-------
-------
NOTICE
The policies and procedures set forth here are intended as guidance to Agency and other government
employees. They do not constitute rulemaking by the Agency, and may not be relied on to create a
substantive or procedural right enforceable by any other person. The Government may take action that is
at variance with the policies and procedures in this manual.
For further information on the Contract Laboratory Program (CLP) or to obtain a copy of the User's Guide
to the Contract Laboratory Program, contact the National Technical Information Service (NTIS) of the
United States Department of Commerce at (703) 487-4650. In addition, the entire current Superfund
bibliography may be purchased from NTIS at (703) 487-4650.
Additional copies of this manual can be obtained from:
National Technical Information Service
U.S. Department of Commerce
5285 Port Royal Road
Springfield, VA 22161
(703) 487-4650
-------
CONTENTS
Page
LO THE CLP NETWORK 1
1.1. Procurement of Contract Laboratory Services 3
1.1.1. Procedures for requesting/scheduling analytical services 3
1.1.2. Chain of Communication within the CLP 3
2.0 CONTRACT LABORATORY 4
3.0 SAMPLE COLLECTION 5
3.1 Sample Definition 5
3.2 CLP Analytical Services and Project Data Quality Objectives 7
3.3 References to CLP Laboratory Services in QAPPs and SAPs 8
3.4 Sample Volume 8
3.5 Sample Containers 9
3.6 Quality Control Samples 9
3.7 Duplicate and Split Samples 11
3.8 Performance Evaluation Samples 11
3.9 Recommendations for CLP Analytical Services Sample Preservation and Holding
Times 11
4.0 GENERAL SAMPLING TECHNIQUES AND CONSIDERATIONS . 15
4.1 General Sampling Techniques 15
4.2 Special Sampling Considerations 15
5.0 SAMPLE DOCUMENTATION 18
5.1 Case Number/Sample Delivery Group 18
5.2 Sample Number 18
5.3 Sample Tag 20
5.4 Traffic Report/Chain-of-Custody Forms 21
5.5 Field Operations Records Management System 22
5.6 Custody Seal 29
6.0 SAMPLE PACKAGING AND SHIPPING 30
6.1 Sample Packaging 30
6.2 Sample Shipping 34
6.3 Potential Sampling Problems 34
6.4 Reporting Sample Shipment 35
6.5 Sample Cooler Returns 36
7.0 COMMUNICATION NETWORK 39
8.0 GLOSSARY 41
9.0 EPA REFERENCE DOCUMENTS 44
111
-------
LIST OF EXHIBITS
Page
Exhibit 1-1 CLP Organization Chart .... 2
Exhibit 1-2 Chain of Communication within the CLP 3
Exhibit 2-1 Contract Laboratory Program Analytical Services :, 4
Exhibit 3-1 Sampling at Leroy's Pond 6
Exhibit 3r2 Table of Sampling at Leroy's Pond 6
Exhibit 3-3 Low/Medium Organics Sample Volume 9
Exhibit 3-4 Low/Medium Inorganics Sample Volume 9
Exhibit 3-5 Sample Container Types : 10
Exhibit 3-6 QC Samples 12
Exhibit 3-7 Recommendations for Sample Preservation and Technical Holding Times 14
Exhibit 5-1 CLPAS Sample Labels .. . . 19
Exhibit 5-2 CLPAS Regional Letter Codes 19
Exhibit 5-3 Sample Tag 20
Exhibit 5-4 Sample Tag Instructions 21
Exhibit 5-5 Organic TR/COC Form Example 24
Exhibit 5-6 Inorganic TR/COC Form Example 26
Exhibit 5-7 Organic and Inorganic Traffic Report/Chain-of-Custody Forms Instructions 28
Exhibit 5-8 Purpose Codes 29
Exhibit 5-9 Custody Seal 29
Exhibit 6-1 Sample Packaging 32
Exhibit 6-la Sample Packaging 32
Exhibit 6-2 Sample Cooler With Documentation 33
Exhibit 6-2a Sample Cooler With Documentation 33
Exhibit 6-3 Sealed Cooler . 34
Exhibit 6-4 Top of Cooler 35
Exhibit 7-1 Regional Technical Project Officers 38
Exhibit 7-2 RSCC Addresses and Contacts 39
Exhibit 7-3 CLASS Contacts 40
IV
-------
PREFACE
The Sampler's Guide to the Contract Laboratory Program has been prepared by the U.S. Environmental
Protection Agency Analytical Operations Center. It is specifically designed for samplers to help clarify
sampling procedures necessary to submit samples for CLP analysis. The Sampler's Guide to the Contract
Laboratory Program acts as a reference for the Regions and sampling contractors to promote consistency
in sampling procedures throughout the Regions and to ensure the proper adherence to CLP requirements.
This document is intended to be used as a supplement to, not as a replacement for, existing Regional
sampling instructions.
-------
ACKNOWLEDGMENTS
This document was developed by EPA's Office of Emergency and Remedial Response (OERR). The
efforts of the work group who assisted in the rewrite of this manual include:
A. F. Beliveau
Philip Guarraia
Hanif Sheikh
Fred Sloan
Gary Bennett
Brian Freeman
Christie Macdowell
Jim Gindelberger
TinaDiebold
Gail Jones
Laura Castrilli
Bruce Woods
Robert Melton
from the Headquarters' staff:
Patricia Gowland,
Howard Fribush,
Michael Wilson and
Lucinda Taylor.
Region 1,
Region 2,
Region 2,
Region 4,
Region 4,
Region 5,
Region 6,
Region 6,
Region 8,
Region 9,
Region 10,
Region 10 and
Region 10
VI
-------
1.0 THE CLP NETWORK
The Contract Laboratory Program (CLP) is a national program of commercial contractor laboratories supporting the
Environmental Protection Agency's (EPA's) Superfund nationwide effort to clean up designated hazardous waste sites.
Superfund was originally established under the 1980 Comprehensive Environmental Response, Compensation, and
Liability Act (CERCLA), and presently exists under the 1986 Superfund Amendments and Reauthorization Act (SARA).
The CLP provides chemical analytical services using state-of-the-art technology for the ten EPA Regions. The program
is structured to provide data of known and documented quality for use in supporting EPA enforcement actions or other
user needs. To achieve this goal, the CLP has established strict quality assurance procedures and detailed documentation
requirements.
The CLP is directed by the Analytical Operations Center (AOC) in the Office of Emergency and Remedial Response
(OERR) in the Office of Solid Waste and Emergency Response (OSWER). AOC includes the Organic and Inorganic
Program Coordinators and the Administrative Project Officers (APOs) for the CLP laboratories, the Project Officer for
the Contract Laboratory Analytical Services Support (CLASS) contract, the Project Officer for the Quality Assurance
Technical Support (QATS) contract, the National Automated Data Processing (ADP) Manager, and the Quality
Assurance Coordinator. AOC responsibilities include the following:
Development of analytical methods;
Development of the Statements of Work (these documents define required analytical methods; quality
control, detection/quantitation limits and holding times) for the analytical services procured under the CLP;
Development of and implementing policies and budgets for Superfund analytical operations;
Development of information management policies and products for analytical data;
Management of the CLASS and QATS contracts;
National administration, evaluation, and management of the CLP; and
Direction of CLP quality assurance activities in coordination with overall OSWER quality assurance
activities.
In coordinating Superrund sampling efforts, AOC is supported by the APOs, the contractor-operated CLASS office, the
Regional Technical Project Officers (TPOs), the Regional Sample Control Centers (RSCCs), and the Regional Site
Managers (Site Assesssment Managers, On-Scene Coordinators and Remedial Project Managers). See Exhibit 1-1 for
a generalized organization chart (functions may vary by Regions).
Currently, AOC is allowing other Agencies/Departments the opportunity to "buy-into" the CLP. This is being done on
a cost-reimbursable basis through Interagency Agreements.
Administrative Project Officer
The APO is responsible for monitoring laboratory performance, initiating contract action, and funding laboratory
contracts. The APO works closely with the TPOs and laboratories to resolve problems. The APO is also responsible
for developing analytical methods and designing new CLP services.
-------
Contract Laboratory Analytical Services Support
The CLASS contractor provides management, operations, and administrative support to the CLP. The CLASS
contractor routinely receives Regional analytical requests, coordinates and schedules sample analyses, tracks sample
shipments and analyses, receives and checks data for completeness and compliance, processes laboratory invoices, and
maintains a repository of sampling records and program data.
Regional Technical Project Officer
The TPO monitors the technical performance of the contract laboratories in his or her Region. The TPO works closely
with the APOs in responding to laboratory technical problems and leads laboratory on-site evaluations. The TPO is the
sole Regional official who may contact the CLP laboratories.
Regional Sample Control Center
In most Regions, the RSCC coordinates the sampling efforts and serves as the central point of contact for sampling
questions and problems. The RSCC assists in coordinating the level of Regional sampling activities to correspond with
the monthly projected demand for analytical services.
Regional Site Manager
The Regional Site Manager (Site Assessment Manager, On-Scene Coordinator or Remedial Project Manager) is
responsible for coordinating the development of data quality objectives and for overseeing project-specific remedial
contractors, state officials, or private parties conducting site sampling efforts.
Exhibit 1-1. CLP Organization Chart
Administrative Reject ^
Officers (APOs) J
Contract Laboratory
Analytic a I Services
Support (CLAS9
CLP
Laboratories
Regional
"fechnical Project
. Officers QPOs)
Samplers
1
Regional Sample
Control Centers
(FSCCs)
1
FtegionalSlte Managers
-------
1.1.
PROCUREMENT OF CONTRACT LABORATORY SERVICES
1.1.1. Procedures for requesting/scheduling analytical services.
To initiate a CLP Analytical Services (CLPAS) request, the RSCC or Regional/Agency designee contacts the
appropriate CLASS Coordinator by telephone or fax and provides a complete description of the analytical requirement.
The information required to initiate a CLPAS request includes the sampler's name, sampler's phone number, site name,
city and state where the site is located, site spill identification number, expected date of sample shipment, number of
samples, type of analyses, turn-around-time, fractions to be analyzed, and sample matrix.
1.1.1. Timing and scheduling
By noon eastern time on the Wednesday of the week prior to the scheduled start of a planned sampling activity, the
RSCC or Regional/Agency designee contacts the CLASS Coordinator to place a CLPAS request and to provide
scheduling information to the CLASS contractor. This lead-time enables the laboratories to prepare for EPA samples,
and to provide for resolution of sampling questions. It also allows the sampler time to prepare the required sample
documentation prior to field activity, if appropriate. Late scheduling requests (i.e., requests received between
Wednesday noon and the date of sampling) are accommodated with available laboratory capacity. To avoid possible
shortfalls, Regions are strongly encouraged to submit all CLPAS scheduling requests prior to Wednesday noon, when
possible. A more complete discussion of the procedures for arranging CLP analytical services can be found in the
User's Guide
to
the
Contract
Laboratory
Program.
1.1.2.
Chain of
Communica
tion within
the CLP
Exhibit 1-2.
CLP Users/Clients
Analyoes Scheduling and Rtorttlzation
Analyses requests
Analytical Operations
Cental/
Contractor-Operated
Contract Laboratory
lytical Services Support
Scheduling
Contract
Compliance
Screening
Invoicing
Contract
oratories
-------
2.0 CONTRACT LABORATORY ANALYTICAL SERVICCES SUPPORT
The CLP provides the user community with a wide range of Contract Laboratory Program Analytical Services (CLPAS)
through laboratories that have been awarded government contracts under the CLP.
CLPAS services generally apply to the analysis of water and soil/sediment samples for specific target organic and
inorganic analytes, and are performed under firm, fixed-price; standardized contracts that include standard analytical
methodologies, quality assurance and quality control (QA/QC) procedures, and data reporting formats. The CLP
analytical services are shown with their corresponding fractions and concentrations in Exhibit 2-1.
EPA Regions may request a portion of the analytical services provided under the CLP. For example, CLP Analytical
Services-volatile analysis may be ordered without CLP Analytical Services-semi-volatile analysis or CLP Analytical
Services-pesticide/Aroclor analysis. However, CLP Analytical Services-pesticide analysis may not be ordered without
CLP Analytical Services-Aroclor analysis, since fractions may not be split.
Exhibit 2-1. Contract Laboratory Program Analytical Services
STATUS
OF
SERVICE
Available
ANALYTICAL
SERVICES
Multi-Media,
Multi-
Concentration
Organics
(Low/Medium)
Multi-Media,
Multi-
Concentration
Inorganics
(Low/Medium)
Low Concentration
Organics
Water Quality/
Wet Chemistry
FRACTIONS
Volatiles,
Semivolatiles,
Pesticides/Aroclors
Total Metals,
Dissolved Metals,
Cyanide
Volatiles,
Semivolatiles,
Pesticides/Aroclors
Alkalinity,
Ammonia,
Total Organic Carbon,
Chemical Oxygen Demand,
Chloride,
Nitrate/Nitrite,
Phosphorus,
Total Dissolved Solids,
Total Suspended Solids,
Sulfate
CONCENTRATION1
Low,
Medium
Low,
Medium
Low3
Low, Medium, High
MATRIX
Water, ,
Soil/
Sediment
Water,
Soil/
Sediment
Water
Water
'
TURN-
AROUND
TIMES2
14 or 35 days, '
depending on
contract
requirements
14 or 35 days,
depending on
contract
requirements
14 days
14 days
See Section 3.1, CLPAS Sample Definition, for the definitions of low, medium, and high concentrations.
Turnaround times are the maximum time allowed under the CLPAS contracts for laboratory submission of all reporting
and deliverable requirements. Turnaround times for each sample are calculated from the day on which the sample is
received at the CLP laboratory, as recorded on the shipper's delivery receipt and traffic report/chain-of-custody form.
Low concentration for these services refers to the analytical quantitation limits for drinking water samples.
-------
3.0 SAMPLE COLLECTION
3.1 Sample Definition
A CLP Analytical Services sample is defined by one sample matrix at one concentration level from one station location
for each individual or set of analytical fraction(s), provided the fractions are all requested from the same CLP Analytical
Service. CLP Analytical Services are generally used to analyze low and medium concentration samples. Low
concentration samples are considered to be those samples collected in areas where immediate hazards are thought to
be significantly reduced either by normal environmental processes or because of limited contamination. Medium
concentration samples are most often those collected on-site in areas of moderate dilution by normal environmental
processes. High concentration samples are considered to be those collected directly from drums, pits, ponds, lagoons,
or areas where no dilution of waste is evident [these sample analyses are not available under current CLP Statements
of Work], For the most current definition of low or medium concentration please refer to the current CLP Statements
of Work. The sampler must identify low, medium, and high concentration samples in the field in order to determine
sample collection volume, packaging, and shipping procedures. CLP Analytical Services matrices can be water, soil
or sediment. In some instances a mixed-matrix sample may be collected which contains either a supernatant (for a
sediment/soil sample) or a precipitate (for a water sample). In those instances, it is best to discuss the required
procedures with the TPO or APO. In general, two individual samples should be collected by separating the aqueous
layer from the solid/precipitate layer at the point of collection is preferable.
A CLP Analytical Services sample consists of all sample aliquots (portions) from one station location, for one matrix,
for one analytical program, for one laboratory necessary to collect appropriate volumes needed for the analysis of each
fraction. One CLP Analytical Services sample may be contained in several bottles and vials. For example for the
Low/Medium Organics CLP Analytical Service, one water sample might consist of all of the containers needed for the
three analytical fractions available under this service (i.e., volatile fraction, semi-volatile fraction, and pesticide/Aroclor
fraction), even though the fractions will be collected in separate containers. Therefore, the fractions of the CLP
Analytical Service, along with the type of matrix and the expected concentration level (low/medium or high level),
determine container type and volume.
As an example, let's say you are sampling at Leroy's Pond (see Exhibits 3.1 and 3.2). You are instructed to collect one
low/medium concentration water sample and one low/medium concentration soil/sediment sample, each to be analyzed
for all of the low/medium organic and inorganic fractions available through CLP Analytical Service. According to CLP
guidelines, each individual inorganic sample may be analyzed for total metals or dissolved metals, but not both. If you
.want data for both dissolved metals and total metals from the same station location, you must collect two separate
samples and assign them each unique CLP sample numbers.
For the CLP Analytical Services Multi-Media, Multi-Concentration Inorganics (Low/Medium) contract, the analytical
fractions of interest are total metals and cyanide. For the CLP Analytical Services Multi-Media, Multi-Concentration
Organics (Low/Medium) contract, the analytical fractions of interest are volatiles, semivolatiles, and pesticides/Aroclors.
In the future it will be possible to consider the Organic Low Concentration (water only) service.
-------
Exhibit 3-1. Sampling at Leroy's Pond
Leroys
Pond:
[Station #2j
1-8 ounce
MFQ572 f: ;;IMFQ573
(Fidd QC)
two 1-liter
(L»b Daplicale)
MFQ571
2-40ml VOA .,
(Matm Spike Dnp) ^Y
one 1-galbn one 1-gallon
amber El
FP896
Exhibit 3-2. Table of Sampling at Leroy's Pond
MATRIX
Water
Soil/Sediment
Total number of samples collected = 4
LOW/MEDIUM ORGANICS
, Volatiles
Semivolatiles
Pesticides/Aroclors
Volatiles
Semivolatiles
Pesticides/Aroclors
2 organic samples
(1 water + 1 soil/sediment)
LOW/MEDIUM INORGANICS
Total Metals
Cyanide
Total Metals
Cyanide
2 inorganic samples
(1 water + 1 soil/sediment)
6
-------
Because you are collecting samples from two matrices for two analytical services, you must collect four separate
samples: one water sample and one soil/sediment sample to be analyzed for CLP Analytical Services organics and one
water sample and one soil/sediment sample to be analyzed for CLP Analytical Services inorganics. Note that a single
sample may consist of several containers because each fraction and each concentration category require a certain volume
for analysis.
3.2 CLP Analytical Services and Project Data Quality Objectives
Before requesting CLP Analytical Services, project managers should evaluate whether the services offered under the
CLP are appropriate to meet the Data Quality Objectives (DQOs)1 established for their project. This evaluation should
take place during the planning stages of a sampling project and be documented in the Quality Assurance Project Plan
(QAPP)1 and/or the Sampling and Analysis Plan (SAP)1.
The following specifications/features of CLP Analytical Services (this information is generally found in the Statement
of Work for the analytical service) should be evaluated to determine the adequacy of the standardized services to meet
the project DQOs:
list of included target analytes/compounds
sample concentrations covered
required minimum sample volumes
laboratory subsample size
sample preparation and digestion methods
analytical methods
turnaround times
Instrument Detection Limits
Contract Required Quantitation/Detection Limits
QA/QC requirements (e.g., identity, frequency, and acceptance criteria for laboratory QC samples)
laboratory sample receipt and custody requirements
data package deliverables '(reporting requirements)
For example, the detection limits required to meet the project DQOs for some risk assessments might be lower than the
Contract Required Detection Limits offered by the CLP. The standard CLP digestion and analytical methods might not
be suitable for the sample matrix of interest. The CLP data turnaround times might be too long for some emergency
response sampling projects. For situations such as the emergency response scenario, it is possible that a combination
of CLP Analytical Services for the non time-critical analytes and alternative fast-turnaround services (14-day turn
around time) for the time-critical analytes would be adequate to meet the project DQOs.
'For more information regarding QA and SAP planning and the DQO process, consult the documents listed in
Section 9.0 of this guide.
-------
If it is determined that CLP Analytical Services will not be .adequate for all or some of the samples to be collected,
alternatives should be explored. Each EPA Region may have developed analytical services options to supplement the
laboratory services available nationally through the CLP. Contact the appropriate Regional analytical services
representatives (usually the personnel listed in Section 7.0, Communications Network) for guidance in obtaining
analytical services that will meet project DQOs.
3.3 References to CLP Laboratory Services in QAPPs and SAPs
QAPPs and SAPs typically contain sections describing analytical laboratory services. Standard, or boiler-plate, language
is often used to describe laboratory requirements for procedures such as sample receipt and notification and laboratory
participation in analyzing Performance Evaluation Samples (PESs). CLP contract specifications are designed to
incorporate many of the most common good laboratory practice requirements, such as the requirement for laboratory
Quality Management Plans (QMPs for further information see Section 9.0). If CLP Analytical Services will be
requested for all or some of the samples covered in a QAPP and/or SAP, care should be taken to ensure that the
QAPP/SAP descriptions of laboratory services for the CLP-destined samples are compatible with the CLP contract
specifications. For example, CLP contracts do not allow CLP laboratories to contact samplers directly regarding
problems with sample receipt. (Note that only the EPA Contracting Officer for the CLP has the authority to modify CLP
contract specifications.) It is generally the responsibility of the project manager to make sure that the project
laboratory services requirements are communicated to the Regional analytical services representatives.
QAPPs and/or SAPs also typically include standard operating procedures (SOPs) for procedures such as completing
chain-of-custody forms, sample identification, and sample packaging and shipment. SOPs that will be used when
collecting samples for analysis through the CLP should be reviewed before use to ensure that CLP requirements are
accommodated. Many consultants' SOPs call for the site name to be provided on the form. However, for CLP
Analytical Services samples, Case Numbers, rather than site names are used. SOPs associated with the collection of
CLP samples should be reviewed before use to ensure that CLP requirements are accommodated.
In addition, QAPPs and SAPs specify such information as the analytical methods and laboratory QC requirements that
will be used for samples. When CLP Analytical Services will be requested for samples, it is common for the QAPP or
SAP to reference the appropriate CLP Statement of Work (SOW) for details such as the laboratory QC sample
frequencies. There is often confusion regarding how to reference CLP SOWs, because several versions of a SOW for
a particular analytical service, such as "Low/Medium Organics," may be active under contracts at the same time. Also
QAPP and SAP authors do not control CLP laboratory assignments and will not know in advance which laboratory and
. corresponding SOW version will be assigned for their samples. Therefore, QAPP and SAP authors should refer to CLP
SOWs as in the following example:
"Low/medium concentration soil samples will be analyzed according to the specifications of the current EPA
Superfund Contract Laboratory Program Statement of Work for Multi-Media, Multi-Concentrations Organics."
3.4 Sample Volume
The collection of proper sample volume is imperative to the success of sample analysis. If sufficient sample volume
is not collected, the analysis of all required parameters and complete quality control determinations may not be possible.
(See Section 3.6, Quality Control Samples.) Therefore, it is especially important to note the volume requirements for
each specified. If adequate sample volume cannot be collected, notify the authorized RSCC or CLP Analytical Services
Support personnel sample immediately. Note that more than one container may be required to provide the total volume
of sample needed (e.g., two-40-ml glass vials for one volatile organic compound [VOC] analysis). Exhibits 3-3 and 3-4
specify the required sample volume and container type for each CLP Analytical Services fraction. Container type codes
are detailed in Section 3.5, Sample Containers, and in Exhibit 3-5.
-------
Exhibit 3-3. Low/Medium Organics Sample Volume
SAMPLE
MATRIX
Water
Soil/
Sediment
CONCENTRATION
Low/Medium
Low/Medium 2
FRACTION
Volatiles
Semivolatiles
Pesticides/Aroclors
Volatiles
Semivolatiles
Pesticides/Aroclors
LABORATORY
QC SAMPLE
VOLUME
4 each (40 mL)
4L
4L
4 each (40 mL)
4oz.
4oz.
MINIMUM
SAMPLE
VOLUME
2 each (40 mL)
2L
2L
2 each (40 mL)
4 oz.
4oz.
CONTAINER
TYPE1
BorD
A,E,F,G,H,J,orK
A,E,F,G,H,J>orK
DorB
A,E,F,G,H,J, or K
A,E,F,G,H,J,orK
1 Some sample containers may have small neck sizes and inhibit sampling efforts. See Exhibit 3.4 for container types.
2 All medium soil/sediment sample containers should be double contained before shipment (e.g., sample bottle/jar/vial
placed in clean, lidded metal paint can). Consult DOT regulations for applicable shipping requirements.
Exhibit 3-4. Low/Medium Inorganics Sample Volume
SAMPLE
MATRIX
Water
Soil/
Sediment
CONCENTRATION
Low/Medium
Low/Medium 2
FRACTION
Total Metals
Dissolved Metals
Cyanide
Total Metals
Cyanide
LABORATORY
QC SAMPLE
VOLUME
1L
1L
1.5 L
6oz.
6oz.
MINIMUM
SAMPLE
VOLUME
1L
1L
1L
6oz.
6oz.
CONTAINER
TYPE1
A,C,E,F,G,H,J,K, or L
A,C,E,F,G,H,J,K, or L
A,C,E,F,G,H,J,K, or L
A,C,E,F,G,H,J,K, or L
A,C,E,F,G,H,J,K,orL
Some sample containers may have small neck sizes and inhibit sampling efforts. See Exhibit 3.4 for container types
All medium concentration soil/sediment sample containers should be double contained before shipping (e.g., sample
bottle/jar/vial placed in clean, lidded metal paint can). Consult DOT regulations for applicable shipping requirements.
3.5 Sample Containers
Exhibit 3-4 lists sample containers generally used during sample collection. Always use clean sample containers of an
assured quality. For container cleaning procedures and additional container information, refer to the current iteration
of Specifications and Guidance for Contaminant-Free Sample Containers,
December 1992, OSWER Directive 92.0-05A. See Exhibits 3-3 and 3-4 for sample volume requirements. Samplers
may wish to purchase pre-pleaned/quality assured bottles in lieu of cleaning their own bottles.
3.6 Quality Control Samples
QC samples are used to estimate the precision and accuracy of analytical results and to examine sources of error
introduced by field and laboratory practices. A designated number of field QC samples may be included in each batch
of samples which are sent to the CLP laboratory, as specified by the Sampling and Analysis Plan. A designated number
of laboratory QC samples must be included in each batch of samples which are sent to the laboratory, as specified by
-------
Exhibit 3-5 Sample Container Types
CONTAI
NER
TYPE
A
B
C
D
E
F
G
H
J
K .
L
M
SPECIFICATIONS
Container: 80-oz. amber glass, ring handle bottle/jug, 38-mm neck finish.
Closure: Polypropylene or phenolic cap, 38-430 size; 0.015-in Teflon liner.
Container: 40-mL glass vial, 24-mm neck finish.
Closure: Polypropylene or phenolic, open-top, screw cap, 15-cm opening, 24-400 size.
Septum: 24-mm disc of 0.005-in Teflon bonded to 0.120-in silicon for total thickness of 0.125-in.
Container: 1-L high density polyethylene, cylinder-round bottle, 28-mm neck finish.
Closure: Polyethylene cap, ribbed, 28-410 size; F217 polyethylene liner.
Container: 120-mL wide mouth glass vial, 48-mm neck finish.
Closure: Polypropylene cap, 48-400 size; 0.015-in Teflon liner.
Container: 16 oz. tall, wide mouth, straight-sided, flint glass jar, 63-mm neck finish.
Closure: Polypropylene or phenolic cap, 63-400 size; 0.015-in Teflon liner.
Container: 8-oz. short, wide mouth, straight-sided, flint glass jar, 70-mm neck finish.
Closure: Polypropylene or phenolic cap, 70-400 size; 0.015-in Teflon liner.
Container: 4-oz. tall, wide mouth, straight-sided, flint glass jar, 48-mm neck finish.
Closure: Polypropylene or phenolic cap, 48-400 size; 0.015-in Teflon liner.
Container: 1-L amber, Boston round, glass bottle, 33-mm pour-out neck finish.
Closure: Polypropylene or phenolic cap, 33-430 size; 0.01 5-in Teflon liner.
Container: 32-oz. tall, wide mouth, straight-sided, flint glass, 89-mm neck finish.
Closure: Polypropylene or phenolic cap, 89-400 size; 0.015-in Teflon liner.
Container: 4-L amber glass, ring handle bottle/jug, 38-mm neck finish.
Closure: Polypropylene or phenolic cap, 38-430 size; 0.015-in Teflon liner.
Container: 500-mL high-density polyethylene, cylinder-round bottle, 28-mm neck finish.
Closure: Polypropylene cap, ribbed, 28-410 size; F217 polyethylene liner.
Container: 120-mL wide mouth glass vial, 48-mm neck finish.
Closure: Polypropylene cap, 48-400 size; 0.015-in Teflon liner.
the CLP contract. Because the amount and type of QC samples collected vary between Regions, always refer to
Regional guidance. Note that the types and frequencies of field QC samples should always meet project DQOs.
Field QG samples may include field duplicate samples, trip blanks, equipment blanks, and field blanks. The field QC
samples should be prepared (i.e., labeled, packaged, preserved, and shipped to the assigned laboratory) identically to
the primary field samples, and should remain "blind" to the laboratory to ensure indiscriminate handling. Each field
QC sample receives a separate sample number. See Section 5.0, Sample Documentation.
Laboratory QC samples include matrix spikes and matrix spike duplicates for organic samples and matrix spike and
sample duplicates for inorganic samples. The laboratory QC sample is an additional volume of an existing sample
required by the laboratory's contract; the additional volume must be supplied by the sampler (see exhibits 3-3 and 3-4).
Samplers should designate one sample per matrix per 20 samples as a "laboratory QC" sample. If the sampler
does not designate a sample as the "laboratory QC," then it is possible that the laboratory could select the blank as the
QC or use the primary field samples to meet contract QC requirements. The laboratory use of primary field samples
for QC analysis can detract from data quality and useability. For example, if a laboratory requires two liters of field
sample to perform a requested analysis without QC, and the laboratory receives two liters of field sample to perform
the requested analysis along with matrix spike and duplicate analyses, the laboratory may split the field sample using
10
-------
one liter for the required analysis and one half liter each for the matrix spike and duplicate analyses. In doing so, the
laboratory will double the achievable sample quantitation limits, and possibly fail to meet project DQOs. Samplers
should label the laboratory QC sample containers and corresponding paperwork as "lab QC" as described in Section 5.4,
Traffic Report/Chain-of-Custody Forms. Remember that the laboratory QC sample is not an additional sample and does
not receive its own unique sample number. Exhibit 3-6 explains some of the types of QC samples that may be collected.
Follow volume requirements as specified in Section 3.4, Sample Volume.
3.7 Duplicate and Split Samples
Duplicate samples may be collected to determine the variability of the sampling process. Duplicate samples should be
collected simultaneously from the same source and under identical conditions as the original sample. Aqueous duplicate
samples are collected from successive volumes from the same sample source and device (e.g., bailers). Soil duplicates
are collected from the same sample source and device.
Split samples may be collected to measure the variability between laboratories. The sample should be collected by
separating one sample into two or more sample containers. Aqueous split samples should be collected by either
obtaining consecutive sample volumes from the same bailer or mixing the volumes in a large intermediate vessel, as
appropriate, depending on the nature of contaminants and Regional guidance. When collecting aqueous samples with
devices, such as a bailer, for example, the following guidance should be followed. If more than one bailer is required
to obtain the required sample volume, the first half volume of the first bailer should be poured into the first container,
and the second half volume of the first bailer should be poured into the second container.
The first half volume of the second bailer should be poured into the second container, and the second half volume of
the second bailer should be poured into the first container. This filling sequence should continue until both containers
are filled. Please note that when sampling for VOC analysis, more than one bailer should not be used and sample
mixing should be avoided because these procedures may increase analyte loss due to evaporation. Refer to Section
4.2.1, Volatile Organic Compound Collection, for guidelines on collecting samples for VOC analysis. When splitl
samples are collected using an intermediate vessel, continually stir the contents of the intermediate vessel with a clean
pipette or precleaned Teflon rod, and allow the contents to be alternately siphoned into respective sample containers
using Teflon tubing. Any device used for stirring, or tubing used for siphoning, must be cleaned in the same manner
as other equipment. Since a true split for sediment, sludge, and soil samples is not feasible under field conditions, a split
soil sample should be considered a duplicate.
3.8 Performance Evaluation Samples
A Performance Evaluation Sample (PES) is a specially prepared Quality Control sample which is used to evaluate a
laboratory's analytical proficiency. Most of the Organic PESs are supplied in ampules while most of the Inorganic PESs
are supplied in plastic bottles. The frequency of use and the type(s) of PES(s) to be used during a sampling event should
be specifically addressed in the Sampling and Analysis Plan. The availability and use of PESs should be coordinated
through the Regional RSCC and/or TPO contact.
3.9 Recommendations for CLP Analytical Services Sample Preservation and Holding Times
Sample Preservation
Some water samples must be chemically preserved before shipment to the laboratory. All low concentration samples
should be cooled to 4° ± 2°C. Samples should be preserved and cooled immediately upon sample collection.
Preservation techniques vary among the Regions; so use the information in Exhibit 3-7 as general guidance for properly
preserving samples. Contact your RSCC for Region-specific instructions.
11
-------
Exhibit 3-6 QC Samples
QC SAMPLE
Field QC
Samples
Laboratory QC
Samples '
SAMPLE
TYPE
Field
Duplicate2
.Field Blank
Volatiles Trip
Blank
Equipment
Blank or
Rinse Blank
Matrix Spike
and Matrix
Spike
Duplicate
Matrix Spike
and Lab
Duplicate
PURPOSE
To check reproducibility of
laboratory and field
procedures. To indicate
matrix non-homogeneity.
To check cross-
contamination during
sample collection, sample
shipment, and in the
laboratory. Also to check
sample containers.
To check contamination
during sample handling and
shipment from field to
laboratory.
To check field decontam-
ination procedures.
Required by laboratory's
contract to check accuracy
and precision of organic
analyses.
Required by laboratory's
contract to check accuracy
and precision of inorganic
analyses.
COLLECTION1
Collect from areas that are
known or suspected to be
contaminated. Collect one
sample per week or 10%
(Regions may vary) of all field
samples per matrix, whichever
is greater.
Collect for each group of
samples of similar matrix per
each day of sampling. Use
water (demonstrated to be free
of the contaminants of concern)
for organics; use metal-free
(deionized or distilled) water
for inorganics.
Collect one sample (water
demonstrated to be free of the
contaminants of concern) per .
each day of organics sampling.
This sample is prepared off-
site, before sampling
commences, and placed in the
cooler used to ship volatile
samples.
Collect when sampling
equipment is decontaminated
and reused in the field or when
a sample collection vessel
(bailer or beaker) will be used.
Use blank water (water
demonstrated to be organic-
free, deionized or distilled for
inorganics) to rinse the
equipment, and collect this
rinse water into the sample
containers.
Collect triple volume for one
water sample per 20 water
samples. The triple volume
water sample should be
collected in the first shipment
of organics samples.
Collect double volume for one
water sample per 20 water
samples. The double water
volume sample should be
collected in the first shipment
of inorganic samples.
SAMPLE NUMBER
Assign two separate (unique) ,
CLP sample'numbers (i.e., one
number to the primary sample
and one to the duplicate).
Submit blind to the lab.
Assign separate CLP sample
numbers to the field blanks.
Submit blind to the lab.
Assign separate CLP sample
numbers to the trip blanks.
Submit blind to the lab.
Assign separate CLP sample
numbers to the equipment
blanks. Submit blind to the lab.
Assign the primary sample,
extra volume, matrix spike and
matrix spike duplicate the same
CLP sample number. Label the
extra volume "Lab QC."
Assign the primary sample,
extra volume, spike and
duplicate the same CLP sample
number. Label the extra
volume "Lab QC."
Consult Regional guidance for field QC sample frequencies, laboratory QC sample frequencies are fixed in the CLP contracts.
2 A true split for sediment, sludge, and soil samples (and other heterogeneous samples such as highly turbid waters) is typically not feasible
under field conditions. A split of this type of sample should generally be considered a duplicate.
No extra volume is required for the soil/sediment matrix; however, the sample to be used for laboratory QC must be designated on the
TR/COC.
12
-------
Holding Times
Samples should be shipped to scheduled CLP laboratories as soon as possible after collection. Daily shipment of
samples to CLP laboratories is very important, whenever possible, because many samples are stable only for a short
period of time following collection. The technical holding times listed in Exhibit 3-7 are the maximum lengths of
time that samples may be held from the time of collection to the time of analysis and still be considered valid.
Samples that exceed these holding times may not be valid, and re-sampling may be necessary. The contractual
holding times in Exhibit 3-8 are holding times that the CLP laboratory must follow to comply with the terms of the
contract and are described in the CLP Analytical Services SOW. Contractual holding times are the same or shorter
than the technical holding times to allow for sample packaging and shipping.
13
-------
Exhibit 3-7 Recommendations for Sample Preservation and Technical Holding Times
PARAMETER
TYPE
Metals
Inorganics,
Non^detals
Organics
MEASUREMENT
Dissolved
Suspended
Total
Chromium6*
Mercury Dissolved
Mercury Total
Alkalinity
Carbon, Total Organic
Chemical Oxygen
Demand
Chloride
Cyanide
Nitrogen
Ammonia
Nitrate plus Nitrite
Phosphorus
Solids, Total Dissolved
Solids, Total Suspended
Sulfate
Anions by Ion
Chromatography
Pesticides/Aroclors
Semivolatiles
Volatiles (preserved)
PRESERVATIVE
Filter on-site, HNO3 to pH<2,
Cool, 4°C
Filter on-site, Cool, 4°C
HN03 to pH<2, Cool 4°C
Cool, 4°C
Filter, HN03 to pH<2,
Cool,4°C
HNO3 to pH<2, Cool, 4°C
Cool, 4°C
Cool, 4°C, H2SO4 to pH<2
Cool, 4°C, H2S04 to pH<2
None Required
Cool, 4°C, NaOH to pH>12,
0.6 g ascorbic acid 2
Cool, 4°C, H2SO4 to pH<2
Cool, 4°C, H2SO4 to pH<2
Cool, 4DC, H2SO< to pH<2
Cool, 4°C
Cool, 4°C
Cool, 4°C
Cool, 4°C
Cool, 4"C, pH 5-9
Cool, 4°C, store in dark
Cool, 4°C, HC1 to PH<2
TECHNICAL
HOLDING TIME
6 Months '
6 Months
6 Months
24 Hours
28 Days
28 Days
14 Days
28 Days
28 Days
28 Days
14 Days3
28 Days
28 Days
28 Days
7 Days
7 Days
28 Days
28 Days
14 Days
Extract in 7 days
14 Days
CONTRACT
MANDATED
HOLDING
TIME
180 Days4
180 Days4
180 Days4
180 Days4
26 Days4
26 Days4
14 Days
28 Days
28 Days
28 Days
12 Days
28 Days
28 Days
28 Days
7 Days
7 Days
28 Days
28 Days
Extract in 10
Days
Extract in 10
Days
10 Days4
'Source; Adapted from EPA-600/4-82-055, Technical Additions to Methods for Chemical Analysis of Water and Wastes and 40
Code of Federal Regulations § 136. Table II Required Containers, Preservation Techniques, and Holding Times. 1995.
is samples. No official technical holding
r i *L _j i i. _ijr ,L- j ..1 . °.
These are recommendations for sanr r
times are specified for soils/sediments under Superfund. However, EPA-specified contractual holding times do apply to
soil/sediments. See Section 4.2.1, Volatile Organic Compound Collection for recommended procedures for the collection,
handling, and preservation of soil samples to minimize the loss of volatile compounds. Please check your CLP Analytical
Services SOW for required preservatives and holding times.
Samples should be filtered immediately on-site before adding a preservative.
Only use ascorbic acid in the presence of residual chloride. See section 4.2.1.
Maximum holding time is 24 hours when sulfide is present. Optionally, all samples may be tested with lead acetate paper
before the pH adjustment to determine if sulfide is present. If sulfide is present it can be removed by adding, cadmium
nitrate powder until a negative spot test is obtained using lead acetate paper. The sample is filtered and thenNaOH is
Analysis Start Date minus Laboratory Receive Date.
14
-------
4.0 GENERAL SAMPLING TECHNIQUES AND CONSIDERATIONS
4.1 General Sampling Techniques
This section provides information on guidance documents available for collecting CLP Analytical Services samples.
Samples should be collected according to the approved site specific Quality Assurance Project Plan and the Sampling
Analysis Plan (EPA QA/R-5 "£PA Requirements for Quality Assurance Project Plans for Environmental Data
Operations" and EPA Order 5360.1). This document does not define specific sampling procedures for the CLP
Analytical Services because specific sampling protocols depend on individual site conditions, Regional requirements,
and DQOs. Regions may have their own specific requirements for individual sampling programs, the Regions are
responsible for generating Region-specific sampling SOPs. Information regarding surface water, sediment, soil and
groundwater sampling can be found in many documents including the following sources:
Compendium ofERT Surface Water and Sediment Sampling Procedures, EPA/540/P-917005.
Compendium ofERT Soil Sampling and Surface Geophysics Procedures, EPA/540/P-91 /006.
Compendium ofERT Groundwater Sampling Procedures, EPA/540/P-91/007
Quality Assurance Sampling Plan for Environmental Response (QASPER) software, Version 4.1, ERT.
Requirements for the Preparation of Sampling and Analysis Plans, Draft, US Army Corps of Engineers. June
30, 1994. EM 200-1-3.
Other sources are available. This list is not exhaustive.
These documents, along with appropriate Regional guidance and procedures, should be consulted for detailed sample
collection, preservation, handling and storing, equipment decontamination, and quality assurance/quality control
procedures. When working with potentially hazardous materials, follow U.S. EPA and OSHA requirements, specific
health and safety procedures, and Department of Transportation (DOT) requirements.
Regional sampling protocols and Regional QA guidelines should be consulted. Proper procedures for insuring good
sampling results should be followed.
4.2 Special Sampling Considerations
This section provides general guidance for VOC, low concentration contaminant, and duplicate and split sample
collection, along with procedures for sample compositing and mixing. The guidance provided in this section may be
useful and appropriate for the collection of CLP Analytical Services samples.
The Regions should have developed specific SOPs to address the procedures for preserving samples in the field.
Testing and amelioration of carbonates, residual chlorine or oxidants in VOC samples and sulfides and residual chlorine
in extractable fractions should be included in Regional guidance.
4.2.1 Volatile Organic Compound Collection
When collecting samples for VOC analysis, care should be taken to prevent analyte loss by evaporation. The following
procedures are designed to minimize sample contamination and analyte loss during aqueous and non-aqueous VOC
sample collection. Also, be sure to follow Regional guidance to ensure that proper prepreservation treatment is
accomplished (e.g., residual chlorine). See Technical Notes on Drinking Water Methods. EPA/600/R-94/173, page 53.
15
-------
Aqueous VOC Sample Collection
Rinse the vial with sample water prior to actual sample collection and preservation. See Section 3.8, Sample
Preservation and Holding Times, and Exhibit 3-7.
Avoid excessive aeration and agitation of the sample by pouring the sample slowly down the edge of the
sample vial.
Fill vial so that a reverse (convex) meniscus is present (in the case of water in a glass container).
Place septum on the vial so that the Teflon side is in contact with the sample and then tighten the cap.
Immediately invert the vial and lightly tap to locate air bubbles.
If air bubbles are present, discard the sample and recollect the sample. Check the recollected sample for air
bubbles. If air bubbles are present, additional sample water may be added to the vial in an attempt to
eliminate the air bubbles. The presence of air bubbles after three consecutive attempts to rid the sample of
the condition should result in the use of a new sample container and recollection of the sample. Regions vary
in their approach to rinsing the sampling vial and recollecting the sample in the same vial. BE SURE TO
FOLLOW REGIONAL GUIDANCE.
Do NOT mix or composite samples.
Immediately transfer the vial to the sample shuttle [device which contains a "set" of VOC vials] once it has
been collected. Do not allow ice to touch the vials.
Solid VOC Sample Collection
Minimize headspace as much as possible.
Pack sample lightly with either a glass rod, Teflon spatula, or stainless steel spatula.
Secure cap with Teflon-side of septum in contact with sample.
Do NOT mix or composite samples.
Immediately transfer the vial to the sample shuttle once it has been collected. Do not allow ice to touch the
vials.
Wipe outside of sample container to remove excess sample from threads to ensure a tight lid fit.
4.2.2 Contaminant Sampling
Some compounds can be detected in the ppb and/or ppt range. Extreme care must be taken to prevent cross-
contamination of these samples. The following precautions should be taken when trace contaminants are of concern:
Disposable gloves should be worn each time a different location is sampled.
When collecting both surface water and sediments samples, surface water samples should be collected first.
This reduces the chance of sediment dispersal into surface water, and the resulting loss of surface water
sample integrity. '
16
-------
Sampling should occur in a progression from the least to most contaminated area, if this information is
known.
Samplers should use equipment constructed of Teflon, stainless steel, or glass that has been properly
precleaned for collecting samples for trace organics compound analyses. (A set of procedures for cleaning
sampling equipment may be found in Regional guidance. Equipment constructed of plastic or PVC should
not be used to collect samples for trace organic compounds analyses.
4.2.3 Sample Compositing and Mixing
When compositing solid samples, (i.e:, sediment, soil, sludge) for analysis of compounds present in trace quantities, a
stainless steel or Teflon bowl and spatula should be used. Samples for VOC analysis should not be composited to
minimize evaporation. The sample should be thoroughly mixed and divided into subsections in the compositing
container. The procedure for sectioning is as follows:
Roll the contents of the compositing container to the middle of the container and mix.
Quarter the sample and move to the sides of the container.
Mix each quarter individually and roll to the middle of the compositing container.
Mix the sample once more, composite quarter subsamples, place in container.
The approximate quantity of each subsection should be recorded in the field logbook.
17
-------
5.0 SAMPLE DOCUMENTATION
Each sample processed by the CLP must be properly documented to ensure timely analysis of all parameters requested
and to support the use of the sample data in potential enforcement actions. It is the sampler's responsibility to fill out
all appropriate paperwork completely and correctly. This section provides instructions for completing all CLP forms
and other sample documentation. Each EPA Region may require additional documentation. It is important to follow
both the national guidelines and Regional guidelines for CLP Analytical Services samples. Contact your RSCC for
Region-specific instructions and guidance prior to the sampling activity. Contact the Region VII RSCC for information
regarding sample documentation for the Rapid Turnaround Dioxin Analytical Service.
5.1 Case Number/Sample Delivery Group
A Case number is assigned by the CLASS contractor to CLP Analytical Services sampling events and is five digits in
length. Each CLP Analytical Services sampling event receives a distinct Case number which helps maintain site
confidentiality. (Contract laboratories should not know the site name for the samples they are analyzing in order to
avoid potential conflict of interest problems.) The Case number also enables the CLASS contractor and the Region to
easily track CLP Analytical Services sampling events. The Sample Delivery Group (SDG) is a unit within a Case'that
is used to identify a group of samples for delivery. An SDG is defined as one of the following, whichever comes first:
all samples with a Case, or every set of 20 field samples within a Case, or the field samples in a Case which are received
at a laboratory during a specified period of time, beginning with receipt of the first sample in the Case or SDG. Note:
Laboratory QC sample frequencies are based on the SDG.
5.2 Sample Number
The CLP sample number is a unique number that identifies each sample under a CLP Analytical Services analytical
program. A CLP Analytical Services sample is defined by one sample matrix at one concentration level from one station
location for each individual or set of analytical fraction(s), provided the fractions are all requested from the same CLP
Analytical Service. The sample number is preprinted on adhesive labels and is provided by your RSCC, who routinely
orders them from the CLASS contractor. Exhibit 5-1 shows examples of CLP Analytical Service sample labels. Sample
numbers are comprised of a Regional letter code and sequential sample numbering. Regional letter codes are listed in
Exhibit 5-2. Use only the labels provided to the Region in which you are sampling. It is your responsibility to assign
this critical sample number correctly and to transcribe it accurately on the appropriate documentation. Place
the label on the appropriate sample container and transcribe the sample number onto the sample tag and TR/COC
. (Tracking Report/Chain of Custody) form. The unique sample number must only be used for one sample. Destroy all
unused labels to prevent duplication of sample numbers. Do not add digits or hyphens to the CLP sample numbers.
If additional sample numbers are needed in the field, contact your RSCC. The sampler should consider placing clear
tape over the adhesive labels as this procedure will help preserve the information on the adhesive labels. Samplers
should attempt to use the provided CLP sample numbers in numerical order [as much as possible]. All samples must
have sample numbers on the label and tag, if tags are used. The use of sample tags is highly recommended (see Section
5-3).
Organic Sample Numbers
Organic sample numbers are five characters long and have the format XXXXX. The first letter indicates the Region,
the remaining letters and numbers are used for sequential sample numbering (see Exhibits 5-1 and 5-2). Organic sample
numbers are preprinted on labels. For the organic fractions, there are ten labels four for semivolatiles (labeled
extractables), two for volatiles, and four are blank (for pesticides/Aroclors and extra sample volume). Remember that
the unique sample number must only be used for one sample. Destroy all unused labels to prevent duplication of sample
numbers.
18
-------
Inorganic Sample Numbers
.Inorganic sample numbers are six characters long and have the format MXXXXX. The "M" indicates that this sample
is inorganic, the second letter indicates the Region, and the remaining letters and numbers are used for sequential sample
numbering (see Exhibits 5-1 and 5-2). Inorganic sample numbers are preprinted on labels, seven labels per strip. Two
labels are for total metals, two for cyanide and three blanks (for extra sample volume). According to CLP guidelines,
each individual inorganic sample may be analyzed for total metals or dissolved metals, but not both. That is, samples
collected for total metal and dissolved metal analyses must receive separate (unique) sample numbers. Remember that
the unique sample number must only be used for one sample. Destroy all unused sample labels.
Exhibit 5-1. CLP Analytical Services Sample Labels
Organic
BLHOl - Semivolatile
BLH01 -Semivolatile
BLHOl -Semivolatile
BLHOl - Semivolatile
BLHOl -VGA
BLHOl-VOA
BLHOl - Pesticide/Aroclor
BLHOl -
BLHOl
[Blanks may be included]
Inorganic
MBJTOl -Total Metals
MBJT01-Total Metals
MBJTOl-Cyanide
MBJTOl-Cyanide
MBJTOl
MBJTOl
MBJTOl
[Blanks may be included]
Exhibit 5-2. CLP Analytical Services Regional Letter Codes
REGION
I
II
III
IV
V
VI
VII
VIII
LX
X
LETTER CODE
ORGANIC
A
B
C
D
E
F
G
H
Y
J
INORGANIC
MA
MB
MC
MD
ME
MF
MG
MH
MY
MJ
19
-------
5.3 Sample Tag
To support the use of sample data in potential enforcement actions, samples should be identified according to EPA
National Enforcement Investigations Center (NEIC) sample control guidelines. NEIC recommends that samples other
than in situ measurements (e.g., pH, temperature, conductivity) be identified with a sample tag. Each sample aliquot
removed from a hazardous waste site to be transferred to a laboratory for analysis should, therefore, be identified with
a sample tag. The sample tag is returned to (he Region by the laboratory along with the corresporiding data package
as physical evidence of sample receipt and analysis.
< \
Check with your authorized requestor (RSCC or Project Manager, it will vary among the Regions) to determine the
availability of and the specific requirements for sample tags. Tie a sample tag on each sample container. (See Section
6.0, Sample Packaging and Shipping for tying procedures.) Exhibit 5-3 is an example of a sample tag. Exhibit 5-4
contains instructions for completing a sample tag.
Section 6.1, Sample Packaging, contains additional information on sample tags
Exhibit 5-3. Sample Tag
Project Code J «0
ro o
ET
,cr
CO
»
n
d>
p
Station No. 3
26
Station Location
nONITOXINQ WELL *2>
3PUT 5TOON *1I
Remarks:
GA3CNO.I746 *~
3/1AFLT NO. rtlfVOI
Pesticides
O
o
o5
D>
7)
«>
Mc./Day/Yeai4
8/9/9/
7
>
Time O
JOO-7
Designate: O
Com p.
Grab
X
Samplers (Signatures) Q
O
Q&Pvn Q0m&4
o
to
Q.
O
X
Z
o>
s
Phenolics
COO. TOC. Nutrients
BOO Anions Solids
(TSS) (TDS) (SS)
ANALYSES O
Preservative:
YC£] NCTJ 0)
o
20
-------
Exhibit 5-4. Sample Tag Instructions
STEPS
INSTRUCTIONS
STEP1
Under the "Remarks" heading, record the CLP Case number and sample number.
STEP 2
Record the project code (e.g., contract number, work assignment number, Interagency Agreement number,
etc.) assigned by EPA.
STEP 3
Enter the station number assigned by the sampling team coordinator.
STEP 4
Record the month, day, and year of sample collection.
STEPS
Enter the military time of sample collection, e.g., 13:01 for 1:01 p.m.
STEP 6
Place an "X" to indicate composite or grab sample.
STEP?
Record the station location (description) as specified in the project plan.
STEPS
Sign the sample tag with your name.
STEP 9
Place an "X" in the box next to "yes" or "no" to indicate if a preservative was added to the sample.
STEP 10 Under "analyses," place an "X" in the box next to the parameters for which the sample is to be analyzed.
Note: Leave the box for "laboratory sample number" blank.
5.4 Traffic Report/Chain-of-Custody Forms
The organic and inorganic traffic report/chain-of-custody (TR/COC) forms enable the CLASS contractor and the Region
to track CLP Analytical Services samples and ensure that the samples are shipped to the appropriate contract laboratory.
The TR/COC form is functionally similar to a packing slip that accompanies a shipment of goods. The TR/COC
form includes a chain-of-custody record located at the bottom of the form. The form is used as physical evidence of
sample custody. EPA-NEIC guidelines specify that official custody of samples must be maintained and documented
from the time of collection until the time the samples are introduced as evidence in the event of litigation. The sampler
is responsible for the care and custody of the sample until sample shipment A sample is considered to be in your
custody if any of the following criteria are met:
The sample is in your possession or is in your view after being in your possession;
The sample was in your possession and then locked up or sealed to prevent tampering; or
You have placed the sample in a secured area.
Document CLP Analytical Services organic, inorganic samples on separate CLP TR/COC forms. TR/COC forms must
be completed for every shipment of CLP Analytical Services samples to a contract laboratory. Use indelible ink only,
no pencil (a ball point pen is best)! Make corrections by drawing a line through and initialing and dating the error,
then enter the correct information. Erasures are not allowed! Each TR/COC form should be imprinted. Each
TR/COC form documents up to 10 samples per Case number and sample shipment.
A separate TR/COC form must accompany each cooler for each daily shipment. The TR/COC forms must address all
samples in that cooler, but not address samples in any other cooler. This practice maintains the chain-of-custody for
all samples in case of mis-shipment.
Instructions summarizing CLP sample volumes, packaging and reporting requirements are printed on the back of the
TR/COC forms.
21
-------
Any errors on the TR/COC forms should be immediately reported to the authorized RSCC or CLASS personnel who
can then inform the laboratory. The faster such problems are identified, the faster they can be corrected and critical
delays in sample analysis may be avoided. See Section 7.0, Communication Network.
Exhibits 5-5, and 5-6 are examples of completed TR/COC forms. Exhibit 5-7 provides step-by-step instructions for
filling out the organic and inorganic TR/COC forms. Exhibit 5-8 provides purpose codes for the forms. Samplers may
find it helpful to carry these instructions to the field. Site managers should consider appending these 'instructions to the
SAP.
After you have properly completed the TR/COC form, place the bottom two copies (white and yellow for organic and:
inorganic samples) in a plastic bag, then tape the bag to the inside of the sample cooler lid. The second copy (pink for
organic and inorganic samples) must, be returned to the CLASS contractor within five days of sample shipment. The
address of the CLASS contractor is provided in Exhibit 7-3. The top copy (blue for organic and-green for inorganic)
should be sent to designated Regional personnel.
Note: All samples in a cooler must be recorded on a TR/COC form inside the cooler and each unique sample
number should be listed on only one TR/COC form. (In the case where aliquots of the same sample are collected
at different times [as may occur when well development is very slow] and shipped sequentially, fractions may be given
different sample numbers. If fractions are given unique sample numbers, it will be necessary for the Region to track
the fractions and maintain the knowledge that the fractions are from the same sample.) If all containers necessary for
the analysis of 10 samples cannot fit into one cooler, divide samples into more coolers, making sure that all containers
for each sample are in the same cooler. Place corresponding sample documentation into each cooler. IF MORE THAN
ONE TR/COC FORM IS USED FOR THE SAMPLES IN ONE COOLER, then all of the forms must have complete
header information and signatures.
5.5 Field Operations Records Management System
In an effort to streamline the resource intensive field documentation functions that occur during sampling activities,
EPA-NEIC, at the request of the AOC, developed the Field Operations Records Management System II (FORMS II).
FORMS II is software that facilitates the capture of field information during sampling events, and automates the
production of bottle labels, sample tags, bottle-specific custody seals, chain-of-custody records, cooler seals, PRP sample
receipt records, and field reports. FORMS II enables field personnel to download data to the laboratory, RSCC, and
Regional users. FORMS II design features include the following:
Hardware portabilitv/compatibility/versatilitv
Because field samplers cannot guarantee access to an AC power source or a stable computer working environment,
FORMS II is compatible with existing portable hardware including portable computers, portable printers, and
portable bar code scanning devices. While FORMS II is mouse-compatible, unknown field conditions prohibit
FORMS II reliance on a mouse; but other pointing devices may be useful.
FORMS II uses hardware units specially selected to minimize the likelihood of failure or downtime as a result of
adverse field conditions.
Bar code application
FORMS II uses bar code technology to accelerate the sample packing process for sample shipment to CLP
laboratories. In addition, laboratory personnel may use the sample bottle bar codes to facilitate receipt and
associated records management activities.
/
Flexibility for multiple samplers/samples
22
-------
Field samplers and field sampling organizations often use unique numbering and identification schemes in addition
to the CLP sample numbers when collecting samples. They also vary in their approach to many other activities.
For that reason, FORMS II design includes choices for: identification scheme, activity names, labeling information,
and number and types of labels/tags/seals.
Sample Definitions
FORMS II design is based on field sample, QC sample, and analytical fraction definitions that are consistent with
those provided in Section 3.0, Sample Collection. FORMS II improves field time management, standardizes
information management, and captures collection information in an electronic format early in the field sampling
process. Estimated training time for new FORMS II users is less than two hours. FORMS II is currently managed
by AOC. If you are interested in using FORMS II, please contact AOC at (703) 603-8870.
23
-------
MUM
Ml ProMeftn Agtney
»y Program
Organic Traffic Report
& Chain of Custody Record
(FofprganteCLPAmlyiia)
SASNo,
root****)
CataNo.
J5025
w
V
o
era
so
O
O
o
3
"2,
5T
1. Project Coda
2/S/HfO.O
Account Code
Ragtonal Information
NcxvSuperfund Program
Cliy. Start
SKBSpillD
zz
2. Region No.
1
SanpHngCo.
Sampler (Nam«)
JOHN SMITH
Sampler Signature
Uofvn '
3. Purpose'
£4**?
"JL&
CLEM
PA
REM
RI
ES&.
FS
F»D
*A ;
O&M
KEL&
4, Date Shipped
8//0/92
Carrier
fern
AhMi Number
/ 23-^56-7890
J25
5. Ship To
8. Matrix
(Enltr
In Column A)
\ . Surface Water
3. Ground Waler
3. Lgichata
4. FI»I(JQC
S. Soil/Sediment
I004AROWW4Y
HOPZ.V4 22111
(High only)
8. O
ATlNr
CUSTQt>!4N
ther (Sfttclfy
IB Column A}
7. Pras«rvattva
f£nt*> fn
Column D)
t.HCl
2.HNO3
3 N«HS04
4. H2S04
S. lea «nly
6.OJM*
w.
dp
Sample
Number*
(from
A
Matrix
{train
Box 6)
8 _
Cone.: Sample Prwe
Low ---n
Mod
High
O
Mr-
vativ*
^
RASAnalyjl*
w
ftegtooalSpadfic
T»cl*w Number
or Tag Number*
ARO
Q
Station
Location
Idtttttflar
H
M»/D*y/
Year/Dm*
Sample
J
Sampler
Innate
K
FteWQC
os
/H/ICC22
1315
/MCC23
477 1 6-47721
4fK2b
X-
47722-47723
M.
1ft
Jl
1Z
IS
J4L
J5.
Jfi_
JL
Jl
ji:
SrHpmant tor Case
Complete? (YJNloQ
Sample(t)l96aOw/«? 1 («> 35
ReoefvwJby:
RaftnquWwdby; (Slgrmturm)
DaM/Tlma
Raealvadby:
(Slgnutun}
Dale/tlme
Rec^vadby: (SfrHtun)
Data/Tkne
Racahwaby:
RalnqulshMby: (SlgnMin)
OaM/Tkna
RacvKiad for UUwMOry IHR'
Oate/Tkna
Ramarto ttcunodyaMlMact? Y/N/oona
3
BUI* - ft^i wi co»r , - M ,
rt Copy "w *»«« <»l*t>" V«te*-tt»CoJ»»erll«MmHil»0
*H MVIMf FOR AOOmONAt STAMOAMD INtTM)CnOM«
-------
Exhibit 5-5. Organic TR/COC Form Example (Continued)
Organic Traffic Report/Chain of Custody Form Instructions
Thisjorm replaces both the individual Trajflc Report and EPA Chain of Custody Record.
Required
volume
Woter Sample
Container Type
Soll/Sedjmont
Sample*
Required
Volum«
Extractoble
Analysis
CLOW Level)
Extractable
Analysis
volatile Analysis
(Low Level')
1 X 4-Uter Amber
Glass Bottle
2 X BO-oz. Amber
Glass Bottle
1 II If If 1
U LJ U U
n n n n 32-
U U U U
nn
4Xl-UterAmber
Slass Bottles
Container Type
Extractoble 6 oz.
Analysis
(Low or Medium
Level')
240ml.
Volatile Analysis
(Low or Medhjm
Level')
U
DO
a o
1 X s-oz.wiae-Mourh
Glass Jar
OR
2 X 4-oz. WkJe-Moutn
Glass Jars
2X120 ml.
Wide-Mouth Glass
vlalst
1So*l VOA vlob undef study, subject to change, cneck to enure proper feal
HIGH CONCENTRATION SAMPLE COLLECTION
REQUIREMENTS
Liquid o. SoUd Required
Somp4e» Volume Conta>ver Type
J 'All Medium and High Level Samples Must be Sealed In
Metal Can for Shipment
Extractable and
volatile Analysis
I x 8-oz wiae-Moutn
Glass Jar
1. Organic Sample Collection Requirements
Please Indicate which sample(s) are to be used for laboratory QC (Matrix Spike/Matrix Spike Duplicate).
Ship medium and high concentration samples In metal cans.
Aqueous samples require one triple-volume sample per twenty for Matrix Spike/Matrix Spike Duplicate.
Oily samples can not be analyzed under the Contract Laboratory Program Analytical Services (CLPAS) program.
2. Cooler and Sample Documentation
Complete all sections of the Traffic Report/Chain of Custody Form - Press firmly with a ball point pen to ensure
that carbon copies are legible. Check the information and correct any errors.
Please remember to complete the Chain of Custody information on the form.
Seal the two sets of laboratory Traffic Report/Chain of Custody Form copies in a plastic bag. Include a return
address and a method for returning the cooler. Tape bag under cooler lid.
Seal each container in a plastic bag.
Pack medium and high concentration samples in metal cans.
Cool low waters to 4° C. Cooling of low soils is optional. Do not cool medium or high concentration waters and
soils.
Separate and surround cooler contents with vermiculite or equivalent packaging.
Seal the cooler, overlapping the lid and body with custody seals.
Mall CLASS the pink copy of the Traffic Report/Chain of Custody Form within 5 days.
3. Sample Shipment and Reporting
All relevent Department of Transportation regulations must be followed when shipping samples.
PHONE IN ALL SHIPMENTS IMMEDIATELY TO CLASS (or to RSCC. If Instructed)
Required Information:
Case Number
Date shipped
Number of samples by concentration, matrix and analyses.
Carrier and airbill number
Next planned shipment
Leave your name and a number where you can be reached.
Information for SATURDAY DELIVERIES must be phoned in by 3:OO PM (Eastern) the preceding FRIDAY.
Report any delays or changes of scope (i.e.. changes In number of samples to be collected, matrix changes, etc.)
CALL IF YOU HAVE ANY QUESTIONS
Contract Laboratory Analytical Services Support
3OO North Lee Street
Alexandria. VA 22314
Phone: (7O3) 519-120O
FAX: (7O3) 519-8626
Uafl
SF - Supwfund
PRP - Commercial Potentially
RMpomMe Party
ST = SUM
FED - Federal Facility
Purpoee Codei
Enrh/Acflon
CLEM - CtaMlcal Emergency SI
PA - Early Action Preliminary ESI
Assessment
REM - Removal HI
- Site Inspection
» Expanded Site
Inspection
FS
RD -
RA >
O*M .
NPLD .
Action
Feasibility Study
Remedial Design
Remedial Action
Operation A
Maintenance
National Priorities Uat
Deletion
* U&WO-. l»«a «9« T«1
25
-------
to
a\
Mnqubhedby.
DMI/ttM
»$»
M»/t»M,
RtctWodty
Rtfnqulihtd by:
OMfnki*
OMt/Tini
U custody MM bud? YffWxx*
iMh«« HIM *n mmmit rat /womotwi
ME MVIMt TO« WWOM M
(Mwucnow
W
x
er
85
O
O
o
3
o_
m1
-------
Exhibit 5-6. Inorganic TR/COC Form Example (Continued)
Inorganic Traffic Report/Chain of Custody Form Instructions
This form replaces both, the individual Traffic Report and. EPA Chain of Custody Record.
Requtod
Volume
ConMmrtyp*
Sot/Sedment toquked
volume
Metafe Anatysb 1 uter
(LowieveO
Metab Analysis 16oz.
(Me Oum Level')
Cyanide
Analysis 1 Liter
(low Level)
Cyanide
Analysis 16 oz.
(Medium level')
000
ooo
1 X 1 -liter
Poryettiylene Bottle
OR
2XSOr>m!.
Polyethylene Bottle
1XI6-OZ
Wide-Mouth Stem
Jar
1 X l-Uter
Polyethylene Bottle
OR
2X500-m!.
Polyethylene Bottle
1X16-OZ
Wide-Mouth Glass
JOJ
ContakMr.Typ*
Metals and 6 oz.
Cyanide (CrT)
Analysis
[LoworMedkjm
Level-)
n
uu
1 X 8-oz.WWe-Moum
Glass Jar
OR
2 X4-oi Wide-Mouth
Glass Jon
HIGH CONCENTRATION SAMPLE COLLECTION
REQUIREMENTS
Liquid or Said
templet
Requited
Volume
Container Type
Metals and
Cyanide-Analysis
D
1 X 8-az. Wide-Mouth
GtaoJar
1.
Al Medum and High Level Samples Must be Sealed In
Metal Can for Shipment
Inorganic Sample Collection Requirements
Please indicate which sample(s) are to be used for laboratory QC (Matrix Spike/Duplicate).
Aqueous samples require one double-volume sample per twenty for laboratory Matrix/Spike Duplicate.
Preserve low level water samples:
Total metals Preserve with HNO3 to pH S 2
Dissolve metals Preserve with HNO3 to pH £ 2 after filtering through a 0.45 nm filter.
Cyanide Preserve with ION NaOH to pH 2 12
Oily samples can not be analyzed under the Contract Laboratory Program Analytical Services (CLPAS) program.
Ship medium and high concentration samples in metal cans.
2. Cooler and Sample Documentation
Complete all sections of the Traffic Report/Chain of Custody Form - Press firmly with a ball point pen to
ensure that carbon copies are legible. Check the Information and correct any errors.
Please remember to complete the Chain of Custody information on the form.
Seal the two sets of laboratory Traffic Report/Chain of Custody Form copies in a plastic bag. Include a return
address and a method for returning the cooler. Tape bag under cooler lid.
Seal each container in a plastic bag.
Pack medium and high concentration samples in metal cans.
Cool low waters to 4° C. Cooling of low soils is optional. Do not cool medium or high concentration waters and
soils.
Separate and surround cooler contents with vermiculite or equivalent packaging.
Seal the cooler, overlapping the lid and body with custody seals.
Mail CLASS the pink copy of the Traffic Report/Chain of Custody Form within 5 days.
3. Sample Shipment and Reporting
All relevent Department of Transportation regulations must be followed when shipping samples.
PHONE IN ALL SHIPMENTS IMMEDIATELY TO CLASS (or to RSCC, if instructed)
Required information:
Case Number
Date shipped
Number of samples by concentration, matrix and analyses.
Carrier and airbill number
Next planned shipment
Leave your name and a number where you can be reached.
Information for SATURDAY DELIVERIES must be phoned in by 3:00 PM (Eastern) the preceding FRIDAY.
Report any delays or changes of scope (i.e., changes In number of samples to be collected, matrix changes, etc.)
CALL IF YOU HAVE ANY QUESTIONS
Contract Laboratory Analytical Services Support
300 North Lee Street
Alexandria. VA 22314
Phone: (703)519-1200
FAX: (703) 519-8626
Purpose Cod«
SF » Superfund
PRP « Commercial Potentially
Responsible Party
ST = Stale
FED » Federal Facility
CLEM = Classical Emergency
PA = Early Action Preliminary
Assessment
REM . Removal
SI
ESI
Rl
Site Inspection
Expanded Site
Inspection
Remedial Investigation
Lgpg-T
FS
RD
RA
O&M
NPLD
arm Action
Feasibility Study *
* Remedial Design
= Remedial Action
Operation &
Maintenance
National Priorities List
Delation
* O«. OPO; 1M639ITH)
27
-------
Exhibit 5-7. Organic and Inorganic Traffic Report/Chain-of-Custody Forms Instructions
STEP
STEP1
STEP 2
STEP 3
STEP 4
STEPS
STEP 6
STEP?
STEPS
STEP 9
STEP 10
STEP 11
STEP 12
STEP 13
STEP 14
STEP 15
STEP 16
STEP 17
STEP 18
INSTRUCTIONS
The SAS Order number is no longer applicable. Leave this box blank.
Record the Case number that has been assigned to the sampling event.
Transcribe the project codes and site information. Enter the project and account codes assigned to the project by
the RSCCs or EPA Site Managers. Record the site name, city, state, and site spill ID (assigned by your Region).
This part of the form is desensitized and -will not print on the laboratory copies. All site information must be
kept confidential.
Record your Region number and the name of your sampling company. Print your name and include your
signature in the space following. Additional space for sampler signatures is provided for in the area designated
as Step 23.
Place a check mark in the appropriate box for funding lead under the column labeled "Lead." Place another
check mark under either the "Early Action" or "Long-Term Action" columns for sampling effort. Two boxes
must be checked in this area. Note that RCRA is an example of a federal lead sampling activity. Purpose codes
.are described in Exhibit 5-8.
Record the date shipped, the carrier name (e.g., Federal Express, Purolator or Airborne) and the air bill number.
Record the name and full address of the contract laboratory. Enter the name of the sample custodian or CLP
contact. If contact name is unknown, write "CLP'Sample Custodian."
Transcribe the CLP sample number from the preprinted sample labels exactly as it appears. Do not add hyphens,
extra zeros, characters, or digits.
Record the appropriate matrix code from the choices listed in box number 6 on the form. If the Region is
shipping a quality control (QC) sample such as a field blank, coolant blank, trip blank, spike, duplicate, or
performance evaluation sample, then "Field QC" should be entered as the matrix for that sample. However, if
the Region -wishes to keep the QC sample blind to the laboratory [this is recommended], then the sampler should
enter either "1, " "2, " or "3" for water QC samples, and "5" for soil/sediment QC samples as the matrix code in
Column A, "Matrix."
Enter the estimated sample concentration. For organic samples, enter "L" for low/medium aqueous samples, "L"
for low concentration solid samples, artd "M" for medium concentration solid samples. For inorganics, enter "L"
for low concentration samples, "M" for medium concentration, and "H" for high concentration.
Enter the sample type, either composite or grab.
Record the type of preservative, using the codes from box number 7 on the form.
In the analysis columns, make a check mark for each fraction to be analyzed. (It is not necessary to write the
number of sample containers used.) Organics fractions are volatiles, semivolatiles, and pesticides/ Aroclors;
Inorganic fractions are total metals, dissolved metals, and cyanide. For each individual inorganic sample, you
may request either total metal or dissolved metal analyses, but not both. That is, samples collected for total
metal and dissolved metal analyses must receive separate (unique) sample numbers. Note: Your form may also.
contain future or recently discontinued fraction analyses.
Transcribe the Region-specific tracking numbers or tag numbers designated by, the RSCC. If possible, all tag
numbers for each CLP sample should be on one line. If several tags with consecutive numbers are used for one
sample, the first number must be completely transcribed. Remaining tag numbers in the sequence can either be
represented by including only those numbers that are unique (separated by commas) or by listing the first and
last numbers of the sequence, separated by a dash. The TR/COC form entries should make it clear which tag
number corresponds to which fraction.
Enter the station location number.
Record the month, day, year, and time, in military style (e.g., 1600 hours = 4:00 p.m.), of sample collection.
This may make field QC samples (e.g., duplicates) non-blind to the laboratory.
Enter the corresponding organic or inorganic CLP sample number, if applicable.
Enter your initials.
28
-------
Exhibit 5-8. Purpose Codes
FUNDING ACTIVITY
CODE
DEFINITION
Funding Lead
SF
PRP
ST
FED
Superfund
Potentially Responsible Party
State
Federal
Early Action
CLEM
PA
REM
RI
SI
ESI
Classic Emergency
Preliminary Assessment
Removal
Remedial Investigation
Site Inspection
Expanded Site Inspection
Long-Term Action
FS
RD
RA
O&M
NPLD
Feasibility Study
Remedial Design
Remedial Action
Operations and Maintenance
National Priorities List Delete
5.6 Custody Seal
The custody seal is used to seal sample containers before they are placed into the cooler. Custody seals are also placed
across the cooler opening after the cooler has been properly secured. The purpose of a custody seal is to indicate that
the sample has not been tampered with prior to analysis. Therefore, for potential litigation purposes, you must sign and
date the custody seal. It is a good practice to place the seal so that it is the signature that would be broken if the
sample/cooler were opened (e.g., place the signature across the cooler/sample opening). Contact your authorized
requestor or RSCC to obtain custody seals. Note: The space for "Sample No." does not need to be filled out on custody
seals placed across the cooler opening. An example of a signed custody seal is shown in Exhibit 5-9. Because the use
of custody seals varies between Regions, always refer to Regional guidance.
Exhibit 5-9. Custody Seal
' UNITED STATES
ENVIRONMENTAL PROTECTION AGENCY
OFFICIAL SAMPLE SEAL
SIGNMURE
PRINT NAME AND TITLE
JOHN JONC3
29
-------
6.0 SAMPLE PACKAGING AND SHIPPING
6.1 Sample Packaging
Follow all state and Federal regulations governing environmental sample packaging and shipment. Ship according to
U.S. Department of Transportation (DOT) and International Air Transportation Association (IATA) regulations. The
following sample packaging and shipping procedures need to be considered as minimum requirements. For some
samples and shipping situations, these requirements may need to be exceeded.
The site name should not appear on any documentation sent to the CLP laboratory.
Aqueous samples for inorganic samples and volatile organic analysis may require chemical preservation.
Note that the Regions may have slightly different requirements for the preservation of samples for volatile
analysis, so Regional requirements should be consulted. Refer to Section 3.8, Sample Preservation and
Holding Times, for these techniques before packaging.
Check all lids/caps to make sure they are tight and will not leak. Place a completed custody seal over each
container lid/cap, except for vials for volatile samples where the custody seal must be wrapped around the
lid. (Note that the Regions may have slightly different requirements for placing custody seals and using tags,
so Regional requirements should also be consulted. For custody seals, the objective is to place the seals in
such a way that sample containers cannot be opened or tampered with without breaking the seal).
Make sure sample labels are intact and covered with a piece of clear tape for protection. Tie on completed
, sample tags. Although there are no procedural requirements for tying on sample tags, a recommended
approach is to tie the tag onto the sample bottle with a string by wrapping the string around the neck of the
sample bottle and then tying the string into a knot.
Enclose the sample container in clear plastic bag and seal the bag. Make sure the sample tags and labels are
visible. See Exhibit 6-1. Note that if bubble wrap or other wrapping material will be placed around the
labeled and tagged containers, write the sample number and fraction (e.g., "BLHOl-VOCs") so that it is
visible on the outside of the wrap, and then place the wrapped container in a clear plastic bag and seal the
bag.
Make sure that all samples that need to be kept cold (4+A2°C) have been thoroughly cooled before placing ,
in packing material so that the packing material serves to insulate the cold. Change the ice prior to shipment
as needed. Ideally, pack the cooled samples into shipping containers that have already been chilled.
Any soil/sediment samples suspected to be of mediumyhigh concentration or containing dioxin must be
enclosed in a metal can with a clipped or scalable lid (e.g., paint cans) to achieve double containment of those
samples. Place suitable absorbent packing material around the sample container in the can. Make sure sample
is securely stored in can and the lid is sealed. Label the outer metal container with the sample number and
fraction of the sample inside. See Exhibit 6-1.
Use a CLEAN waterproof metal or hard plastic ice chests or coolers in good repair for shipping samples.
Remove the inapplicable previous shipping labels. Make sure any drain plugs are shut and seal plugs shut
on the inside and outside with a suitable tape such as duct tape. Line the cooler with plastic (e.g., large
heavy-duty garbage bag) before inserting samples.
Ship samples at 4° +/- 2°C, place double-bagged ice on top of samples. Ice must be sealed in double plastic -
bags to prevent melting ice from soaking the packing material. Loose ice must not be poured into the cooler. <
30
-------
It is good practice to conduct an inventory of sample numbers, fractions, and containers when placing
samples into the coolers, and then check the inventory against the corresponding TR/COC form before
sealing the cooler to make sure that all samples and containers are present.
Pack the lined shipping containers with noncombustible, absorbent packing material such as vermiculite or
rock wool. Place the packing material on the bottom of the shipping container (inside the plastic liner) and
around sample bottles or metal cans to avoid breakage during shipment. Never use earth, ice, paper, or
styrofoam to pack samples. Earth is a contaminant, melted ice may cause complications and allow the sample
containers to bang together when the snipping container is moved, and styrofoam presents a disposal problem
(it also may easily blow out of the shipping container at the site).
For samples that need to be shipped at 4° +/-2°C, place double-bagged ice on top of samples and fill
remaining space with packing material. Note that if sample bottles have been protected with packaging
material such as bubble wrap, then some double-bagged ice or ice packs may also be placed between
samples.
Use tape to securely fasten the top of the plastic used to line the shipping container. It is a good idea to then
place a completed custody seal around the top of the bag which contains the sample in case the outer seals
placed across the cooler lid are inadvertently damaged during shipment.
Enclose all sample documentation (i.e., TR/COC, other chain-of-custody forms, and cooler return shipping
documents) in a waterproof plastic bag, and tape the bag to the underside of the cooler lid. See Exhibit 6-2.
This documentation should address all samples in the cooler, but not address samples in any other cooler.
If more than one cooler is being used, place separate sample documentation in each cooler.
Instructions for returning the cooler should be documented inside the cooler lid. Write a return name and
address for the sample cooler on the inside of the cooler lid in permanent ink to ensure return of the cooler.
Tape the cooler shut using strapping tape over the hinges. Place completed custody seals across the top and
sides of the cooler lid so that lid cannot be opened without breaking the seal. See Exhibit 6-3.
Place clear tape over the seal to prevent inadvertent damage to the seal during shipment. Do not place clear
tape over the seals in a manner that would allow the seals to be lifted off with die tape and then reaffixed
without breaking the seal.
31
-------
Exhibit 6-1. Sample Packaging
Custody
Seal
Sample
Container
Clear plastic
Dag
Exhibit 6-la. Sample Packaging
32
-------
Exhibit 6-2. Sample Cooler With Documentation
SAMPLE DOCUMENTATION
Exhibit 6-2a. Sample Cooler With Documentation
33
-------
Exhibit 6-3. Sealed Cooler
CUSTODY SEALS
6.2 Sample Shipping
Clearly label cooler and fill out appropriate shipping papers. Exhibit 6-4 shows the top of a cooler ready to be shipped.
Place return address labels clearly on the outside of the cooler.
If more than one cooler is being delivered to a laboratory, mark each cooler as "1 of 2," "2 of 2," etc. An air
bill should be filled out for each cooler being shipped. When addressing the air bill to ship samples, identify
the recipient as the "sample custodian."
Ship samples through a commercial carrier, such as Federal Express, Purolator, or equivalent.
Fill out all required government and commercial carrier shipping papers according to DOT and IATA
commercial carrier regulations.
Ship all samples by overnight delivery, in accordance with DOT and IATA regulations.
6.3 Potential Sampling Problems
Sometimes problems arise during sampling from improper sampling practices or other reasons. Some common
problems to watch out for are:
Filling out paperwork incorrectly or incompletely.
Using the wrong Case number.
Collecting less than the required sample volume.
34
-------
Shipping samples to the wrong laboratory.
Exhibit 6-4. Top of Cooler
Return
Address
Label
Airbill
§-
f
"M
J Env. lab samples "]
Tape over
hinges
Assigning the same CLP sample number to dissolved and total metals water samples collected from the same
location.
Using incorrect sample containers.
Improperly filling or packing sample containers.
Preserving sample with incorrect preservative.
Improperly labeling cooler.
These problems may delay sample analysis. If any of these problems occur, contact your RSCC or CLASS Coordinator
immediately for instructions.
6.4 Reporting Sample Shipment
Notify the authorized RSCC or CLASS personnel, as directed, of all sample shipments on the day of shipment. This
notification enables the CLASS contractor to track the shipment of samples from the field to the laboratory and ensures
timely laboratory receipt of samples. When calling the CLASS contractor [General number: (703) 519-1200], provide
the following information:
Your name, phone number, and Region.
Case number of the project.
35
-------
Exact number(s) of samples (not number of containers), matrix(ces) and concentration^) of samples shipped.
Type of analysis required.
Laboratory(ies) to which samples were shipped.
Carrier name and air bill number(s) for the shipment.
Method of shipment (e.g., overnight, two day).
Date of shipment.
Suspected contaminants associated with the samples or site (e.g., dioxin, radio chemicals).
Information on completions, changes, delays, continuations, etc., pertinent to the Case and sampling project.
Sample shipments made after 5 p.m. EST should be scheduled with the CLASS contractor at the start of business the
next day (8 a.m. EST). You must notify the CLASS contractor by 3 p.m. EST Friday for sample shipments that
will be delivered on Saturday. If the CLASS contractor cannot notify the laboratory of a Saturday delivery, there may
not be anyone present at the CLP laboratory to receive samples until Monday.
6.5 Sample Cooler Returns
Regional and Regional Support Contractor Responsibilities
The EPA Regions and their support contractors are responsible for providing a mechanism for shipping empty sample
coolers from the CLP laboratories back to the originating sampling office. AOC provides the following suggestions
to maintain consistency among cooler transportation programs:
Sampling contractors should include a completed shipping label in the cooler, which can have any coded
information for tracking purposes.
The label should consist of multi-copies so the laboratory and the sampling contractors can each retain one
for their records.
The label should be designed so that the laboratory can simply place the already-completed label on the
cooler for shipment purposes.
The label should include third-party billing information so that the transportation carrier is able to invoice
the correct sampling contractor. The laboratory should be informed of the identity of the carrier.
To avoid confusion, each Region should attempt to use only a minimum number of different carriers.
Sufficient information should be included on the label to enable the sampling contractor to track use of the
billing number.
The process should be as easy as possible for the laboratories.
Laboratory Responsibilities ,
The laboratory is required to return sample coolers to the appropriate sampling office within 14 calendar days following
shipment receipt. The laboratory should ensure that the account numbers provided by the Region are used only for the
return of Government-owned shipping containers.
36
-------
Laboratories are required to remove packing and other materials from the coolers before each pick-up and are required
to ensure that the coolers are clean. Laboratories can determine from visual inspection if the coolers are clean. An
authorized laboratory official is required to sign and telefax the pick-up records to the designated transportation
contractor or sampler within two calendar days of cooler pick-up for return.
If laboratories do not follow the procedures, notify the TPO listed in Exhibit 7-1 for the Region where the laboratory
is located.
37
-------
7.0 COMMUNICATION NETWORK
This section provides Regional contacts for questions or concerns regarding CLP Analytical Services sampling and
analysis. Exhibit 7-1 lists names and telephone numbers for Regional Technical Project Officers, who serve as the first
line of contact for the laboratory for all technical problem resolution. Exhibit 7-2 gives names, addresses, and telephone
numbers of Regional primary RSCCs. These contacts are available for CLP Analytical Services analytical requests and
serve as the first contact for information regarding sampling.' Exhibit 7-3 gives names, addresses, and telephqne
numbers of the CLASS Regional CLP Analytical Service contacts, who serve as a second contact for information
regarding sampling. The RSCCs and CLASS coordinators can advise samplers regarding problems that occur in the
field.
Exhibit 7-1. Regional Technical Project Officers
Region
Region I
Region II
Region III
Region IV
Region V
Region VI
Region VII
Region VIII
Region IX
Region X
Technical Project Officer
Deb Szaro, Moira Lataille
Pat Sheridan
Stevie Wilding
Gary Bennett
Brian Freeman
Ray Flores
Larry Marchin
Steve Callio
Steve Remaley
Bruce Woods ;
Telephone
Number
(617)860-4312
(908)906-6169
(410)573-6833
(706) 546-3287
(312)353-2720
(713)983-2139
(913)551-5170
(303)312-7290
(415)744-1496
(206)553-1193
38
-------
Exhibit 1-2. RSCC Addresses and Contacts
Regional Sample Control Centers
USEPA Region I, WMD
60 Westvoew Street
Lexington, MA 02173
USEPA Region II, BSD
2890 Woodbridge Ave. Bldg. 209, MS220
Edison, NJ 08837
USEPA Region III, CRL
201 Defense Highway, Suite 200
Annapolis, MD 21401
USEPA Region IV, BSD
Env. Compliance Branch
College Station Road
Athens, GA 30613
USEPA Region V, WMD
77 W. Jackson Blvd. (HSMC-5J)
Chicago, IL 60604
USEPA Region VI, Laboratory
1 0625 Fallstone Road
Houston, TX 77099
USEPA Region VII, BSD
25 Funston Rd.
Kansas City, KS 66115
USEPA Region VIII, 8ES-MEB
999 18th St.
5th Floor
Denver, CO 80202
USEPA Region IX, QPM, P-3-2
75 Hawthorne St.
San Francisco, CA 94105
USEPA Region X, BSD
1200 Sixth Ave. (M/S ES-095)
Seattle, WA 98101
Primary RSCC*
Christine Clark
(617) 860-4615
Phil Guarraia
(908)321-6697
Carolyn Sierra
(410) 573-2755
Bill Bokey
(706) 546-3299
Cecilia Luckett
(312)886-1488
Myra Perez
(713)983-2130
Nicole Roblez
(913)551-5130
Carol Beard
(303)312-6047
Gail Jones
(415)744-1498
Laura Castrilli
(206) 553-4323/1795
* Primary RSCC assignments are subject to change.
39
-------
Exhibit 7-3. CLASS CLP Analytical Services Coordinators '
Region
Region I
Region II
Region III
Region IV
Region V
Region VI
Region VII
Region VIII
Region IX
Region X
CLASS Regional
Coordinator2
Neil Rogers
Neil Rogers
Carol Shaeffer
Carol Shaeffer
Mistie Llewellyn
Mistie Llewellyn
Mistie Llewellyn
Carol Shaeffer
Neil Rogers
Neil Rogers
Telephone
Number
(703)519-1019
(703)519-1019
(703)519-1461
(703)519-1461
(703)519-1084
(703)519-1084
(703)519-1084
(703)519-1461
(703)519-1019
(703)519-1019
1 The address for CLASS is Contract Laboratory Analytical Services Support, P.O. Box 818,
Alexandria, VA, 22313. The phone number for CLASS is (703) 519-1200.
2 The coordinator assignment is subject to change.
40
-------
8.0 GLOSSARY
AOC: Analytical Operations Center.' The U.S. EPA Center which directs the national Contract Laboratory Program.
APO: Administrative Project Officer. The APOs are part of AOC and monitor laboratory performance, initiate contract
action and laboratory funding, help resolve problems, and develop and design analytical services and methods.
Aliquot: A measured portion of a sample taken for analysis. One or more aliquots make up a sample.
Case: A finite, usually predetermined number of samples collected over a given time period from a particular site. A
Case consists of one or more sample delivery groups (SDGs). See sample delivery group.
Case number: Number assigned to a set of CLP Analytical Services samples by the CLASS contractor for tracking
purposes.
CLASS: Contract Laboratory Analytical Services Support. The contractor-operated CLASS office provides
management, operations, and administrative support to the CLP. The CLASS contractor schedules sample shipment
for CLP Analytical Services requests.
CLP: Contract Laboratory Program. The CLP provides analytical services to the 10 EPA Regions through contracted
commercial laboratories.
CLPAS: Routine CLP Analytical Services performed by laboratories that have been awarded CLP government
contracts.
Concentration: Defined as high, medium, or low and used to determine how much volume is collected or the analytical
protocol to be followed.
Data turnaround time: The maximum length of time allowed for laboratories to submit analytical data to EPA in order
to avoid liquidated damages. Data turnaround time begins at the validated time of sample receipt (VTSR) at the
laboratory.
DOT: Department of Transportation.
Fraction: A specific subunit of an analytical protocol. For example, for low/medium organics, the fractions are
volatiles, semivolatiles, and pesticides/Aroclors.
FORMS II: FORMS II is software that facilitates the capture of field information during sampling events, and
automates the production of bottle labels, sample tags, bottle-specific custody seals, chain-of-custody records, cooler
seals, PRP sample receipt records, and field reports.
Headspace: Air pocket in a VOA vial.
Holding time: The maximum amount of time a sample may be stored before analysis.
IATA: International Air Transportation Association.
Matrix: The principal material of which the sample is composed of, usually water or soil/sediment for CLP Analytical
Services samples.
41
-------
NEIC: National Enforcement Investigations Center, a part of EPA, which is supporting the Agency's enforcement
program, located in Denver, Colorado.
Preservative: A chemical added to inorganic and volatile water samples to maintain the integrity of the sample. Some
common preservatives include nitric acid, hydrochloric acid, and sodium hydroxide.
QC Samples: Samples used to estimate the precision and accuracy of analytical results in the field and in the
laboratory. ,
RSCC: Regional Sample Control Center. The RSCC coordinates Regional sampling efforts.
Sample: A single, discrete portion of the environment collected from a specified physical location at a specific time.
The single sample may be placed in multiple vessels. The aliquots are identified by the same sample number.
Sample container: The individual bottle that contains the sample or an aliquot of the sample. The type of sample
container varies for different sample fractions and concentrations.
Sample custody: Legal possession of and responsibility for an EPA sample. Documentation of sample custody is
maintained on the chain-of-custody part of the traffic report or packing list. The sample is in your custody if any of the
following criteria are met: 1) the sample is in your possession or is in your view after being in your possession, 2) the
sample was in your possession and then locked up or sealed to prevent tampering, or 3) you have placed the sample in
a secured area.
Sample label: Adhesive labels distributed by the RSCC that provide the sample numbers to be assigned to me samples.
Sample number: The sample number from the sample label that identifies the sample or an aliquot of the sample.
SDG: The sample delivery group (SDG) is a unit within a Case that is used to identify a group of samples for delivery
An SDG is defined as one of the following, whichever comes first:
all samples within a Case, or
every set of 20 field samples within a Case, or
all field samples in a Case which are received at a laboratory during a specified period of tune, beginning
with receipt of the first sample in the Case or SDG.
SOW: Statement of work. This document specifies how laboratories analyze samples under a particular CLP analytical
program.
Station location: The specific location where samples are collected on a site.
TAL: Target Analyte List. TALs list the target analytes to test for in inorganic analyses.
TCL: Target Compound List. TCLs list the target compounds to test for in organic analyses.
TPO: Regional Technical Project Officer. The TPO monitors the activities of the contract laboratories located in his
or her Region.
TR/COC: CLP Analytical Services Traffic Report/Chain of Custody form. This form is used to track CLP Analytical <
Services samples from sample collection to sample receipt by the laboratory.
Volume: The amount of sample collected. Volume requirements differ between CLP Analytical Services programs,
matrices, fractions, and concentrations.
42
-------
VOA: Volatile Organic compound Analysis. Used synonymously with VOC.
VOC: Volatile Organic Compound.
VTSR: Verified Time of Sample Receipt.
43
-------
9.0 EPA REFERENCE DOCUMENTS
Copies of the EPA Reference documents may be obtained from:
National Technical Information Service
U.S. Department of Commerce
5285 Port Royal Road
Springfield, VA 22161
(703) 487-4650
U.S. EPA, "The Data Quality Objectives process for Environmental Decisions,'' QAMS EPA OA/G4.
U.S. EPA, "The Data Quality Objectives process for Superfund," EPA540-R-93-071.
U.S. EPA, "EPA Requirements for Quality Assurance Project Plans for Environmental Data Operations," EPA QA/R5,
Draft Interim Final, August 1994.
U.S. EPA, "EPA Requirements for Quality Management Plans," QAMS Interim Final, 8/94.
U.S. EPA, "User's Guide to the Contract Laboratory Program," EPA/540/P-91/002, 1991.
U.S. EPA, Compendium of ERT Surface Water and Sediment Sampling Procedures, EPA/540/P-91/005.
U.S. EPA, Compendium of ERT Soil Sampling and Surface Geophysics Procedures, EPA/540/P-91/006.
U.S. EPA, Compendium of ERT Groundwater Sampling Procedures, EPA/540/P-91/007.
U.S. EPA, Soil Sampling and Analysis for Volatile Organic Compounds, EPA/540/4-91/001,
U.S. EPA, Technical Notes on Drinking Water Methods, EPA/600/R-94/173.
Specifications and Guidance for Contaminant-Free Sample Containers, December 1992, OSWER Directive 92.0-05A.
Current CLP Statements of Work are available through NTIS and the CLU-IN Bulletin Board [System Operator at (301)
589-8368] on the Internet (via telnet) at CLU-IN.EPA.GOV.
US Army Corps of Engineers. Requirements for the Preparation of Sampling and Analysis Plans, Draft, June 30, 1994.
EM 200-1-3.
44
------- |