAS)
NO. OF
BOTTLES
PER
ANALYSIS
NO. OF
BOTTLES
PER
ANALYSIS
»
-------
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-------
Table 5.0 • ANALYSES REQUESTED fpage 1 Of 4) MATRIX • GROUKDUATER
ENISTRYTYPE I ORSANICS INORGANICS
| RAS* SAS
ECIFIC ANALYSES REQUESTED | VOAS
(Fast TA Tie*
| SAS
Tetranyoro*
| thlophene
| RAS RAS ICI.K02/N03.I TOC
j SEMI VOAS METALS j $04, ALT *| and
1 Ctotal) j TDS j COD
(Add 2 drops (Add 2 drops (Chill to 4 C Add NNOS | Chill (H2SOI to
=SERVATIVES | 1:1 NCI | 1:1 NCI ( to pH «2 | to 4 C |pH «2 I
(Chill to 4 C (Chill to 4 C | I (Chill
(Hold -1D
j NO. OF | NO. OF | NO. OF NO. OF | NO. OF NO. OF
x SAMPLE 1 BOTTLES j BOTTLES j BOTTLES j BOTTLES j BOTTLES BOTTLES
(PER ANALYSIS (PER ANALYSIS (PER ANALYSIS (PER ANALYSIS! KR ANALY (PER ANALY
SAMPLING
SCHEDULE
1/8/90
>-2D 1/8/90
VB OC)|
:-2D
JP OF
-2D.)
>.JD
>-4D
>-5D
>UHP
XEN?)
5-60
1
1/8/90
1/8/90
1/8/90
1/9/90
1/9/90
ICOHCEN
L/M
L
L
L
L
L
1
L
(3 x 40 •! (2 x 40 ml (2x1 liter |1 x 1 liter
(glass (glsss (eater (polyethylene
(vial (vial (glass bottle (bottle
| (3)« | «>• j <1>* (1/2)*
3
6
3
3
3
3
3
2
4
2
2
2
2
2
2
4
2
. ' ..
2
2
2
2
1
2
1
1
1
1
1
1x500»l (IxSOtal
poly (poly
bottle (bottle
(1/2)* | (1/2)*
1
2
•
1
1
1
1
—
1
2
1
1
1
1
1
TOTAL
BOTTLES
10
20
10.
10
10
10
10
«nni.un volune needed when full recovery of e well purged dry exceeds 3 hours
-------
ANALYSES REQUESTED
MTtlX • LOU CONCENTRATION HATERS
OP ANALYSES REQUESTE
CHEMISTRY TYPE
ANALYSES REQUESTED
PRESERVATIVES
ANALYTICAL
HOLDING TINE (8)
CONTRACT
HOLDING TINE (a)
SAMPLE X SAMPLE
SAMPLE SAMPLING
LOCATION SCHEDULE
RAS+SAS
RAS+SAS
VOA«S
(extra QC)
Add 2 drops
1s1 RCl
Chill to 4
RoId•••»••••»»»•
Hold «7 days
prior to
extraction,
40 days after
extraction
Hold «S days
prior to
extraction,
40 days of tor
extraction
MO. OF
BOTTLES
PER
ANALYSIS
2jt 1 liter
floss bottle
RAS
PESTtPCRs
Chill to 4 C
Hold <7 days
prior to
extraction,
40 days otter
extraction
Hold «
- -
BBHUIS
MO. OF
BOTTLES
PER
ANALYSIS
1 X80Z
gloss bottle
SAS
Gross alpha*.
beta, gam
in
field
Hold to <6
— ~>- _
•onuu
Hold to <6
aanths
BO. OF
BOTTLES
PER
ANALYSIS
4 x 1 liter
poly
bottle
KW-109
MU-112
HW-U7
MU-206
LAB DC
CU-210
(blank near
(MW-206
MW-219
CU-220
dup of
(NU-219
MW-251
2/25-2/28
2/25-2/28
2/25-2/28
2/25-2/28
2/25-2/28
2/25-2/28
2/25-2/28
2/25-2/28
TOTALS
3
3
3
9
2
2
4
2
2
«
4
2
1 4
4
2
6
1
1
1
2
1
1
1
1
9
'
^ •
1
S
1
1
1
. 2
1
1
1
1
o
4
4
•
8
4
4 '
4
' -I
I 36
-------
APPENDIX E
Sample Container Requirements
for
CLP Analyses
(08/93)
-------
ORGANIC SAMPLE COLLECTION
REQUIREMENTS
WATER SAMPLES
REQUIRED
VOLUME
CONTAINER TYPE
EXTRACTABLE ANALYSIS 1 GALLON
(LOW LEVEU
EXTRACTABLE ANALYSIS 1 GALLON
(MEDIUM LEVEL*)
VOLATILE ANALYSIS 80 ML
(LOW OR MEDIUM LEVEL*)
0000-
LITER AMBER
GLASS BOTTLES
BB
4 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 O2.
, VOLATILE ANALYSIS
(LOW OR MEDIUM LEVEL*)
240 ML
0
•OD
1 x 8-OZ. WIDE-MOUTH
GLASS JAR
OR
2 x 4-OZ. WIDE-MOUTH
.GLASS JARS
2 X120-ML WIDE-MOUTH
GLASS VIALS
*ALL MEDIUM LEVEL SAMPLES TO BE SEALED IN METAL PAINT CAN FOR SHIPMENT
-------
INORGANIC SAMPLE COLLECTION
REQUIREMENTS
WATER SAMPLES
VOLUME
CONTAINER TYPE
METALS ANALYSIS 1 LITER
(LOW LEVEL!
METALS ANALYSIS 16 OZ. •
(MEDIUM LEVEL-)
CYANIDE (CN'I ANALYSIS 1 LITER
(LOW LEVEL!
CYANIDE (CN~) ANALYSIS 16 OZ.
(MEDIUM LEVEL*!
1 x 1-LITER
POLYETHYLENE BOTTLE
1 x 16-OZ, WIDE-MOUTH
GLASS JAR
D
1 x 1-UTER
POLYETHYLENE BOTTLE
1 x 16-OZ. WIDE-MOUTH
GLASS JAR
SOIL/SEDIMENT SAMPLES
REQUIRED
VOLUME
CONTAINER TYPE
METALS'AND CYANIDE (CN~|
ANALYSIS
(LOW OR MEDIUM LEVEL*)
6OZ.
0
3D
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
2J.7.8-TCOD
ANALYSIS
JMULTI-CONCENTRATIONI
2.3.7.8-TCOD
ANALYSIS
(MULTI-CONCENTRATION)
REQUIRED
VOLUME
2 LITERS
REQUIRED
VOLUME
402.
00
o
D
CONTAINER TYPE
2 x 1-UTER AMBER
GLASS BOTTLES
CONTAINER TYPE
___I————
1 x 4-O2. WIDE-MOUTH
GLASS JAR
OR
1 x 8-O2. WIDE-MOUTH
GLASS JAR
HIGH HAZARD SAMPLE COLLECTION
REQUIREMENTS
LIQUID OR SOLID SAMPLES
REQUIRED
VOLUME
CONTAINER TYPE
ORGANIC AND INORGANIC
ANALYSIS
602.
D
1 x 8-OZ. WIDE-MOUTH
GLASS JAR
•ALL MEDIUM LEVEL SAMPLES TO BE SEALED IN METAL PAINT CAN FOR SHIPMENT
-------
(08/93)
APPENDIX F
Sample Holding Times, Treatment and Preservation
for
RAS and Common SAS Analyses
-------
(08/93)
farameter
Volatiles
concentratIon
Low/Medium
Semivolatilee
Pesticides/PCBs
Dissolved Metals
Low/Medium
Low/Medium
Low/Medium
Requirements for HAS Analyses
WATER SAMPLES
preservation
Acidify to pB < 2 with BCl.
Add 2 drops Isl BCl 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 pB test on at least one vial
at each site for each aquifer. The tested
vial must be discarded. If the pR is > 2,
additional BCl 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 trihalo-
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.
Chill to 4° C
Chill to 4° C
Filter Sample through 0.45 micron filter
immediately after sample collection or with
in-line filtration when possible. Acidify to
pH < 2 with BN03 after filtration.
Total Metals
Low/Medium Includes suspended sediments and
particulates. Acidify to pH < 2 with HNO
'3-
-------
(08/93)
Parameter
Preservation Requirements for BAfi Analyses
RATER SAMPLES
Concentration Praaervatien
Cyanide* Lew/Medium Preserve all sample* with 2 ml of 10 N NaOB
per liter of sample to pH > 12. Chill to 4°
C.
Treatment for chlorine or other known oxidis-
ing agents may be necessary. Test a drop of
the sample with potassium iodide-starch test
paper (K-X 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
volt
Preservation Requirementa for HAS Analyses
SOIL SAMPLES
Parameter Concentration Preservation
Organics Low/Medium Chill to 4° C
Metals Low/Medium None
Cyanide Low/Medium Chill to 4° C
-------
(08/93)
Analytical and Contractual Holding Tinea for HAS Analyses
Matrixi
Analysis
VOA
B/N/A
Pest./PCB
Mercury
Cyanide
Metals
Water
Analytical * Contractual**
Holding Times Holding Times
14 days
7 days
7 days
28 days
14 days
6 months
10 days
5 days
5 days
26 days
12 days
35 days
Soil
Analytical*
Holding Times
14 days
14 days
14 days
28 days
14 days
6 months
Contractual**
Holding Times
10 days
10 days
10 days
26 days
12 days
35 days
* The Analytical Holding Tine is the amount of tine 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, cither domestic sewage, industrial wastes, or
natural waters, is a practical impossibility. Regardless of the nature of the sample, complete stability
for every 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 parr*-:
source. The changes that lake place in a sample are either chemical or biological In the former case.
cenain 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 constituents.
cations or anions may change valence states under certain reducing or oxidizing conditions; other
constituents may dissolve or volatilize with' the passage of time. Metal cations may also adsorb onh-
surfaces (glass, plastic, quartz, etc.), such as. iron and lead. Biological changes taking place in «
sample may change the valence of an element or a radical to a different valence. Soluble constituents
may be convened 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 examples ni
biological influence on sample composition. Therefore, as a general rule, it is best to analyze the
samples as soon as possible after collection. This is especially true when the anaiyte concentration •>
expected to be in the low i/g/1 range.
Methods of preservation are relatively limited and are intended generally to (1) retard
action. (2) retard hydrolysis of chemical compounds and complexes, (3) reduce volatility
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' Quality Assurance
Coordinators As more data become available, these recommended holding times will be adjustta '••
reflect neu information. Other information provided in the table is an estimation of the volume of
sample required for the analysis, the suggested type of container, and the maximum recommended
holding times for samples properly preserved.
-------
TABLE 1
RECOMMEN
OFSAJ
Measurement
100 Physical Properties
Odor
Conductance
Hardness
Odor
PH
Residue
Filterable
Non-
Filterable
Total
Volatile
Settleable Matter
Temperature
Turbidity
DATION
fflPLES A
VoL
Req.
(ml)
SO
too
, too
200
25
100
100
100
100
1000
1000
100
FOR SAMPLING AND PRESERVATION
OCORDING TO MEASUREMENT"
Holding
Container* Preservative*4 Tune8
P.6
TJB
P.O
G only
PXJ
P,0
P.G
P.G
P.O
P.O
P.O
P.G
cod. re
CoolfC
UNO, topH<2
Cool.4lC
None Rrq.
C001.4-C
Cooirc
cooirc
Cool 4^
Cool.4°C
NooeReq.
cooirc
46 Hn.
28 Day,
6Mos.
24 Mrs.
Atulv/r
Immttluiit h
7 Days
7 Days
7 Days
7 Days
48 HIV
Analwr
ImrmtiiairlY
48Hrv
200 Metals
Dissolved
Suspended
Total
200 P.G
200
100
P.G
Filter OB rite
HNO, to pH<2
Fther on rite
HNOJlopH<2
6 Mas.
6 Mov"
6 Mas.
-------
TABLE 1 (COND
Vol.
Req.
Measurement (ml)
Chromium"*
Mercury
Dissolved
Total
300 Inorganics. Non-Metallies
Acidity
Alkalinity
Bromide
Chloride
Chlorine
Cyanides
Fluoride
Iodide
Nitrogen
Ammonia
Kjeidahl. Total
Nitrate plus Nitrite
Nitrate*
Nitrite
••^•iM
200
100
100
100
100
100
SO
200
500
300
100
400
500
100
100
so
Container* Preservative*4
fJD
P.G
P.G
P.G
P.G
P.G
P.G
P.G
P.G
P.G
P.G
P.G
P,G
P.G
P.G
P.G
Cool.4T.
Filler
HNOj to pH<2
HNOj topH<2
Cool.4°C:
Cool. 4X
NonrRrq.
Nose Req.
Nonr Rrq.
cooirc
NaOHtopH>12
O.fij; asrnrbir arid*
None Req.
Cool 4*C
CooWC
H,SO4 topH<2
Cool. 4*C
Cool. 4*C
H,SO4 topH<2
Coolie
Cool^
Holding
Timr8
24 Hn.
«»,„
28 Days
NDa\k
14 Da\k
28Dii\K
28 Day*
Anal\«r
lmmrdi:iifh
H DaysT
28Da>i
24 Hn
28 D.iyi
HD.>,
28 D.ivs
48 Hn.
48 Hn.
-------
TABLE 1 (COND
Measurement
Dissolved Oxygen
Probe
WinLler
Phosphorus
Ortho-
phosphate,
Dissolved
Hydrolyuble
Total
Total.
Dissolved
Silica
Sulfate
Sulfide
Sulfite
40U Organics
BOD
COD
Oil & Crease
Organic carbon
Phenolics
Vol.
Req.
(ml)
•MM^^M
300
300
50
SO
so
so
so
so
500
50
1000
50
1000
25
500
Container8 Preservative*4
C! Untie* ami ui|>
G bottle and top
P.G
P.G
P.G
P,G
Ponry
P,G
P.G
P.G
P,G
P,G
G only
P.G
G only
NimrRvq.
UK on siir
andctnrr
in dark
Filter on site
CooL4!C
C0014-C
H]SO«topH<2
cooirc
H,SO, topH<2
Fthef • on site '
Coolt 4*C
H,SO. to pH<2
Cool, 4*C
Cool4X:
Cool.4*C
add 2 ml urn
arrtutr plu* XaOH
topH>9
Konc R«J.
Cooirc
C^xiI.4°C
HjSO4 to pH<2
cootrc
HjSO« to pH<2
Cool 4*C
H^O« or HO to pH<2
Cool,4°C
Holding
Time5
Analyzr
Immrdiatrly
8 Hours
48 HIV
2»Dnvs
28 Day*
24Hrs.
2* Day*
28 Days
7 Day*
Analyze
Immediately
4ft Hrv
28 Day*
2K Days
28Davt
28 Days
-------
TABLE 1 (CONT)
Vol.
Req. Holding
Measurement (ml) Container* Preservative** Time*
MBAS .250 P.G Cool, 4"C «Hr».
NTA SO P.G 0001410 24 Hrs
1. More specific instructions for preservation and sampling are found with each 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 0-3370.
2. Plastic (?) or Class (G). For metals, polyethylene with a polypropylene cap (no liner) is
preferred.
• pi estivation tlmiilcl be performed immediately upon sample collection. Foi
site sample's each aliquot should be preserved at ihetimeof collection. When uftcitl
>matedsami>lci makes iiimiMts&ihle in nrrMtvfMirhalinttm i Kr*n •.nmnl*.. m-n i>..
3. Sample
composite
an automated sample-intakes it impossible to preserve each aliquot, then samples max !*•
pit-served by maintaining at JeC: until compositing and sample splitting is completed
1. When am sample is 10 be ship|»ecl by common carrier or sen I through the I'niied Sun »
Mails, it mtisi comply with the Department of Transportation Hazardous Materials
Regulations H9 CIFR Pan 172). The person offering such material for transportation is
it-sponsible for ensuring such compliance. For the preservation requirements of Table 1.
the Office of Hazardous Materials. Materials Transportation Bureau. Department of
I lansporiation has detei mined that the Hazardous Materials Regulations do not apply m
the following materials: Hydrochloric acid (HCI) in water solutions at concentrations of
0.0-T. b> weight or less(pH about 1.96 01 greater): Xitricacid(HNOaiin water solutions at
< onrentiatiom of 0.15% by weight or less (pH about 1.62 or greater); Sulf uric acid (HjSO4.
in wain solutions at concentrations of OJ5* by weight or less (pH about 1715 or greatei r
Sodium hydroxide (NaOH) in water solutions at concentrations of 0.080% bv weight 01
!<•>•. (pH abom 12.30 or less). • '•
:>. Sample* should be analy/ed as soon as possible after collection. The times listed are the
maximum limes that samples may be held before analysis and still considered t~.,lid
Samples may be held for longer periods only if the peimiiiee. or monitoring blmraiiirv.
has data on file io show that the specific types of sample under »tudv are stable for the
l'»nKrr time, and has received a variance from the Regional Adminisira.o,. Some sampl.-s
may not !«• stable foi the maximum time |Miiod given in the table A peritiitiee 01
mimiioriiig laboratory, is obligated to hold the sample for a shorter time if
exists to khow this is necessary to maintain sample stability.
6. Should only be used in the presence of residual chlorine.
-------
i M minimi holiliiiu limr •% 21 Hmm wlirn .ulfidr i» |»«mi. Opiiemally. all umpK m;.x
MT MdR- the i I adusimmi in .mlrr 10 ilrterminr if ,ul(,(h-
i- i, «« hr o^i * ** ^
Jxnvilrr until a m-ffiiivr M»«»« ««' » •*««"««• The «amplc u fil
pH 12.
rfmuW IK- filirml imimtliaicly on-riic b^f.iir adding pmeromr for diisc,lv,xl
H.
tiiriaU.
.»M»rtmr*Wh
-------
Superseded By
INSTRUCTIONS FOR SAMPLE
SHIPPING AND DOCUMENTATION
(October, 1994)
-------
MZD DOOTMEOTJkTIOH
October 1994
Quality Assurance Management Section
U. S. EPA Region 9
San Francisco, CA
-------
TABLE OF CONTENTS
1.0 GENERAL ..............................
1.3 DISTRIBUTION OF COPIES ................... 1
1.3.1 CLP SERVICES ..... ................ 1
1.3.2 ESB Regional Analytical Program (RAP) ......... 2
1.3.3 FIELD QA/QC SUMMARY FORM ......... ...... 2
2.0 CALLING IB SHIPPING INFORMATION TO THE ESAT RSCC COORDINATOR ... 2
3.0 CLP ANALYTICAL SERVICES (CLPAS1 TRAFFIC REPORT/CHAIK-OP-CUSTODY
FORMS FOR ORGANIC AND INORGANIC ANALYSES ............. 3
3.1 CASE DOCUMENTATION ..................... 3
3.2 HEADER INFORMATION ..................... 3
3.2.1 Box 1 - PROJECT CODE/SITE INFORMATION ......... 3
3.2.2 Box 2 - REGIONAL INFORMATION ............. 4
3.2.3 Box 3 - TYPE OF ACTIVITY ... ............ 4
3.2.4 Box 4 - SHIPPING INFORMATION ............. 4
3.2.5 Box 5 - SHIP TO .................... 4
3.2.6 Box 6 , PRESERVATIVE .................. 4
3.2.7 Box 7 - SAMPLE DESCRIPTION .............. 4
3.3 SAMPLE DOCUMENTATION ..................... .4
3.3.1 SAMPLE NUMBERS .......... .......... 4
3.3.2 Column A - SAMPLE DESCRIPTION ............. 5
3.3.3 Column B - CONCENTRATION . .............. 5
3.3.4 Column C - SAMPLE TYPE COMPOSITE/GRAB ......... 5
3.3.5 Column D - PRESERVATIVE USED ............. 5
3.3.6 Column E - CLPAS ANALYSIS ............... 5
3.3.7 Column F - REGIONAL SPECIFIC TRACKING NUMBERS OR TAG
NUMBERS ....... ................. 5
3.3.8 Column G - STATION LOCATION NUMBER .......... 6
3.3.9 Column H - MO/DAY/YEAR/TIME OF SAMPLE COLLECTION ... 6
3.3.10 Column I - SAMPLER INITIALS .......... ... 6
3.3.11 Column J - CORRESPONDING CLP ORGANIC/INORGANIC SAMPLE
NUMBER ........................ 6
3.3.12 Column K - DESIGNATED FIELD QC ............ 6
3.4 "SHIPMENT FOR CASE COMPLETE (Y/N)" ............. 7
3.5 "PAGE 1 OF _ " ................. '.'.'.'.'. 7
3.6 "SAMPLE USED FOR SPIKE AND/OR DUPLICATE" ......... . 7
3.7 "ADDITIONAL SAMPLER SIGNATURES" ............... 7
3.8 "CHAIN OF CUSTODY SEAL NUMBER" ....... ....... '. 7
3.9 "SPLIT SAMPLES ACCEPTED/DECLINED" ..... ..... '.'.'.'. 8
4.0 ESB REGIONAL ANALYTICAL PROGRAM (RAP> CHAIN- OF -CUSTODY FORMS . . 8
4.1 CASE DOCUMENTATION ................. 8
4.1.1 PROJECT NUMBER ............ '.'.'.'.'.'.'' 8
4.1.2 PROJECT NAME .............. \ ] ..... g
4.1.3 SAMPLERS (Signature) ..... '.'.'.'.'. ....... 8
4.2 SAMPLE DOCUMENTATION ............ . . ' 8
4.2.1 SAMPLE NUMBERS ......... [ ......... 8
4.2.2 DATE ........... '.'.'.'.'.'. ........ 8
-------
4.2.3 TIME 8
4.2.4 COMP./GRAB 8
4.2.5 STATION LOCATION 9
4.2.6 SAMPLE 9
4.2.7 NO. OF CONTAINERS 9
4.2.8 SAMPLE ANALYSES 9
4.2.9 REMARKS 9
4.3 AIRBILL NUMBER 10
4.4 "REMARKS0 BOX 10
4.4.1 CHAIN OF CUSTODY SEAL NUMBER 10
4.4.2 LABORATORY NAME 10
4.4.3 SHIPPING COMPLETE? 10
4.4.4 CARRIER 11
5.0 SAMPLE BOmJES 11
6.0 FIELD OA/OC SUMMARY FORM 11
-------
1.0 GENERAL
1.1 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).
For CLP Analytical Services, Contract Laboratory Analytical
Services Support's (CLASS) 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
weekly. (Note: The ESAT RSCC coordinator will not forward
CLASS'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
CLASS address:
Contract Laboratory Analytical Services Support
P. 0. Box 818
Alexandria, VA 22313
Attn: Region 9 Coordinator
1.2 For analyses performed by the Regional Laboratory, DO NOT send any
copies of the paperwork to the Contract Laboratory Analytical
Services Support (CLASS). Send both the Regional and CLASS copies
to the USEPA Region 9 Quality Assurance Management Section.
1.3 DISTRIBUTION OF COPIES
1.3.1 CLP ANALYTICAL SERVICES
1.3.1.1 ORGANIC TRAFFIC REPORT/CHAIN-OF-CUSTODY FORM
a. Blue (original) copy to QAMS, Region 9
b. Pink (second) copy to CLASS
c. White (third) and Yellow (fourth) copies
accompany samples to laboratory
d. Photocopy for sampler's files
1.3.1.2 INORGANIC TRAFFIC REPORT/CHAIN-OF-CUSTODY FORM
a. Green (original) copy to QAMS, Region 9
b. Pink (second) copy to CLASS
CLPPAPER.SOP 1 10/94
-------
c. Uhitc (third) and Yellow (fourth) copies
accompany samples to laboratory
d. Photocopy for sampler's files
1.3.2 ESB REGIONAL ANALYTICAL PROGRAM (RAP): Analytical
services arranged by the Environmental Services Branch (ESfi)
of the EPA and performed by the Region 9 Laboratory or a
commercial laboratory.
1.3.2.1 RAP CHAIN-OF-CUSTODY FORM
a. White (original) copy to laboratory with samples
b. Pink copy to QAMS, Region 9
c. Photocopy for sampler's file
1.3.3 FIELD QA/QC SUMMARY FORM
a. Original to QAMS, Region 9
b. Photocopy for sampler's files
2.0 CALLING IN SHIPPIHG INFORMATION TO THE BSAT RSCC COORDIHATOR
2.1 Call the Environmental Services Assistance Team Regional Sample
Control Center (ESAT RSCC) coordinator on a daily basis, even if
no shipments were made. The ESAT RSCC coordinator may be reached
at (415) 882-3069.
2.2 Try to stick to the sampling schedule. If this is not possible,
let the. ESAT RSCC coordinator know immediately so other
arrangements can be made.
2.3 Notify the ESAT RSCC coordinator within 12 hours of sample
shipments. Calling in sample shipments to the ESAT RSCC
coordinator is MANDATORY. Notification of special shipments, such
as Saturday deliveries, are detailed below.
2.3.1 Friday shipments for Saturday delivery must be called in by
noon (12:00 pm) Friday. This is to enable the ESAT RSCC
coordinator to pass the information on to CLASS or to the
laboratories. Saturday pickup cannot be guaranteed if
shipping information is received late. Samplers may not
contact the laboratories directly. (Laboratories do not
have to accept notification of delivery of samples from
sources other than CLASS or RSCC.)
2.3.2 Laboratories may request advance notification of the arrival
of certain types of samples, such as samples with very short
holding times (e.g., Cr +6) that will be hand delivered to
the laboratory. Required deadlines for notification of
sample shipments in these special cases will be determined
CLPPAPKR.SOP 2 10/94
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on a case by case basis. The ESAT RSCC coordinator will
inform the samplers as to when notification of sample
delivery is required (e.g., by noon on the day samples will
be delivered). This is to facilitate the laboratory(ies)
having personnel available to analyze the samples as soon as
they arrive.
2.4 Provide the following information to the ESAT RSCC coordinator:
1. Case number
2. Name of Laboratory
3. Date of shipment
4. Carrier and airbill number
5. Number of samples shipped by matrix and analysis type
6. Number of coolers shipped
7. Information on completions, changes, delays, etc.
2.5 If you have an emergency and need to get information to a
laboratory, your calls should be directed, in order of succession,
to:
ESAT RSCC Coordinator - (415) 882-3069
EPA RSCC Task Monitor - (415) 744-1499
CLASS Region 9 Coordinator (CLPAS) - (703) 519-1471
DO NOT call the laboratory(ies) directly under any circumstances.
3 .0 CLP ANALYTICAL SERVICES (CLPAS) TRAFFIC REPORT/CHAIN-OF-CUSTODY FORMS
FOR ORGANIC AND INORGANIC ANALYSES
3.1 CASE DOCUMENTATION
Complete this form when collecting CLPAS samples. See Attachments
1 through 3 for examples.
Enter the CLPAS case number in the box(es) located in the upper
right corner of the form. CLPAS case numbers have the format
"xxxxx" (e.g., 18123).
3.2 HEADER INFORMATION
3.2.1 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 (e.g., RCRA) in the
box titled "Non-Superfund program."
CLPPAPER.SOP
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3.2.2 Box 2 - REGIONAL INFORMATION
Enter the Region number, the nasae of your sampling company,
and your name and signature in the designated spaces.
3.2.3 Box 3 - TYPE OF ACTIVITY
Check the appropriate box(es) for the type of activity for
this sampling event. See Appendix A for acronym
definitions.
3.2.4 Box 4 - SHIPPING INFORMATION
Enter the date shipped, the carrier (e.g., Federal Express,
Airboume, etc.) and the air bill number in the appropriate
spaces.
3.2.5 Box 5 - SHIP TO
Enter the laboratory name, full address and laboratory
contact (e.g., Sample Custodian).
3.2.6 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 (e.g., in the Cyanide box enter "2")
or list them, separated by commas, in the same order as the
checked sample analyses. (Alternatively, the analyses may
be listed on separate lines.)
3.2.7 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.
3.3 SAMPLE DOCUMENTATION
3.3.1 SAMPLE NUMBERS
Carefully transcribe the CLPAS sample numbers from the
printed labels onto the Organic or Inorganic Traffic
Report/Chain-of-Custody forms in the column labeled "CLP
Sample Numbers".
CLPPAPER.SOP 4 10/94
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CLPAS sample numbers have the following formats: YX123 for
organic and MYX123 for inorganic samples. See Appendix B
for examples.
3.3.2 Column A - SAMPLE DESCRIPTION
Enter the appropriate sample description code from Box 7.
Note: Item #6 "Oil" and Item #7 "Waste" are for RAP
projects only. Do not ship oily samples or waste samples
without making prior arrangements with the EPA.
3.3.3 r.nlumn B - CONCENTRATION
Enter "L" for low and "M* for medium concentration samples.
(Prior arrangements must have been made with the ESAT RSCC
coordinator, CLASS and the laboratories accepting the
samples before shipping medium concentration samples. At
this time, high concentration samples must be scheduled
through the RAP system.)
NOTE: Medium concentration samples must be shipped in metal
cans.
3.3.4 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.
3.3.5 Column D - PRESERVATIVE USED
Enter the preservative used from Box 6.
3.3.6 Column E - CLPAS 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: If dissolved metals are requested, a note must be
added indicating that the samples have been field filtered
and that digestion is required. See Attachment 2 for an
example.
3.3.7 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
CLPPAPER.SOP 5 10/94
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this as "Special Instructions0, be sure to note, at the
bottom of the "Sample Documentation0 area, what the special
handling is. The number and type of containers could be
entered here, (e.g., 3-40 raL, 6-1L)
3.3.8 Column G - STATION LOCATION NUMBER
Enter the station location in the space provided.
3.3.9 Column H - MO/DAY/YEAR/TIME OF SAMPLE COLLECTION
Record the month, day, year and time (use military time,
e.g., 1600 ° 4:00 pm) of sample collection.
3.3.10 Column I - SAMPLER INITIALS
Enter your initials.
3.3.11 Column J - CORRESPONDING CLP ORGANIC/INORGANIC SAMPLE
NUMBER
Enter the corresponding CLP sample number for organic or
inorganic CLPAS analysis.
3.3.12 Column K - DESIGNATED FIELD QC
NOTE: This column is NOT to be used for the designated
laboratory QC samples. Information entered here is
not reproduced onto the laboratories" copies.
Enter the appropriate qualifier as listed below for "Blind"
Field QC samples in this column. (NOTE: All samples must
have a qualifier.)
Blind Field PC Qualifier
Blind Blanks (field, etc.) B
Blind Field Duplicates D
Blind Field Spikes S
Blind PE Samples PE
All other field samples
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.
These are field duplicates. Do not include samples
designated as laboratory duplicates. The primary
sample is identified with B--° and the duplicate is
CLPPAPER.SOP 6 10/94
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given °Dn in column K. In addition, the station
locations should also identify the primary and
duplicate samples. For example, MH-1 is the primary
sample and MW-1B is the duplicate sample.
"SH =• 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 blind field QC
samples are given this qualifier.
3.4 "SHIPMENT FOR CASE COMPLETE (Y/N)H
This should reflect the status of the samples scheduled to be
shipped to a laboratory for a specific case. Only when ALL
samples scheduled for shipment to a laboratory for a specific case
have been shipped is the case complete.
3.5 "PAGE 1 OF "
Enter the number of Traffic Report/Chain-of-Custody Record form(s)
enclosed in each cooler. The form(s) accompanying each cooler
must list only those samples contained in that cooler.
3.6 "SAMPLE USED FOR SPIKE AND/OR DUPLICATE"
Enter the sample number of the sample designated for laboratory
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).
DO WOT enter samples designated as blind field duplicates in this
block.
3.7 "ADDITIONAL SAMPLER SIGNATURES"
Record additional sampler signatures that are different from that
in Box 2.
3.8 "CHAIN OF CUSTODY SEAL NUMBER"
Enter the Chain of Custody Seal Number used to seal the cooler, if
applicable.
CLPPAPER.SOP
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3.9 Instructions summarizing CLP sample, volusaes, packaging and
shipiaent reporting requirements are printed on the back of the
Traffic Reports.
4.0 P.SB BECIOMAL AMLYTZCAX. PROGRAM (BAP) CMSH-OF-C?SyOpy gORjfS
4.1 CASE DOCUMENTATION
Complete this form when collecting RAP samples. See Attachment 4
for an example.
4.1.1 PROJECT NUMBER
Enter the RAP case number in this box.
4.1.2 PROJECT NAME
Leave this space blank.
4.1.3 SAMPLERS (Signature)
Record all sampler signatures in this box.
4.2 SAMPLE DOCUMENTATION
4.2.1 SAMPLE NUMBERS
Carefully transcribe the RAP saaple numbers from the printed
sample labels onto the R9/COC form in the space labelled
STA.NO.
RAP sample numbers have the format SYxxxx (e.g., SYD234).
See Appendix B for examples.
4.2.2 DATE
Enter the month, day and year the sample was collected in
the "DATE" column.
4.2.3 TIME
Enter the time (using military time) in the "TIME" column.
4.2.4 COMP./GRAB
Check the kind of sample collected in the composite or grab
column.
4.2.5 STATION LOCATION
Enter the sample site location in the space provided.
CLPPAPER.SOP 8 10/9<1
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4.2.6 SAMPLE MATRIX
For each sample, enter the appropriate sample matrix
description in the right third portion of the "STATION
LOCATION" column.
4.2.7 NO. OF CONTAINERS
Enter the total number of sample containers collected for
each matrix at each station location.
4.2.8 SAMPLE ANALYSES
There are six slanted columns to be used to specify the kind
of analysis to be performed by the laboratory. Enter the
appropriate analysis in each column. Mark the box of the
appropriate analysis for each sample collected.
4.2.9 REMARKS
The items listed below are to be included in this area on
the appropriate sample line.
4.2.9.1 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.
4.2.9.2 PRESERVATIVE USED
Enter the preservative used.
If more than one type of preservative is used for a
sample, separate the preservative references with
commas. The sequence of the reference numbers must
follow the sequence of the requested "RAP Analysis"
parameters that are recorded in the analysis columns.
4.2.9.3 SAMPLE USED FOR SPIKE AND/OR DUPLICATE
Enter the sample number 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).
CLPPAPER.SOP
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4.3 AIRBILL NUMBER
The airbill number should be entered on the first signature line,
in the box marked "Received by: (Signature)0.
4.4 "REMARKS" BOX
Located in the lower right hand corner of the Chain of Custody is
a box labelled "Remarks". The following items should be entered
there.
4.4.1 CHAIN OF CUSTODY SEAL NUMBER
Enter the Chain of Custody Seal Number used to seal the
coolers, if applicable, in the box labelled "Remarks", in
the lower right-hand corner.
4.4.2 LABORATORY NAME
Enter the Laboratory name in the box labelled "Remarks", in
the lower right-hand corner.
4.4.3 SHIPPING COMPLETE?
Enter °yes, shipping is complete" or "No, shipping is not
complete" in the box labelled "Remarks", in the lower right-
hand corner.
4.4.4 CARRIER
Enter the carrier (e.g., "Fed Ex") in the box labelled
"Remarks", in the lower right-hand corner.
5.0 SAMPLE BOTTLES
5.1 Sample bottles be labeled with the following information:
a. Case number
b. Date/Time of collection
c. Matrix/Concentration
d. Station Location
e. Sample number (from the pre-printed labels)
£. Analysis
g. Preservative
5.2 Pre-printed, self-adhesive labels are provided for CLPAS Organic,
CLPAS Inorganic and RAP samples.
5.2.1 Transcribe the appropriate sample number onto the
corresponding bottle label and/or affix the sample number
label onto the bottle.
CLPPAPER.SOP 10 10/94
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5.2.2 Destroy all unused labels or return them to the ESAT RSCC
coordinator. DO NOT use them for future samplings. New
cample numbers will be assigned.
6.0 FIEUQ OA/OC SUMMARY FORM
6.1 Complete one form per laboratory per matrix for each sampling
event. For long term projects, complete a form(s) after each week
of sampling. Complete the header portion even if no QA/QC samples
were provided.
6.2 Complete all applicable entries. Please use the appropriate
sample numbers for each laboratory, (e.g., for the laboratory
performing CLPAS organics, use the CLP organic sample numbers,
YX123, etc. For the laboratory performing RAP analyses, use the
RAP sample numbers, SY0123, etc.) Please do not use station
locations. If a laboratory is performing more than one type of
analysis, list all applicable sample numbers.
6.3 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. Failure
to provide this information will delay the completion of
validation.
CLPPAPER. SOP 1 1
Li 10/94
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TYPE OF ACTIVITY
Check the box which describes the funding lead for this sampling event:
Funding Lead
SF = Superfund
PRP = Potentially Responsible Party
ST ~ State
FED = Federal
Check one or more boxes, as appropriate, which describe the task of this
sampling event:
Pre-Remedlal
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
REHA = Removal Assessment
REH = Removal
OIL = Oil Response
UST = Underground Storage Tank Response
CLPPAPER.SOP I? ,
•" 10/94
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lise B
a o
CLP SAMPLE NUMBERS
Each sample is assigned a unique sample number. A "sample" is defined as
follows:
o one matrix, e.g., water, soil/sediment, fish, etc.
o one station location
o one analytical program, e.g., CLPAS organics, CLPAS inorganics or
a RAP analysis
o one laboratory
Sample numbers for CLPAS and RAP analyses:
° CLPAS Organic sample numbers consist of five alpha-numerics,
always beginning with "Y"
Example - YJ386
° CLPAS Inorganic sample numbers consist of six alpha-numerics,
always beginning with "MY"
Example - MYG528
o RAP sample numbers consist of six alpha-numerics, always beginning
with "SY"
Example - SYD905
Examples for assigning sample numbers:
CLPAS Volatiles & CLPAS Pesticides/PCBs receive the SAME SAMPLE
NUMBER, if the samples are:
the same matrix
part of the same analytical program, e.g., CLPAS
organics
from the same station location
going to the same laboratory
CLPPAPER.SOP 1o
1J 10/94
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CLPAS Volatiles & CLPAS Pesticides/PCBs receive DlggfeKENT SAMPLE
HUMBERS. if the samples are:
the same matrix
part of the same analytical program, e.g., CLPAS
organics
from the same station location
going to different laboratories
CLPAS Volatiles & CLPAS Hetals receive PJLygaREHT SAMPLE HPMBERS.
if the samples are:
the same matrix
part of different analytical programs, e.g., CLPAS
organics & CLPAS inorganics
from the same station location
going to the same laboratory
CLPAS Volatiles 6 RAP Herbicides receive DlgygREHT SAMPLE HUMBERS.
if the samples are:
the same matrix
part of different analytical programs, e.g., CLPAS
organics & RAP organics
from the same station location
going to the same laboratory
RAP TDS & RAP Nitrate/Nitrite receive the SAME SAMPLE HUMBER. if
the samples are:
the same matrix
part of the same analytical program, e.g., RAP
inorganics
from the same station location
going to the same laboratory
CLPPAPER. SOP 14.
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United Staleo Envtmranontd Protection Agency
Conuoa laboratory P
-------
LWlod Sloloo Efwironmoniol Pioiocton Agoncy
Cont«Qct Loboictory P^Qfom Sanipfo Management Oflice
POBoiSlfl Alo«»nd'ia. VA
Account Code
Regional Information
Won Supcrtund Program
CLP
Sample
Numbers
(from
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Enter
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9
Sampling Co.
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-------
Organle Traffic Report
& Chain of Custody Record
(Hoi Ogantc CIP Ane
4 Dale Shipped Carrier
SAS No.
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United Sloloo Environmental Protection Agency
Contort Lohaianry ftoffam Sonplo Management Ofl.co
PO BOD 818 fllonrxjria VA 7731)
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2 Hegion No f Sampling Co
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Regional Information
Sampler (Nomo)
J Suilaos Water
Ground Wfflof
3.
. Rlnsaio
S. Soil/SeriJmsnJ
I MCI
2.HN03
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Won-Supsrfund Program
Senator Signature
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Sample
Collection
G
Staflon
location
Number
Regional Spedlte
Tracking Numb®?
or Teg Numbers
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-------
ENVIRONMENTAL PROTECTION AGENCY
Office of Enforcement
CHAIN OF CUSTODY RECORD
REGION 9
75 Hawthorne Street
San Francisco, California 94105
PROJ. NO
PROJECT NAME
SAMPLERS (Signature)
STA NO
DATE
TIME
STATION LOCATION
NO.
OF
CON-
TAINERS
REMARKS
X
G
Relinquished by: {Signature)
Date /Time
Received by: tsi&ioturo)
Retinquijhcd by: tSif/noturol
Date /Time
Received by: fStgnotural
elmquished by: (Signature)
Date /Time
Received by: ISignaturol
Relinquiihed by: tSirjnoturel
Dote / Time
Received by: (Signature)
lelinquished by: (Signoturol
Ooto /Time
Received (or Laborofory by:
Dote /Time Remarks
Distribution: Otgtnol Aeeom^cnlCB Shlpmani; Copy to Coordinator Plold Plloo
7
-------
ono fora par laboratory and per saatria for aaeh aospling ev^? Vte ^$3 /**& **&4^
Equip / Field / Trmval «=====_=====1===. >^? ^ &W /°»^ °^<^
Equip / Fisld / Travsl
-------
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
REGION IX
75 Hawthorne Street
San Francisco, CA 94105
MEMORANDUM
DATE;
SUBJECT!
FROM?
THROUGH5
TO:
December 16, 1992
Revised Region 9 guidance for preparation of
opling plans for EPA-lead Superfund projects
brTEnviroranental Scientist
Quality Assurance Management Section, P-3-2
Kent Kitchingman, Ch
Quality Assurance Manag
Section, P-3-2
Superfund Remedial Proj'ectyManagers, H-6-1, H-6-2,
H-5-3, H-6-4, H-7-1, H-7-2
Superfund Site Assessment Managers, H-8-1
Superfund Project Officers, H-8-2
The following is a summary of the changes in the Region 9 sampling
plan guidance revised in November 1992„
The most significant change in the guidance is the new SAS
procedure. Other significant changes involve the preservation
protocol for volatile organic samples and the required inclusion of
the CERCLIS identification number in the Request for Analysis
section.
Please ensure that your contractors (EPA-lead sites, anyone using
the CLP) are aware of this revised field sampling plan guidance.
Sample Plan Training will be conducted in the near future. Contact
Robbie Hedeen at 415/744-1535 to request this training or for any
questions concerning the sample plan guidance.
1. New SAS Request proceduress
Section V; Request for Analysis
A; The entire Narrative Request for Analysis section
has been revised to reflect the preparation of new
Special Analytical Services (SAS) Client Request
Forms (CRFs), the procedures for obtaining and
using "generic" SAS CFRs, and the requirements for
inclusion of SAS CRFs in sampling plans.
Appendix Ds
Contains the SOP for completing or creating a
new SAS CRF.
-------
2. Other revisions;
Introduction:
Paragraph 7 clarifies the required sections of an
amendment to an existing sample plan. The
requirements include an entire Request for
Analysis section complete with all SAS CRFs.
Section V: Request for Analyses
Paragraph 4 provides updated examples of RAS+SAS
analyses. Low quantitation limit (25 ml purge)
volatile analysis and RAS analyses with
additional compounds are no longer considered
RAS+SAS. They have been redefined by SMO as SAS
analyses.
Section V.A; Narrative Request for analyses
Paragraph 1 requires that the Site CERCLI8 ID is
included in the paragraph summarizing the lab
analyses to be performed.
Section VI.Ds Field Methods and Procedures
Sample Containiers
A notice regarding the collection of soil samples
in metal sleeves has been added.
Bibliography: The bibliography has been expanded.
Appendix A: Contains an expanded ESB Referral List.
Revised Field Investigation Flow Chart.
Appendix B: Revised Sampling Plan Cover Sheet format.
Appendix C; Contains an updated Target Compound List.
Appendix D: Contains the SAS CRT SOP, including examples.
Appendix F: Revised VGA preservation procedure.
Contractual and Analytical Holding Times are
defined.
Appendix Gs Current CLP Paperwork instructions.
ccs Superfund Section Chiefs (except H-7-4)
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